data_shelxl_1Zn _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 Br4 N4 Zn' _chemical_formula_sum 'C36 H30 Br4 N4 Zn' _chemical_formula_weight 903.65 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' 'Br' 'Br' -0.2901 2.4595 '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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.116(5) _cell_length_b 11.382(5) _cell_length_c 27.793(13) _cell_angle_alpha 90.00 _cell_angle_beta 94.543(8) _cell_angle_gamma 90.00 _cell_volume 3505(3) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 10912 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 5.291 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4175 _exptl_absorpt_correction_T_max 0.7778 _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.629 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25541 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.44 _reflns_number_total 7841 _reflns_number_gt 6123 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SIR92 (Altomare, et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_publication_material 'CrystalStructure 4.0' _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^)+(0.1000P)^2^+5.0000P] 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 7841 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0816 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1932 _refine_ls_wR_factor_gt 0.1784 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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 Br1 Br 0.52818(6) 0.18736(7) 0.51332(2) 0.0647(2) Uani 1 1 d . . . Br2 Br 0.83167(5) 0.04011(7) 0.73510(3) 0.0612(2) Uani 1 1 d . . . Br3 Br 0.73158(7) -0.20865(6) 0.60483(3) 0.0623(2) Uani 1 1 d . . . Br4 Br 0.48093(5) 0.32970(6) 0.67080(2) 0.0567(2) Uani 1 1 d . . . Zn1 Zn 0.64092(5) 0.08563(6) 0.62892(2) 0.04222(18) Uani 1 1 d . . . N1 N 0.4831(4) 0.0537(4) 0.59376(17) 0.0429(10) Uani 1 1 d . . . N2 N 0.6081(4) -0.0079(4) 0.68631(16) 0.0410(10) Uani 1 1 d . . . N3 N 0.7886(4) 0.0307(4) 0.59960(17) 0.0440(10) Uani 1 1 d . . . N4 N 0.6873(4) 0.2532(4) 0.62940(16) 0.0430(10) Uani 1 1 d . . . C1 C 0.4344(5) 0.0950(6) 0.5520(2) 0.0497(13) Uani 1 1 d . . . C2 C 0.3129(6) 0.0611(6) 0.5414(2) 0.0574(15) Uani 1 1 d . . . H2 H 0.2604 0.0828 0.5142 0.069 Uiso 1 1 calc R . . C3 C 0.2873(5) -0.0107(6) 0.5794(2) 0.0539(15) Uani 1 1 d . . . H3 H 0.2130 -0.0498 0.5830 0.065 Uiso 1 1 calc R . . C4 C 0.3919(5) -0.0155(5) 0.6123(2) 0.0456(12) Uani 1 1 d . . . C5 C 0.4066(5) -0.0792(5) 0.65521(19) 0.0415(11) Uani 1 1 d . . . C6 C 0.5070(5) -0.0808(5) 0.68900(19) 0.0402(11) Uani 1 1 d . . . C7 C 0.5258(5) -0.1553(5) 0.7295(2) 0.0464(12) Uani 1 1 d . . . H7 H 0.4713 -0.2129 0.7395 0.056 Uiso 1 1 calc R . . C8 C 0.6391(5) -0.1288(5) 0.7521(2) 0.0491(13) Uani 1 1 d . . . H8 H 0.6777 -0.1637 0.7803 0.059 Uiso 1 1 calc R . . C9 C 0.6829(5) -0.0393(5) 0.72381(19) 0.0422(12) Uani 1 1 d . . . C10 C 0.8250(5) -0.0774(5) 0.5906(2) 0.0480(13) Uani 1 1 d . . . C11 C 0.9351(6) -0.0812(6) 0.5692(3) 0.0577(16) Uani 1 1 d . . . H11 H 0.9773 -0.1487 0.5594 0.069 Uiso 1 1 calc R . . C12 C 0.9684(5) 0.0361(6) 0.5653(2) 0.0553(15) Uani 1 1 d . . . H12 H 1.0390 0.0642 0.5520 0.066 Uiso 1 1 calc R . . C13 C 0.8788(5) 0.1062(5) 0.5848(2) 0.0444(12) Uani 1 1 d . . . C14 C 0.8773(5) 0.2286(5) 0.5888(2) 0.0449(12) Uani 1 1 d . . . C15 C 0.7912(5) 0.2979(5) 0.6092(2) 0.0440(12) Uani 1 1 d . . . C16 C 0.7896(6) 0.4220(5) 0.6122(2) 0.0486(13) Uani 1 1 d . . . H16 H 0.8493 0.4737 0.6016 0.058 Uiso 1 1 calc R . . C17 C 0.6850(6) 0.4553(6) 0.6335(2) 0.0525(14) Uani 1 1 d . . . H17 H 0.6586 0.5324 0.6405 0.063 Uiso 1 1 calc R . . C18 C 0.6282(5) 0.3484(6) 0.6423(2) 0.0466(13) Uani 1 1 d . . . C19 C 0.3006(5) -0.1560(5) 0.6665(2) 0.0459(12) Uani 1 1 d . . . C20 C 0.2891(6) -0.2689(6) 0.6484(2) 0.0517(14) Uani 1 1 d . . . C21 C 0.1856(6) -0.3354(6) 0.6580(2) 0.0595(16) Uani 1 1 d . . . H21 H 0.1768 -0.4129 0.6456 0.071 Uiso 1 1 calc R . . C22 C 0.0984(6) -0.2906(7) 0.6848(3) 0.0626(18) Uani 1 1 d . . . C23 C 0.1126(6) -0.1778(6) 0.7033(3) 0.0597(16) Uani 1 1 d . . . H23 H 0.0523 -0.1467 0.7221 0.072 Uiso 1 1 calc R . . C24 C 0.2124(6) -0.1086(6) 0.6951(2) 0.0543(14) Uani 1 1 d . . . C25 C 0.3831(7) -0.3223(6) 0.6183(3) 0.0682(19) Uani 1 1 d . . . H25A H 0.4558 -0.3411 0.6391 0.082 Uiso 1 1 calc R . . H25B H 0.4034 -0.2660 0.5935 0.082 Uiso 1 1 calc R . . H25C H 0.3509 -0.3942 0.6028 0.082 Uiso 1 1 calc R . . C26 C -0.0113(7) -0.3644(8) 0.6955(3) 0.082(2) Uani 1 1 d . . . H26A H 0.0086 -0.4480 0.6933 0.098 Uiso 1 1 calc R . . H26B H -0.0791 -0.3458 0.6720 0.098 Uiso 1 1 calc R . . H26C H -0.0338 -0.3468 0.7282 0.098 Uiso 1 1 calc R . . C27 C 0.2252(7) 0.0112(7) 0.7173(3) 0.083(3) Uani 1 1 d . . . H27A H 0.1560 0.0270 0.7361 0.100 Uiso 1 1 calc R . . H27B H 0.2280 0.0702 0.6917 0.100 Uiso 1 1 calc R . . H27C H 0.2998 0.0147 0.7385 0.100 Uiso 1 1 calc R . . C28 C 0.9835(5) 0.2905(5) 0.5686(2) 0.0471(13) Uani 1 1 d . . . C29 C 0.9779(5) 0.3164(5) 0.5193(2) 0.0467(13) Uani 1 1 d . . . C30 C 1.0797(6) 0.3645(6) 0.5007(2) 0.0539(14) Uani 1 1 d . . . H30 H 1.0769 0.3830 0.4673 0.065 Uiso 1 1 calc R . . C31 C 1.1860(6) 0.3863(5) 0.5298(2) 0.0520(14) Uani 1 1 d . . . C32 C 1.1868(5) 0.3625(6) 0.5779(2) 0.0559(15) Uani 1 1 d . . . H32 H 1.2580 0.3789 0.5980 0.067 Uiso 1 1 calc R . . C33 C 1.0871(6) 0.3149(6) 0.5992(2) 0.0567(16) Uani 1 1 d . . . C34 C 0.8668(6) 0.2912(6) 0.4871(2) 0.0557(15) Uani 1 1 d . . . H34A H 0.8579 0.2061 0.4828 0.067 Uiso 1 1 calc R . . H34B H 0.8735 0.3285 0.4557 0.067 Uiso 1 1 calc R . . H34C H 0.7961 0.3225 0.5018 0.067 Uiso 1 1 calc R . . C35 C 1.2980(6) 0.4333(7) 0.5081(3) 0.069(2) Uani 1 1 d . . . H35A H 1.3642 0.3769 0.5138 0.083 Uiso 1 1 calc R . . H35B H 1.3213 0.5085 0.5232 0.083 Uiso 1 1 calc R . . H35C H 1.2805 0.4447 0.4733 0.083 Uiso 1 1 calc R . . C36 C 1.0923(7) 0.2912(9) 0.6520(3) 0.082(3) Uani 1 1 d . . . H36A H 1.1637 0.3293 0.6680 0.098 Uiso 1 1 calc R . . H36B H 1.0969 0.2063 0.6577 0.098 Uiso 1 1 calc R . . H36C H 1.0195 0.3225 0.6652 0.098 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 Br1 0.0604(4) 0.0760(5) 0.0574(4) 0.0197(3) 0.0036(3) -0.0052(3) Br2 0.0423(3) 0.0696(5) 0.0693(4) 0.0122(3) -0.0099(3) -0.0096(3) Br3 0.0637(4) 0.0457(4) 0.0792(5) -0.0009(3) 0.0160(3) -0.0034(3) Br4 0.0408(3) 0.0637(4) 0.0668(4) -0.0068(3) 0.0109(3) 0.0023(3) Zn1 0.0339(3) 0.0442(4) 0.0488(3) 0.0029(3) 0.0046(3) -0.0017(3) N1 0.038(2) 0.042(2) 0.049(2) 0.0030(19) 0.0021(19) 0.0017(19) N2 0.033(2) 0.043(2) 0.046(2) 0.0040(19) 0.0045(18) 0.0011(19) N3 0.038(2) 0.045(3) 0.049(2) 0.001(2) 0.0053(19) -0.001(2) N4 0.040(2) 0.046(3) 0.043(2) 0.0063(19) 0.0029(18) -0.001(2) C1 0.050(3) 0.052(3) 0.047(3) 0.008(2) 0.003(2) -0.001(3) C2 0.047(3) 0.067(4) 0.057(3) 0.007(3) -0.008(3) -0.003(3) C3 0.042(3) 0.064(4) 0.054(3) 0.006(3) -0.002(3) -0.010(3) C4 0.035(3) 0.045(3) 0.056(3) -0.002(2) 0.000(2) -0.003(2) C5 0.039(3) 0.040(3) 0.046(3) -0.001(2) 0.007(2) 0.003(2) C6 0.039(3) 0.039(3) 0.043(3) -0.003(2) 0.007(2) -0.002(2) C7 0.045(3) 0.043(3) 0.051(3) 0.004(2) 0.004(2) -0.001(2) C8 0.053(3) 0.043(3) 0.051(3) 0.004(2) 0.001(3) 0.004(3) C9 0.034(2) 0.044(3) 0.048(3) 0.001(2) -0.002(2) 0.006(2) C10 0.049(3) 0.038(3) 0.057(3) -0.003(2) 0.006(3) 0.001(2) C11 0.049(3) 0.049(4) 0.076(4) -0.004(3) 0.010(3) 0.009(3) C12 0.042(3) 0.058(4) 0.068(4) 0.003(3) 0.014(3) 0.003(3) C13 0.039(3) 0.047(3) 0.047(3) 0.003(2) 0.006(2) 0.004(2) C14 0.039(3) 0.050(3) 0.046(3) 0.005(2) 0.005(2) -0.002(2) C15 0.033(3) 0.048(3) 0.050(3) 0.002(2) 0.005(2) -0.002(2) C16 0.051(3) 0.042(3) 0.054(3) 0.007(2) 0.008(3) -0.006(3) C17 0.049(3) 0.053(4) 0.055(3) 0.002(3) 0.004(3) 0.003(3) C18 0.036(3) 0.055(3) 0.048(3) 0.003(2) -0.001(2) 0.007(2) C19 0.037(3) 0.052(3) 0.048(3) 0.002(2) 0.000(2) -0.005(2) C20 0.050(3) 0.053(3) 0.052(3) 0.001(3) 0.001(3) -0.008(3) C21 0.061(4) 0.058(4) 0.059(3) 0.006(3) -0.003(3) -0.020(3) C22 0.051(4) 0.072(5) 0.064(4) 0.021(3) -0.001(3) -0.019(3) C23 0.048(3) 0.068(4) 0.065(4) 0.014(3) 0.016(3) -0.005(3) C24 0.043(3) 0.053(4) 0.068(4) 0.001(3) 0.013(3) -0.005(3) C25 0.073(5) 0.053(4) 0.081(5) -0.018(3) 0.019(4) -0.012(3) C26 0.062(4) 0.093(6) 0.089(5) 0.019(5) 0.000(4) -0.038(4) C27 0.074(5) 0.064(5) 0.117(7) -0.017(5) 0.047(5) 0.001(4) C28 0.039(3) 0.049(3) 0.054(3) -0.001(2) 0.011(2) -0.001(2) C29 0.044(3) 0.041(3) 0.057(3) 0.002(2) 0.012(2) 0.001(2) C30 0.064(4) 0.048(3) 0.052(3) 0.002(3) 0.018(3) -0.001(3) C31 0.052(3) 0.041(3) 0.066(4) -0.005(3) 0.020(3) -0.004(3) C32 0.043(3) 0.061(4) 0.064(4) -0.001(3) 0.004(3) -0.004(3) C33 0.042(3) 0.070(4) 0.058(3) 0.001(3) 0.003(3) -0.008(3) C34 0.051(3) 0.065(4) 0.051(3) -0.004(3) 0.005(3) 0.001(3) C35 0.057(4) 0.060(4) 0.094(5) -0.010(4) 0.027(4) -0.011(3) C36 0.056(4) 0.120(7) 0.066(4) 0.025(4) -0.010(3) -0.019(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 Br1 C1 1.878(6) . ? Br2 C9 1.889(5) . ? Br3 C10 1.879(6) . ? Br4 C18 1.886(6) . ? Zn1 N1 1.974(5) . ? Zn1 N4 1.975(5) . ? Zn1 N2 1.976(4) . ? Zn1 N3 1.990(5) . ? N1 C1 1.327(7) . ? N1 C4 1.411(7) . ? N2 C9 1.330(7) . ? N2 C6 1.403(7) . ? N3 C10 1.325(7) . ? N3 C13 1.407(7) . ? N4 C18 1.332(8) . ? N4 C15 1.418(7) . ? C1 C2 1.413(8) . ? C2 C3 1.383(9) . ? C2 H2 0.9500 . ? C3 C4 1.422(8) . ? C3 H3 0.9500 . ? C4 C5 1.395(8) . ? C5 C6 1.401(7) . ? C5 C19 1.519(8) . ? C6 C7 1.411(8) . ? C7 C8 1.395(8) . ? C7 H7 0.9500 . ? C8 C9 1.398(8) . ? C8 H8 0.9500 . ? C10 C11 1.404(8) . ? C11 C12 1.392(9) . ? C11 H11 0.9500 . ? C12 C13 1.417(8) . ? C12 H12 0.9500 . ? C13 C14 1.398(8) . ? C14 C15 1.395(8) . ? C14 C28 1.520(8) . ? C15 C16 1.416(8) . ? C16 C17 1.399(9) . ? C16 H16 0.9500 . ? C17 C18 1.401(9) . ? C17 H17 0.9500 . ? C19 C20 1.383(9) . ? C19 C24 1.418(9) . ? C20 C21 1.420(9) . ? C20 C25 1.517(9) . ? C21 C22 1.367(11) . ? C21 H21 0.9500 . ? C22 C23 1.387(10) . ? C22 C26 1.531(9) . ? C23 C24 1.394(9) . ? C23 H23 0.9500 . ? C24 C27 1.498(10) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.398(8) . ? C28 C33 1.404(8) . ? C29 C30 1.394(9) . ? C29 C34 1.494(9) . ? C30 C31 1.400(9) . ? C30 H30 0.9500 . ? C31 C32 1.365(9) . ? C31 C35 1.522(9) . ? C32 C33 1.405(9) . ? C32 H32 0.9500 . ? C33 C36 1.490(10) . ? 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 . ? 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 Zn1 N4 113.76(19) . . ? N1 Zn1 N2 94.95(19) . . ? N4 Zn1 N2 125.44(19) . . ? N1 Zn1 N3 117.98(19) . . ? N4 Zn1 N3 94.7(2) . . ? N2 Zn1 N3 111.87(19) . . ? C1 N1 C4 105.2(5) . . ? C1 N1 Zn1 130.7(4) . . ? C4 N1 Zn1 123.9(4) . . ? C9 N2 C6 104.7(4) . . ? C9 N2 Zn1 129.3(4) . . ? C6 N2 Zn1 124.2(3) . . ? C10 N3 C13 106.0(5) . . ? C10 N3 Zn1 130.0(4) . . ? C13 N3 Zn1 124.0(4) . . ? C18 N4 C15 104.4(5) . . ? C18 N4 Zn1 130.8(4) . . ? C15 N4 Zn1 124.4(4) . . ? N1 C1 C2 113.7(5) . . ? N1 C1 Br1 119.5(4) . . ? C2 C1 Br1 126.7(5) . . ? C3 C2 C1 104.6(5) . . ? C3 C2 H2 127.7 . . ? C1 C2 H2 127.7 . . ? C2 C3 C4 107.8(5) . . ? C2 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? C5 C4 N1 124.3(5) . . ? C5 C4 C3 127.1(5) . . ? N1 C4 C3 108.6(5) . . ? C4 C5 C6 127.8(5) . . ? C4 C5 C19 115.8(5) . . ? C6 C5 C19 116.4(5) . . ? C5 C6 N2 123.8(5) . . ? C5 C6 C7 127.0(5) . . ? N2 C6 C7 109.2(5) . . ? C8 C7 C6 107.5(5) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? C7 C8 C9 104.2(5) . . ? C7 C8 H8 127.9 . . ? C9 C8 H8 127.9 . . ? N2 C9 C8 114.4(5) . . ? N2 C9 Br2 119.1(4) . . ? C8 C9 Br2 126.5(4) . . ? N3 C10 C11 113.5(5) . . ? N3 C10 Br3 121.1(4) . . ? C11 C10 Br3 125.4(5) . . ? C12 C11 C10 104.4(5) . . ? C12 C11 H11 127.8 . . ? C10 C11 H11 127.8 . . ? C11 C12 C13 108.1(6) . . ? C11 C12 H12 125.9 . . ? C13 C12 H12 125.9 . . ? C14 C13 N3 124.9(5) . . ? C14 C13 C12 127.2(6) . . ? N3 C13 C12 107.9(5) . . ? C15 C14 C13 127.6(5) . . ? C15 C14 C28 117.7(5) . . ? C13 C14 C28 114.7(5) . . ? C14 C15 C16 126.9(5) . . ? C14 C15 N4 124.3(5) . . ? C16 C15 N4 108.7(5) . . ? C17 C16 C15 108.1(5) . . ? C17 C16 H16 126.0 . . ? C15 C16 H16 126.0 . . ? C16 C17 C18 103.9(6) . . ? C16 C17 H17 128.1 . . ? C18 C17 H17 128.1 . . ? N4 C18 C17 114.9(5) . . ? N4 C18 Br4 119.0(4) . . ? C17 C18 Br4 126.1(5) . . ? C20 C19 C24 120.6(6) . . ? C20 C19 C5 120.7(5) . . ? C24 C19 C5 118.7(5) . . ? C19 C20 C21 118.7(6) . . ? C19 C20 C25 121.6(6) . . ? C21 C20 C25 119.7(6) . . ? C22 C21 C20 121.6(7) . . ? C22 C21 H21 119.2 . . ? C20 C21 H21 119.2 . . ? C21 C22 C23 118.9(6) . . ? C21 C22 C26 120.8(7) . . ? C23 C22 C26 120.3(7) . . ? C22 C23 C24 122.1(7) . . ? C22 C23 H23 119.0 . . ? C24 C23 H23 119.0 . . ? C23 C24 C19 118.1(6) . . ? C23 C24 C27 119.9(6) . . ? C19 C24 C27 122.0(6) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 121.4(6) . . ? C29 C28 C14 119.0(5) . . ? C33 C28 C14 119.5(5) . . ? C30 C29 C28 118.2(6) . . ? C30 C29 C34 120.6(6) . . ? C28 C29 C34 121.1(5) . . ? C29 C30 C31 121.9(6) . . ? C29 C30 H30 119.1 . . ? C31 C30 H30 119.1 . . ? C32 C31 C30 118.0(6) . . ? C32 C31 C35 121.1(6) . . ? C30 C31 C35 120.9(6) . . ? C31 C32 C33 123.1(6) . . ? C31 C32 H32 118.5 . . ? C33 C32 H32 118.5 . . ? C28 C33 C32 117.3(6) . . ? C28 C33 C36 121.7(6) . . ? C32 C33 C36 121.0(6) . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 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 . . ? 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 N4 Zn1 N1 C1 42.6(6) . . . . ? N2 Zn1 N1 C1 174.9(5) . . . . ? N3 Zn1 N1 C1 -67.1(6) . . . . ? N4 Zn1 N1 C4 -131.7(4) . . . . ? N2 Zn1 N1 C4 0.6(5) . . . . ? N3 Zn1 N1 C4 118.6(4) . . . . ? N1 Zn1 N2 C9 170.4(5) . . . . ? N4 Zn1 N2 C9 -65.7(5) . . . . ? N3 Zn1 N2 C9 47.6(5) . . . . ? N1 Zn1 N2 C6 8.5(4) . . . . ? N4 Zn1 N2 C6 132.4(4) . . . . ? N3 Zn1 N2 C6 -114.4(4) . . . . ? N1 Zn1 N3 C10 -64.3(6) . . . . ? N4 Zn1 N3 C10 175.6(5) . . . . ? N2 Zn1 N3 C10 44.2(6) . . . . ? N1 Zn1 N3 C13 117.0(4) . . . . ? N4 Zn1 N3 C13 -3.2(4) . . . . ? N2 Zn1 N3 C13 -134.5(4) . . . . ? N1 Zn1 N4 C18 52.8(5) . . . . ? N2 Zn1 N4 C18 -62.6(5) . . . . ? N3 Zn1 N4 C18 176.3(5) . . . . ? N1 Zn1 N4 C15 -118.7(4) . . . . ? N2 Zn1 N4 C15 125.9(4) . . . . ? N3 Zn1 N4 C15 4.7(4) . . . . ? C4 N1 C1 C2 2.0(7) . . . . ? Zn1 N1 C1 C2 -173.1(4) . . . . ? C4 N1 C1 Br1 -177.3(4) . . . . ? Zn1 N1 C1 Br1 7.6(8) . . . . ? N1 C1 C2 C3 -2.3(8) . . . . ? Br1 C1 C2 C3 176.9(5) . . . . ? C1 C2 C3 C4 1.6(8) . . . . ? C1 N1 C4 C5 177.6(6) . . . . ? Zn1 N1 C4 C5 -6.9(8) . . . . ? C1 N1 C4 C3 -0.9(7) . . . . ? Zn1 N1 C4 C3 174.6(4) . . . . ? C2 C3 C4 C5 -178.9(6) . . . . ? C2 C3 C4 N1 -0.5(7) . . . . ? N1 C4 C5 C6 5.0(9) . . . . ? C3 C4 C5 C6 -176.8(6) . . . . ? N1 C4 C5 C19 -175.1(5) . . . . ? C3 C4 C5 C19 3.1(9) . . . . ? C4 C5 C6 N2 5.6(9) . . . . ? C19 C5 C6 N2 -174.4(5) . . . . ? C4 C5 C6 C7 -172.4(6) . . . . ? C19 C5 C6 C7 7.6(8) . . . . ? C9 N2 C6 C5 -178.1(5) . . . . ? Zn1 N2 C6 C5 -12.5(7) . . . . ? C9 N2 C6 C7 0.2(6) . . . . ? Zn1 N2 C6 C7 165.8(4) . . . . ? C5 C6 C7 C8 178.2(5) . . . . ? N2 C6 C7 C8 0.0(6) . . . . ? C6 C7 C8 C9 -0.1(6) . . . . ? C6 N2 C9 C8 -0.3(6) . . . . ? Zn1 N2 C9 C8 -164.9(4) . . . . ? C6 N2 C9 Br2 -178.6(4) . . . . ? Zn1 N2 C9 Br2 16.8(7) . . . . ? C7 C8 C9 N2 0.2(7) . . . . ? C7 C8 C9 Br2 178.4(4) . . . . ? C13 N3 C10 C11 -1.4(7) . . . . ? Zn1 N3 C10 C11 179.7(4) . . . . ? C13 N3 C10 Br3 -180.0(4) . . . . ? Zn1 N3 C10 Br3 1.1(8) . . . . ? N3 C10 C11 C12 0.6(8) . . . . ? Br3 C10 C11 C12 179.1(5) . . . . ? C10 C11 C12 C13 0.5(7) . . . . ? C10 N3 C13 C14 -178.6(5) . . . . ? Zn1 N3 C13 C14 0.4(8) . . . . ? C10 N3 C13 C12 1.7(6) . . . . ? Zn1 N3 C13 C12 -179.4(4) . . . . ? C11 C12 C13 C14 178.9(6) . . . . ? C11 C12 C13 N3 -1.3(7) . . . . ? N3 C13 C14 C15 2.3(9) . . . . ? C12 C13 C14 C15 -178.0(6) . . . . ? N3 C13 C14 C28 -178.1(5) . . . . ? C12 C13 C14 C28 1.6(9) . . . . ? C13 C14 C15 C16 -178.7(6) . . . . ? C28 C14 C15 C16 1.7(9) . . . . ? C13 C14 C15 N4 -0.5(9) . . . . ? C28 C14 C15 N4 179.9(5) . . . . ? C18 N4 C15 C14 -177.2(5) . . . . ? Zn1 N4 C15 C14 -3.8(8) . . . . ? C18 N4 C15 C16 1.3(6) . . . . ? Zn1 N4 C15 C16 174.7(4) . . . . ? C14 C15 C16 C17 177.7(6) . . . . ? N4 C15 C16 C17 -0.8(7) . . . . ? C15 C16 C17 C18 -0.1(7) . . . . ? C15 N4 C18 C17 -1.5(6) . . . . ? Zn1 N4 C18 C17 -174.3(4) . . . . ? C15 N4 C18 Br4 179.4(4) . . . . ? Zn1 N4 C18 Br4 6.7(7) . . . . ? C16 C17 C18 N4 1.0(7) . . . . ? C16 C17 C18 Br4 -180.0(4) . . . . ? C4 C5 C19 C20 86.3(7) . . . . ? C6 C5 C19 C20 -93.8(7) . . . . ? C4 C5 C19 C24 -92.6(7) . . . . ? C6 C5 C19 C24 87.4(7) . . . . ? C24 C19 C20 C21 1.6(9) . . . . ? C5 C19 C20 C21 -177.1(5) . . . . ? C24 C19 C20 C25 -179.0(6) . . . . ? C5 C19 C20 C25 2.2(9) . . . . ? C19 C20 C21 C22 -0.4(10) . . . . ? C25 C20 C21 C22 -179.7(7) . . . . ? C20 C21 C22 C23 -0.6(10) . . . . ? C20 C21 C22 C26 -178.9(6) . . . . ? C21 C22 C23 C24 0.5(11) . . . . ? C26 C22 C23 C24 178.8(7) . . . . ? C22 C23 C24 C19 0.7(10) . . . . ? C22 C23 C24 C27 -178.0(7) . . . . ? C20 C19 C24 C23 -1.8(9) . . . . ? C5 C19 C24 C23 177.0(6) . . . . ? C20 C19 C24 C27 176.9(7) . . . . ? C5 C19 C24 C27 -4.3(10) . . . . ? C15 C14 C28 C29 -95.5(7) . . . . ? C13 C14 C28 C29 84.8(7) . . . . ? C15 C14 C28 C33 87.8(7) . . . . ? C13 C14 C28 C33 -91.8(7) . . . . ? C33 C28 C29 C30 1.7(9) . . . . ? C14 C28 C29 C30 -174.9(5) . . . . ? C33 C28 C29 C34 -179.4(6) . . . . ? C14 C28 C29 C34 4.0(9) . . . . ? C28 C29 C30 C31 0.5(9) . . . . ? C34 C29 C30 C31 -178.4(6) . . . . ? C29 C30 C31 C32 -2.1(10) . . . . ? C29 C30 C31 C35 177.0(6) . . . . ? C30 C31 C32 C33 1.5(10) . . . . ? C35 C31 C32 C33 -177.5(7) . . . . ? C29 C28 C33 C32 -2.2(10) . . . . ? C14 C28 C33 C32 174.4(6) . . . . ? C29 C28 C33 C36 177.9(7) . . . . ? C14 C28 C33 C36 -5.5(11) . . . . ? C31 C32 C33 C28 0.5(11) . . . . ? C31 C32 C33 C36 -179.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.576 _refine_diff_density_min -1.013 _refine_diff_density_rms 0.127 #===END data_shelxl_2H2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H32 N6' _chemical_formula_sum 'C36 H32 N6' _chemical_formula_weight 548.68 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 8.412(4) _cell_length_b 23.757(10) _cell_length_c 7.831(4) _cell_angle_alpha 90.00 _cell_angle_beta 113.799(5) _cell_angle_gamma 90.00 _cell_volume 1431.9(11) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 3797 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 27.61 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9589 _exptl_absorpt_correction_T_max 0.9923 _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.629 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12409 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.52 _reflns_number_total 3094 _reflns_number_gt 2907 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'Il Milione (Burla, et al., 2007)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' _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^)+(0.0300P)^2^+1.2000P] 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 3094 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0728 _refine_ls_wR_factor_ref 0.1520 _refine_ls_wR_factor_gt 0.1483 _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_restrained_S_all 1.173 _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 N1 N 0.6957(2) 0.03307(7) 0.7113(2) 0.0306(4) Uani 1 1 d . . . H1 H 0.6092 0.0183 0.6156 0.037 Uiso 0.50 1 calc PR . . N2 N 0.5452(2) 0.05200(7) 0.3212(2) 0.0308(4) Uani 1 1 d . . . H5 H 0.5279 0.0292 0.4005 0.037 Uiso 0.50 1 calc PR . . N3 N 0.3143(2) 0.02142(7) 0.0312(2) 0.0340(4) Uani 1 1 d . . . C1 C 0.8052(2) 0.07538(8) 0.7068(3) 0.0306(4) Uani 1 1 d . . . C2 C 0.9291(3) 0.08821(9) 0.8949(3) 0.0356(5) Uani 1 1 d . . . H2 H 1.0178 0.1160 0.9298 0.043 Uiso 1 1 calc R . . C3 C 0.1059(3) -0.05333(9) -0.0095(3) 0.0384(5) Uani 1 1 d . . . H3 H 0.0465 -0.0516 -0.1415 0.046 Uiso 1 1 calc R . . C4 C 0.2516(3) -0.01873(9) 0.1060(3) 0.0327(4) Uani 1 1 d . . . C5 C 0.4483(3) 0.05347(8) 0.1329(3) 0.0326(4) Uani 1 1 d . . . C6 C 0.5181(3) 0.09692(9) 0.0555(3) 0.0358(4) Uani 1 1 d . . . H6 H 0.4754 0.1077 -0.0720 0.043 Uiso 1 1 calc R . . C7 C 0.6559(3) 0.11966(8) 0.1977(3) 0.0341(4) Uani 1 1 d . . . H7 H 0.7280 0.1490 0.1870 0.041 Uiso 1 1 calc R . . C8 C 0.6742(2) 0.09192(8) 0.3667(3) 0.0299(4) Uani 1 1 d . . . C9 C 0.7981(2) 0.10270(8) 0.5464(3) 0.0305(4) Uani 1 1 d . . . C10 C 0.9277(2) 0.14837(8) 0.5667(3) 0.0307(4) Uani 1 1 d . . . C11 C 1.0891(3) 0.13520(8) 0.5638(3) 0.0317(4) Uani 1 1 d . . . C12 C 1.2041(3) 0.17905(9) 0.5778(3) 0.0358(4) Uani 1 1 d . . . H12 H 1.3133 0.1704 0.5751 0.043 Uiso 1 1 calc R . . C13 C 1.1640(3) 0.23498(9) 0.5957(3) 0.0364(5) Uani 1 1 d . . . C14 C 1.0049(3) 0.24668(9) 0.6010(3) 0.0371(5) Uani 1 1 d . . . H14 H 0.9760 0.2846 0.6140 0.045 Uiso 1 1 calc R . . C15 C 0.8856(3) 0.20430(8) 0.5876(3) 0.0344(4) Uani 1 1 d . . . C16 C 1.1412(3) 0.07491(9) 0.5519(3) 0.0393(5) Uani 1 1 d . . . H16A H 1.0385 0.0531 0.4742 0.047 Uiso 1 1 calc R . . H16B H 1.1922 0.0586 0.6774 0.047 Uiso 1 1 calc R . . H16C H 1.2268 0.0739 0.4963 0.047 Uiso 1 1 calc R . . C17 C 1.2882(3) 0.28197(10) 0.6065(3) 0.0459(6) Uani 1 1 d . . . H17A H 1.2794 0.3116 0.6892 0.055 Uiso 1 1 calc R . . H17B H 1.2587 0.2975 0.4815 0.055 Uiso 1 1 calc R . . H17C H 1.4072 0.2673 0.6557 0.055 Uiso 1 1 calc R . . C18 C 0.7153(3) 0.21930(10) 0.5970(4) 0.0452(6) Uani 1 1 d . . . H18A H 0.7094 0.2020 0.7079 0.054 Uiso 1 1 calc R . . H18B H 0.6193 0.2054 0.4850 0.054 Uiso 1 1 calc R . . H18C H 0.7065 0.2603 0.6042 0.054 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 N1 0.0296(8) 0.0291(8) 0.0319(8) -0.0019(6) 0.0112(7) -0.0036(6) N2 0.0317(8) 0.0281(8) 0.0305(8) 0.0001(6) 0.0105(7) -0.0029(6) N3 0.0313(8) 0.0376(9) 0.0319(9) 0.0013(7) 0.0115(7) -0.0019(7) C1 0.0276(9) 0.0296(9) 0.0346(10) -0.0034(8) 0.0124(8) -0.0020(7) C2 0.0309(10) 0.0378(11) 0.0347(11) -0.0060(8) 0.0098(8) -0.0056(8) C3 0.0342(10) 0.0448(12) 0.0317(11) -0.0058(9) 0.0087(8) -0.0062(9) C4 0.0307(9) 0.0374(10) 0.0292(9) -0.0017(8) 0.0113(8) -0.0005(8) C5 0.0340(10) 0.0319(10) 0.0313(10) 0.0014(8) 0.0124(8) 0.0027(8) C6 0.0405(11) 0.0327(10) 0.0345(10) 0.0052(8) 0.0153(9) 0.0006(8) C7 0.0358(10) 0.0279(9) 0.0404(11) 0.0042(8) 0.0173(9) -0.0001(8) C8 0.0307(9) 0.0261(9) 0.0342(10) -0.0011(7) 0.0145(8) 0.0002(7) C9 0.0298(9) 0.0246(9) 0.0373(10) -0.0026(7) 0.0137(8) -0.0017(7) C10 0.0292(9) 0.0293(9) 0.0322(10) -0.0015(7) 0.0108(8) -0.0031(7) C11 0.0310(9) 0.0354(10) 0.0275(9) -0.0004(8) 0.0106(8) 0.0010(8) C12 0.0275(9) 0.0441(11) 0.0358(10) 0.0027(9) 0.0128(8) -0.0004(8) C13 0.0338(10) 0.0371(11) 0.0342(10) 0.0012(8) 0.0094(8) -0.0079(8) C14 0.0340(10) 0.0296(10) 0.0419(12) -0.0020(8) 0.0095(9) -0.0024(8) C15 0.0312(10) 0.0294(10) 0.0400(11) -0.0035(8) 0.0116(8) -0.0009(8) C16 0.0399(11) 0.0375(11) 0.0396(12) -0.0012(9) 0.0151(9) 0.0056(9) C17 0.0385(12) 0.0469(13) 0.0483(13) 0.0011(10) 0.0134(10) -0.0140(10) C18 0.0353(11) 0.0365(11) 0.0651(16) -0.0092(10) 0.0217(11) -0.0006(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 N1 C4 1.359(3) 3_656 ? N1 C1 1.373(2) . ? N1 H1 0.8800 . ? N2 C5 1.367(3) . ? N2 C8 1.375(2) . ? N2 H5 0.8800 . ? N3 C5 1.327(3) . ? N3 C4 1.334(3) . ? C1 C9 1.394(3) . ? C1 C2 1.452(3) . ? C2 C3 1.339(3) 3_656 ? C2 H2 0.9500 . ? C3 C2 1.339(3) 3_656 ? C3 C4 1.450(3) . ? C3 H3 0.9500 . ? C4 N1 1.359(3) 3_656 ? C5 C6 1.437(3) . ? C6 C7 1.354(3) . ? C6 H6 0.9500 . ? C7 C8 1.430(3) . ? C7 H7 0.9500 . ? C8 C9 1.396(3) . ? C9 C10 1.500(3) . ? C10 C15 1.402(3) . ? C10 C11 1.402(3) . ? C11 C12 1.396(3) . ? C11 C16 1.512(3) . ? C12 C13 1.392(3) . ? C12 H12 0.9500 . ? C13 C14 1.384(3) . ? C13 C17 1.508(3) . ? C14 C15 1.396(3) . ? C14 H14 0.9500 . ? C15 C18 1.506(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 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 C4 N1 C1 105.86(16) 3_656 . ? C4 N1 H1 127.1 3_656 . ? C1 N1 H1 127.1 . . ? C5 N2 C8 109.08(16) . . ? C5 N2 H5 125.5 . . ? C8 N2 H5 125.5 . . ? C5 N3 C4 122.51(18) . . ? N1 C1 C9 125.34(18) . . ? N1 C1 C2 109.99(17) . . ? C9 C1 C2 124.66(18) . . ? C3 C2 C1 106.76(18) 3_656 . ? C3 C2 H2 126.6 3_656 . ? C1 C2 H2 126.6 . . ? C2 C3 C4 106.96(19) 3_656 . ? C2 C3 H3 126.5 3_656 . ? C4 C3 H3 126.5 . . ? N3 C4 N1 128.50(18) . 3_656 ? N3 C4 C3 121.06(19) . . ? N1 C4 C3 110.42(18) 3_656 . ? N3 C5 N2 128.69(18) . . ? N3 C5 C6 123.49(19) . . ? N2 C5 C6 107.82(17) . . ? C7 C6 C5 107.43(19) . . ? C7 C6 H6 126.3 . . ? C5 C6 H6 126.3 . . ? C6 C7 C8 108.29(18) . . ? C6 C7 H7 125.9 . . ? C8 C7 H7 125.9 . . ? N2 C8 C9 125.32(18) . . ? N2 C8 C7 107.39(17) . . ? C9 C8 C7 127.30(18) . . ? C1 C9 C8 124.48(18) . . ? C1 C9 C10 118.43(17) . . ? C8 C9 C10 117.05(17) . . ? C15 C10 C11 120.38(18) . . ? C15 C10 C9 119.37(17) . . ? C11 C10 C9 120.25(18) . . ? C12 C11 C10 118.49(18) . . ? C12 C11 C16 120.20(18) . . ? C10 C11 C16 121.29(18) . . ? C13 C12 C11 122.16(19) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C14 C13 C12 118.12(18) . . ? C14 C13 C17 120.4(2) . . ? C12 C13 C17 121.5(2) . . ? C13 C14 C15 121.87(19) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C14 C15 C10 118.97(19) . . ? C14 C15 C18 119.67(19) . . ? C10 C15 C18 121.36(18) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 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 C4 N1 C1 C9 179.92(19) 3_656 . . . ? C4 N1 C1 C2 -0.8(2) 3_656 . . . ? N1 C1 C2 C3 0.6(2) . . . 3_656 ? C9 C1 C2 C3 179.85(19) . . . 3_656 ? C5 N3 C4 N1 2.0(3) . . . 3_656 ? C5 N3 C4 C3 -179.44(19) . . . . ? C2 C3 C4 N3 -178.36(19) 3_656 . . . ? C2 C3 C4 N1 0.4(2) 3_656 . . 3_656 ? C4 N3 C5 N2 0.9(3) . . . . ? C4 N3 C5 C6 179.96(19) . . . . ? C8 N2 C5 N3 178.5(2) . . . . ? C8 N2 C5 C6 -0.7(2) . . . . ? N3 C5 C6 C7 -178.27(19) . . . . ? N2 C5 C6 C7 1.0(2) . . . . ? C5 C6 C7 C8 -0.9(2) . . . . ? C5 N2 C8 C9 179.85(18) . . . . ? C5 N2 C8 C7 0.1(2) . . . . ? C6 C7 C8 N2 0.5(2) . . . . ? C6 C7 C8 C9 -179.22(19) . . . . ? N1 C1 C9 C8 2.0(3) . . . . ? C2 C1 C9 C8 -177.12(18) . . . . ? N1 C1 C9 C10 179.73(17) . . . . ? C2 C1 C9 C10 0.6(3) . . . . ? N2 C8 C9 C1 -2.0(3) . . . . ? C7 C8 C9 C1 177.64(19) . . . . ? N2 C8 C9 C10 -179.73(17) . . . . ? C7 C8 C9 C10 -0.1(3) . . . . ? C1 C9 C10 C15 -91.7(2) . . . . ? C8 C9 C10 C15 86.1(2) . . . . ? C1 C9 C10 C11 88.6(2) . . . . ? C8 C9 C10 C11 -93.6(2) . . . . ? C15 C10 C11 C12 -1.4(3) . . . . ? C9 C10 C11 C12 178.24(18) . . . . ? C15 C10 C11 C16 176.62(19) . . . . ? C9 C10 C11 C16 -3.7(3) . . . . ? C10 C11 C12 C13 0.4(3) . . . . ? C16 C11 C12 C13 -177.68(19) . . . . ? C11 C12 C13 C14 0.5(3) . . . . ? C11 C12 C13 C17 -178.6(2) . . . . ? C12 C13 C14 C15 -0.4(3) . . . . ? C17 C13 C14 C15 178.7(2) . . . . ? C13 C14 C15 C10 -0.6(3) . . . . ? C13 C14 C15 C18 179.1(2) . . . . ? C11 C10 C15 C14 1.5(3) . . . . ? C9 C10 C15 C14 -178.14(19) . . . . ? C11 C10 C15 C18 -178.1(2) . . . . ? C9 C10 C15 C18 2.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.274 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.053 #===END data_shelxl_2Pd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 N6 Pd' _chemical_formula_sum 'C36 H30 N6 Pd' _chemical_formula_weight 653.06 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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P -3' _symmetry_space_group_name_Hall '-P 3' _symmetry_Int_Tables_number 147 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 15.384(5) _cell_length_b 15.384(5) _cell_length_c 11.304(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2317.1(12) _cell_formula_units_Z 3 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 6187 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 27.61 _exptl_crystal_description platelet _exptl_crystal_colour purple _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1002 _exptl_absorpt_coefficient_mu 0.636 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8081 _exptl_absorpt_correction_T_max 0.9874 _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.629 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18116 _diffrn_reflns_av_R_equivalents 0.0861 _diffrn_reflns_av_sigmaI/netI 0.0883 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.51 _reflns_number_total 3520 _reflns_number_gt 2339 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'Il Milione (Burla, et al., 2007)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' _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^)+(0.0200P)^2^+0.1000P] 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 3520 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0673 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 Pd1 Pd 0.0000 0.5000 0.5000 0.02778(13) Uani 1 2 d S . . N1 N 0.00305(19) 0.4578(2) 0.3354(2) 0.0280(6) Uani 1 1 d . . . N2 N 0.10394(19) 0.63950(19) 0.4582(2) 0.0286(6) Uani 1 1 d . . . N3 N 0.1291(2) 0.6169(2) 0.2515(2) 0.0346(7) Uani 1 1 d . . . C1 C -0.0502(2) 0.3631(2) 0.2893(3) 0.0302(8) Uani 1 1 d . . . C2 C -0.0225(3) 0.3663(3) 0.1661(3) 0.0365(9) Uani 1 1 d . . . H2 H -0.0480 0.3110 0.1131 0.044 Uiso 1 1 calc R . . C3 C 0.0460(3) 0.4619(3) 0.1409(3) 0.0365(9) Uani 1 1 d . . . H3 H 0.0775 0.4869 0.0666 0.044 Uiso 1 1 calc R . . C4 C 0.0623(3) 0.5184(3) 0.2462(3) 0.0303(8) Uani 1 1 d . . . C5 C 0.1467(2) 0.6701(3) 0.3500(3) 0.0338(8) Uani 1 1 d . . . C6 C 0.2193(3) 0.7761(3) 0.3548(3) 0.0397(9) Uani 1 1 d . . . H6 H 0.2601 0.8163 0.2914 0.048 Uiso 1 1 calc R . . C7 C 0.2184(3) 0.8070(3) 0.4651(3) 0.0393(9) Uani 1 1 d . . . H7 H 0.2588 0.8733 0.4945 0.047 Uiso 1 1 calc R . . C8 C 0.1449(2) 0.7215(2) 0.5312(3) 0.0306(8) Uani 1 1 d . . . C9 C 0.1193(2) 0.7223(2) 0.6495(3) 0.0309(8) Uani 1 1 d . . . C10 C 0.1641(2) 0.8218(2) 0.7115(3) 0.0306(8) Uani 1 1 d . . . C11 C 0.1162(3) 0.8782(3) 0.7000(3) 0.0378(9) Uani 1 1 d . . . C12 C 0.1526(3) 0.9666(3) 0.7644(3) 0.0440(10) Uani 1 1 d . . . H12 H 0.1187 1.0038 0.7594 0.053 Uiso 1 1 calc R . . C13 C 0.2370(3) 1.0021(3) 0.8357(3) 0.0435(10) Uani 1 1 d . . . C14 C 0.2855(3) 0.9469(3) 0.8409(3) 0.0386(9) Uani 1 1 d . . . H14 H 0.3447 0.9715 0.8874 0.046 Uiso 1 1 calc R . . C15 C 0.2510(3) 0.8571(3) 0.7810(3) 0.0367(9) Uani 1 1 d . . . C16 C 0.0260(3) 0.8432(3) 0.6215(4) 0.0471(10) Uani 1 1 d . . . H16A H -0.0237 0.7737 0.6413 0.057 Uiso 1 1 calc R . . H16B H 0.0463 0.8468 0.5386 0.057 Uiso 1 1 calc R . . H16C H -0.0034 0.8862 0.6333 0.057 Uiso 1 1 calc R . . C17 C 0.2745(3) 1.0991(3) 0.9046(3) 0.0575(12) Uani 1 1 d . . . H17A H 0.2286 1.0881 0.9704 0.069 Uiso 1 1 calc R . . H17B H 0.2773 1.1512 0.8522 0.069 Uiso 1 1 calc R . . H17C H 0.3417 1.1206 0.9357 0.069 Uiso 1 1 calc R . . C18 C 0.3068(3) 0.8006(3) 0.7888(4) 0.0485(10) Uani 1 1 d . . . H18A H 0.2665 0.7382 0.8332 0.058 Uiso 1 1 calc R . . H18B H 0.3708 0.8419 0.8294 0.058 Uiso 1 1 calc R . . H18C H 0.3193 0.7846 0.7089 0.058 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 Pd1 0.0265(2) 0.0269(2) 0.0266(2) 0.00020(15) 0.00070(16) 0.01081(17) N1 0.0288(16) 0.0262(15) 0.0252(15) -0.0001(12) -0.0012(12) 0.0108(13) N2 0.0282(15) 0.0271(15) 0.0247(15) 0.0003(12) 0.0008(12) 0.0096(13) N3 0.0332(17) 0.0349(17) 0.0313(17) 0.0023(14) 0.0037(14) 0.0137(15) C1 0.0322(19) 0.0299(19) 0.0282(19) -0.0016(15) -0.0057(15) 0.0154(16) C2 0.042(2) 0.039(2) 0.027(2) -0.0032(17) -0.0027(17) 0.0193(18) C3 0.042(2) 0.039(2) 0.0249(19) 0.0014(16) 0.0019(17) 0.0176(19) C4 0.032(2) 0.031(2) 0.0252(19) 0.0014(15) 0.0015(15) 0.0141(16) C5 0.031(2) 0.030(2) 0.034(2) -0.0022(16) 0.0011(16) 0.0106(16) C6 0.039(2) 0.030(2) 0.036(2) 0.0046(17) 0.0068(18) 0.0064(17) C7 0.035(2) 0.028(2) 0.040(2) 0.0020(17) 0.0029(18) 0.0048(17) C8 0.0277(19) 0.0259(18) 0.030(2) 0.0003(15) -0.0013(15) 0.0072(15) C9 0.0313(19) 0.0289(19) 0.032(2) -0.0022(16) -0.0052(16) 0.0150(16) C10 0.032(2) 0.0279(19) 0.028(2) 0.0001(15) 0.0025(15) 0.0120(16) C11 0.043(2) 0.034(2) 0.037(2) 0.0041(17) 0.0038(18) 0.0203(19) C12 0.057(3) 0.035(2) 0.041(2) -0.0011(18) -0.001(2) 0.024(2) C13 0.056(3) 0.031(2) 0.035(2) 0.0011(17) 0.0013(19) 0.016(2) C14 0.041(2) 0.033(2) 0.030(2) -0.0044(16) -0.0083(17) 0.0105(18) C15 0.039(2) 0.033(2) 0.033(2) 0.0028(17) -0.0017(17) 0.0148(18) C16 0.048(2) 0.046(2) 0.051(3) -0.008(2) -0.011(2) 0.027(2) C17 0.088(3) 0.045(3) 0.040(2) -0.009(2) -0.012(2) 0.034(3) C18 0.047(2) 0.047(2) 0.053(3) -0.007(2) -0.013(2) 0.024(2) _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 Pd1 N1 1.979(3) 4_566 ? Pd1 N1 1.979(3) . ? Pd1 N2 1.989(3) . ? Pd1 N2 1.989(3) 4_566 ? N1 C4 1.366(4) . ? N1 C1 1.368(4) . ? N2 C5 1.356(4) . ? N2 C8 1.370(4) . ? N3 C5 1.327(4) . ? N3 C4 1.342(4) . ? C1 C9 1.393(4) 4_566 ? C1 C2 1.449(4) . ? C2 C3 1.343(4) . ? C2 H2 0.9500 . ? C3 C4 1.421(4) . ? C3 H3 0.9500 . ? C5 C6 1.445(4) . ? C6 C7 1.337(5) . ? C6 H6 0.9500 . ? C7 C8 1.442(4) . ? C7 H7 0.9500 . ? C8 C9 1.395(4) . ? C9 C1 1.393(4) 4_566 ? C9 C10 1.501(4) . ? C10 C11 1.398(4) . ? C10 C15 1.404(4) . ? C11 C12 1.389(5) . ? C11 C16 1.502(5) . ? C12 C13 1.387(5) . ? C12 H12 0.9500 . ? C13 C14 1.384(5) . ? C13 C17 1.518(5) . ? C14 C15 1.385(4) . ? C14 H14 0.9500 . ? C15 C18 1.498(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 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 N1 Pd1 N1 180.0 4_566 . ? N1 Pd1 N2 90.42(11) 4_566 . ? N1 Pd1 N2 89.58(11) . . ? N1 Pd1 N2 89.58(11) 4_566 4_566 ? N1 Pd1 N2 90.42(11) . 4_566 ? N2 Pd1 N2 180.0 . 4_566 ? C4 N1 C1 106.6(3) . . ? C4 N1 Pd1 125.9(2) . . ? C1 N1 Pd1 127.5(2) . . ? C5 N2 C8 107.7(3) . . ? C5 N2 Pd1 125.3(2) . . ? C8 N2 Pd1 127.0(2) . . ? C5 N3 C4 122.6(3) . . ? N1 C1 C9 125.7(3) . 4_566 ? N1 C1 C2 108.7(3) . . ? C9 C1 C2 125.6(3) 4_566 . ? C3 C2 C1 107.3(3) . . ? C3 C2 H2 126.4 . . ? C1 C2 H2 126.4 . . ? C2 C3 C4 107.1(3) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? N3 C4 N1 127.7(3) . . ? N3 C4 C3 122.0(3) . . ? N1 C4 C3 110.3(3) . . ? N3 C5 N2 129.0(3) . . ? N3 C5 C6 122.1(3) . . ? N2 C5 C6 108.9(3) . . ? C7 C6 C5 107.3(3) . . ? C7 C6 H6 126.3 . . ? C5 C6 H6 126.3 . . ? C6 C7 C8 107.5(3) . . ? C6 C7 H7 126.2 . . ? C8 C7 H7 126.2 . . ? N2 C8 C9 125.7(3) . . ? N2 C8 C7 108.5(3) . . ? C9 C8 C7 125.8(3) . . ? C1 C9 C8 123.6(3) 4_566 . ? C1 C9 C10 118.3(3) 4_566 . ? C8 C9 C10 118.0(3) . . ? C11 C10 C15 120.5(3) . . ? C11 C10 C9 118.2(3) . . ? C15 C10 C9 121.3(3) . . ? C12 C11 C10 118.6(3) . . ? C12 C11 C16 120.6(3) . . ? C10 C11 C16 120.8(3) . . ? C13 C12 C11 122.0(4) . . ? C13 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? C14 C13 C12 117.9(4) . . ? C14 C13 C17 121.7(4) . . ? C12 C13 C17 120.4(4) . . ? C13 C14 C15 122.4(3) . . ? C13 C14 H14 118.8 . . ? C15 C14 H14 118.8 . . ? C14 C15 C10 118.4(3) . . ? C14 C15 C18 120.3(3) . . ? C10 C15 C18 121.3(3) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 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 N1 Pd1 N1 C4 -88(5) 4_566 . . . ? N2 Pd1 N1 C4 0.2(3) . . . . ? N2 Pd1 N1 C4 -179.8(3) 4_566 . . . ? N1 Pd1 N1 C1 89(5) 4_566 . . . ? N2 Pd1 N1 C1 177.9(3) . . . . ? N2 Pd1 N1 C1 -2.1(3) 4_566 . . . ? N1 Pd1 N2 C5 179.5(3) 4_566 . . . ? N1 Pd1 N2 C5 -0.5(3) . . . . ? N2 Pd1 N2 C5 41(4) 4_566 . . . ? N1 Pd1 N2 C8 -0.8(3) 4_566 . . . ? N1 Pd1 N2 C8 179.2(3) . . . . ? N2 Pd1 N2 C8 -139(4) 4_566 . . . ? C4 N1 C1 C9 179.5(3) . . . 4_566 ? Pd1 N1 C1 C9 1.4(5) . . . 4_566 ? C4 N1 C1 C2 -0.3(4) . . . . ? Pd1 N1 C1 C2 -178.4(2) . . . . ? N1 C1 C2 C3 -0.1(4) . . . . ? C9 C1 C2 C3 -179.9(3) 4_566 . . . ? C1 C2 C3 C4 0.5(4) . . . . ? C5 N3 C4 N1 0.2(6) . . . . ? C5 N3 C4 C3 -178.4(3) . . . . ? C1 N1 C4 N3 -178.1(3) . . . . ? Pd1 N1 C4 N3 0.0(5) . . . . ? C1 N1 C4 C3 0.6(4) . . . . ? Pd1 N1 C4 C3 178.7(2) . . . . ? C2 C3 C4 N3 178.1(3) . . . . ? C2 C3 C4 N1 -0.7(4) . . . . ? C4 N3 C5 N2 -0.7(6) . . . . ? C4 N3 C5 C6 179.7(3) . . . . ? C8 N2 C5 N3 -178.8(3) . . . . ? Pd1 N2 C5 N3 0.9(5) . . . . ? C8 N2 C5 C6 0.9(4) . . . . ? Pd1 N2 C5 C6 -179.4(2) . . . . ? N3 C5 C6 C7 179.5(3) . . . . ? N2 C5 C6 C7 -0.3(4) . . . . ? C5 C6 C7 C8 -0.4(4) . . . . ? C5 N2 C8 C9 178.4(3) . . . . ? Pd1 N2 C8 C9 -1.4(5) . . . . ? C5 N2 C8 C7 -1.1(4) . . . . ? Pd1 N2 C8 C7 179.1(2) . . . . ? C6 C7 C8 N2 1.0(4) . . . . ? C6 C7 C8 C9 -178.5(3) . . . . ? N2 C8 C9 C1 2.9(6) . . . 4_566 ? C7 C8 C9 C1 -177.7(3) . . . 4_566 ? N2 C8 C9 C10 -173.3(3) . . . . ? C7 C8 C9 C10 6.1(5) . . . . ? C1 C9 C10 C11 -91.3(4) 4_566 . . . ? C8 C9 C10 C11 85.1(4) . . . . ? C1 C9 C10 C15 87.7(4) 4_566 . . . ? C8 C9 C10 C15 -95.8(4) . . . . ? C15 C10 C11 C12 -3.9(5) . . . . ? C9 C10 C11 C12 175.1(3) . . . . ? C15 C10 C11 C16 177.2(3) . . . . ? C9 C10 C11 C16 -3.8(5) . . . . ? C10 C11 C12 C13 2.5(5) . . . . ? C16 C11 C12 C13 -178.6(3) . . . . ? C11 C12 C13 C14 0.4(6) . . . . ? C11 C12 C13 C17 180.0(3) . . . . ? C12 C13 C14 C15 -2.1(5) . . . . ? C17 C13 C14 C15 178.4(3) . . . . ? C13 C14 C15 C10 0.7(5) . . . . ? C13 C14 C15 C18 179.5(3) . . . . ? C11 C10 C15 C14 2.4(5) . . . . ? C9 C10 C15 C14 -176.6(3) . . . . ? C11 C10 C15 C18 -176.4(3) . . . . ? C9 C10 C15 C18 4.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 4.155 _refine_diff_density_min -0.961 _refine_diff_density_rms 0.112 #===END data_shelxl_2Pt _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 N6 Pt' _chemical_formula_sum 'C36 H30 N6 Pt' _chemical_formula_weight 741.75 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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P -3' _symmetry_space_group_name_Hall '-P 3' _symmetry_Int_Tables_number 147 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 15.3958(18) _cell_length_b 15.3958(18) _cell_length_c 11.2532(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2310.0(5) _cell_formula_units_Z 3 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 7912 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 27.46 _exptl_crystal_description platelet _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1098 _exptl_absorpt_coefficient_mu 4.591 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3397 _exptl_absorpt_correction_T_max 0.9138 _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method ?\w _diffrn_detector_area_resol_mean 14.629 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27782 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3536 _reflns_number_gt 3476 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_structure_solution 'Il Milione (Burla, et al., 2007)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _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^)+(0.0280P)^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 3536 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0241 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0557 _refine_ls_wR_factor_gt 0.0533 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 Pt1 Pt 0.5000 1.0000 0.5000 0.02013(6) Uani 1 2 d S . . N1 N 0.45446(16) 0.99692(15) 0.33430(18) 0.0213(4) Uani 1 1 d . . . N2 N 0.53532(16) 0.89618(15) 0.45814(18) 0.0228(5) Uani 1 1 d . . . N3 N 0.48688(17) 0.87083(16) 0.2502(2) 0.0270(5) Uani 1 1 d . . . C1 C 0.41271(19) 1.05051(19) 0.2885(2) 0.0227(5) Uani 1 1 d . . . C2 C 0.3879(2) 1.0228(2) 0.1651(2) 0.0288(6) Uani 1 1 d . . . H2 H 0.3582 1.0485 0.1121 0.035 Uiso 1 1 calc R . . C3 C 0.4145(2) 0.9542(2) 0.1388(2) 0.0298(6) Uani 1 1 d . . . H3 H 0.4074 0.9229 0.0639 0.036 Uiso 1 1 calc R . . C4 C 0.45576(19) 0.93702(19) 0.2448(2) 0.0242(6) Uani 1 1 d . . . C5 C 0.5232(2) 0.85281(19) 0.3477(2) 0.0255(6) Uani 1 1 d . . . C6 C 0.5567(2) 0.7808(2) 0.3530(3) 0.0320(6) Uani 1 1 d . . . H6 H 0.5561 0.7400 0.2893 0.038 Uiso 1 1 calc R . . C7 C 0.5890(2) 0.7816(2) 0.4640(3) 0.0303(6) Uani 1 1 d . . . H7 H 0.6152 0.7414 0.4931 0.036 Uiso 1 1 calc R . . C8 C 0.57656(19) 0.85466(19) 0.5309(2) 0.0238(6) Uani 1 1 d . . . C9 C 0.60303(19) 0.88038(19) 0.6489(2) 0.0242(6) Uani 1 1 d . . . C10 C 0.65816(19) 0.83574(18) 0.7117(3) 0.0248(6) Uani 1 1 d . . . C11 C 0.6064(2) 0.7486(2) 0.7801(2) 0.0280(6) Uani 1 1 d . . . C12 C 0.6622(2) 0.7137(2) 0.8409(3) 0.0323(6) Uani 1 1 d . . . H12 H 0.6278 0.6544 0.8873 0.039 Uiso 1 1 calc R . . C13 C 0.7659(2) 0.7628(2) 0.8359(3) 0.0331(7) Uani 1 1 d . . . C14 C 0.8145(2) 0.8477(2) 0.7646(3) 0.0336(7) Uani 1 1 d . . . H14 H 0.8855 0.8815 0.7592 0.040 Uiso 1 1 calc R . . C15 C 0.7627(2) 0.8846(2) 0.7010(3) 0.0286(6) Uani 1 1 d . . . C16 C 0.4938(2) 0.6921(2) 0.7870(3) 0.0390(7) Uani 1 1 d . . . H16A H 0.4711 0.6269 0.8249 0.047 Uiso 1 1 calc R . . H16B H 0.4658 0.6818 0.7066 0.047 Uiso 1 1 calc R . . H16C H 0.4712 0.7308 0.8338 0.047 Uiso 1 1 calc R . . C17 C 0.8252(3) 0.7258(3) 0.9053(3) 0.0462(8) Uani 1 1 d . . . H17A H 0.8379 0.7540 0.9857 0.055 Uiso 1 1 calc R . . H17B H 0.8892 0.7468 0.8652 0.055 Uiso 1 1 calc R . . H17C H 0.7868 0.6524 0.9100 0.055 Uiso 1 1 calc R . . C18 C 0.8182(2) 0.9743(2) 0.6205(3) 0.0374(7) Uani 1 1 d . . . H18A H 0.8153 1.0316 0.6540 0.045 Uiso 1 1 calc R . . H18B H 0.7869 0.9585 0.5418 0.045 Uiso 1 1 calc R . . H18C H 0.8883 0.9911 0.6136 0.045 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 Pt1 0.02189(9) 0.01827(8) 0.02119(9) 0.00006(5) -0.00009(5) 0.01076(6) N1 0.0235(11) 0.0206(11) 0.0196(11) 0.0008(8) 0.0006(9) 0.0109(9) N2 0.0259(11) 0.0214(11) 0.0237(11) 0.0022(9) 0.0018(9) 0.0138(9) N3 0.0329(13) 0.0265(12) 0.0246(12) -0.0024(10) 0.0001(10) 0.0170(10) C1 0.0231(13) 0.0234(13) 0.0222(13) 0.0024(11) 0.0003(11) 0.0121(11) C2 0.0321(15) 0.0338(15) 0.0227(14) 0.0017(12) -0.0028(12) 0.0182(13) C3 0.0373(16) 0.0330(15) 0.0205(14) -0.0013(12) -0.0010(12) 0.0186(13) C4 0.0258(13) 0.0236(13) 0.0217(13) 0.0000(11) 0.0023(11) 0.0112(11) C5 0.0315(14) 0.0245(13) 0.0236(14) -0.0023(11) -0.0001(11) 0.0162(12) C6 0.0460(17) 0.0283(15) 0.0304(16) -0.0051(12) -0.0002(13) 0.0251(14) C7 0.0367(16) 0.0270(14) 0.0348(16) -0.0010(12) -0.0002(13) 0.0217(13) C8 0.0260(13) 0.0218(13) 0.0266(14) 0.0028(11) 0.0014(11) 0.0142(11) C9 0.0238(13) 0.0230(13) 0.0276(14) 0.0036(11) 0.0018(11) 0.0130(11) C10 0.0306(15) 0.0261(14) 0.0235(15) -0.0006(10) -0.0011(11) 0.0184(12) C11 0.0325(15) 0.0310(15) 0.0257(14) 0.0025(12) 0.0023(12) 0.0198(13) C12 0.0435(17) 0.0362(16) 0.0266(15) 0.0077(12) 0.0054(13) 0.0268(14) C13 0.0428(17) 0.0468(18) 0.0249(15) -0.0015(13) -0.0018(13) 0.0338(15) C14 0.0300(15) 0.0443(18) 0.0330(16) -0.0017(14) 0.0003(13) 0.0235(14) C15 0.0305(15) 0.0315(15) 0.0274(15) -0.0005(12) -0.0008(12) 0.0181(13) C16 0.0352(17) 0.0375(17) 0.0451(19) 0.0138(14) 0.0058(14) 0.0187(14) C17 0.057(2) 0.071(2) 0.0338(18) 0.0102(16) 0.0017(15) 0.049(2) C18 0.0308(16) 0.0332(16) 0.0468(19) 0.0046(14) -0.0005(14) 0.0148(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 Pt1 N1 1.984(2) 4_676 ? Pt1 N1 1.984(2) . ? Pt1 N2 1.985(2) 4_676 ? Pt1 N2 1.985(2) . ? N1 C4 1.372(3) . ? N1 C1 1.375(3) . ? N2 C8 1.374(3) . ? N2 C5 1.379(3) . ? N3 C5 1.322(3) . ? N3 C4 1.327(3) . ? C1 C9 1.395(4) 4_676 ? C1 C2 1.447(4) . ? C2 C3 1.341(4) . ? C2 H2 0.9500 . ? C3 C4 1.438(4) . ? C3 H3 0.9500 . ? C5 C6 1.438(4) . ? C6 C7 1.342(4) . ? C6 H6 0.9500 . ? C7 C8 1.443(4) . ? C7 H7 0.9500 . ? C8 C9 1.387(4) . ? C9 C1 1.395(4) 4_676 ? C9 C10 1.508(4) . ? C10 C11 1.400(4) . ? C10 C15 1.401(4) . ? C11 C12 1.399(4) . ? C11 C16 1.502(4) . ? C12 C13 1.385(4) . ? C12 H12 0.9500 . ? C13 C14 1.390(4) . ? C13 C17 1.513(4) . ? C14 C15 1.387(4) . ? C14 H14 0.9500 . ? C15 C18 1.509(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 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 N1 Pt1 N1 180.000(1) 4_676 . ? N1 Pt1 N2 89.63(8) 4_676 4_676 ? N1 Pt1 N2 90.37(8) . 4_676 ? N1 Pt1 N2 90.37(8) 4_676 . ? N1 Pt1 N2 89.63(8) . . ? N2 Pt1 N2 180.0 4_676 . ? C4 N1 C1 107.2(2) . . ? C4 N1 Pt1 125.57(17) . . ? C1 N1 Pt1 127.15(17) . . ? C8 N2 C5 107.1(2) . . ? C8 N2 Pt1 127.54(17) . . ? C5 N2 Pt1 125.34(17) . . ? C5 N3 C4 123.5(2) . . ? N1 C1 C9 125.4(2) . 4_676 ? N1 C1 C2 108.5(2) . . ? C9 C1 C2 126.1(2) 4_676 . ? C3 C2 C1 107.7(2) . . ? C3 C2 H2 126.1 . . ? C1 C2 H2 126.1 . . ? C2 C3 C4 107.4(2) . . ? C2 C3 H3 126.3 . . ? C4 C3 H3 126.3 . . ? N3 C4 N1 128.0(2) . . ? N3 C4 C3 122.8(2) . . ? N1 C4 C3 109.2(2) . . ? N3 C5 N2 128.0(2) . . ? N3 C5 C6 123.3(2) . . ? N2 C5 C6 108.7(2) . . ? C7 C6 C5 107.8(2) . . ? C7 C6 H6 126.1 . . ? C5 C6 H6 126.1 . . ? C6 C7 C8 107.5(2) . . ? C6 C7 H7 126.3 . . ? C8 C7 H7 126.3 . . ? N2 C8 C9 125.2(2) . . ? N2 C8 C7 108.9(2) . . ? C9 C8 C7 126.0(2) . . ? C8 C9 C1 124.3(2) . 4_676 ? C8 C9 C10 118.0(2) . . ? C1 C9 C10 117.6(2) 4_676 . ? C11 C10 C15 120.9(2) . . ? C11 C10 C9 120.9(2) . . ? C15 C10 C9 118.2(2) . . ? C12 C11 C10 118.2(3) . . ? C12 C11 C16 120.3(3) . . ? C10 C11 C16 121.5(2) . . ? C13 C12 C11 122.2(3) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C12 C13 C14 117.9(3) . . ? C12 C13 C17 121.4(3) . . ? C14 C13 C17 120.7(3) . . ? C15 C14 C13 122.3(3) . . ? C15 C14 H14 118.9 . . ? C13 C14 H14 118.8 . . ? C14 C15 C10 118.5(3) . . ? C14 C15 C18 120.5(3) . . ? C10 C15 C18 121.0(2) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 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 N1 Pt1 N1 C4 -29(31) 4_676 . . . ? N2 Pt1 N1 C4 -179.7(2) 4_676 . . . ? N2 Pt1 N1 C4 0.3(2) . . . . ? N1 Pt1 N1 C1 149(31) 4_676 . . . ? N2 Pt1 N1 C1 -2.3(2) 4_676 . . . ? N2 Pt1 N1 C1 177.7(2) . . . . ? N1 Pt1 N2 C8 -0.9(2) 4_676 . . . ? N1 Pt1 N2 C8 179.1(2) . . . . ? N2 Pt1 N2 C8 150(8) 4_676 . . . ? N1 Pt1 N2 C5 179.7(2) 4_676 . . . ? N1 Pt1 N2 C5 -0.3(2) . . . . ? N2 Pt1 N2 C5 -29(8) 4_676 . . . ? C4 N1 C1 C9 179.4(2) . . . 4_676 ? Pt1 N1 C1 C9 1.7(4) . . . 4_676 ? C4 N1 C1 C2 -0.4(3) . . . . ? Pt1 N1 C1 C2 -178.20(17) . . . . ? N1 C1 C2 C3 0.0(3) . . . . ? C9 C1 C2 C3 -179.8(3) 4_676 . . . ? C1 C2 C3 C4 0.4(3) . . . . ? C5 N3 C4 N1 -0.2(4) . . . . ? C5 N3 C4 C3 -178.7(3) . . . . ? C1 N1 C4 N3 -177.9(3) . . . . ? Pt1 N1 C4 N3 -0.1(4) . . . . ? C1 N1 C4 C3 0.7(3) . . . . ? Pt1 N1 C4 C3 178.48(17) . . . . ? C2 C3 C4 N3 178.0(3) . . . . ? C2 C3 C4 N1 -0.7(3) . . . . ? C4 N3 C5 N2 0.3(4) . . . . ? C4 N3 C5 C6 179.9(3) . . . . ? C8 N2 C5 N3 -179.4(3) . . . . ? Pt1 N2 C5 N3 0.1(4) . . . . ? C8 N2 C5 C6 0.9(3) . . . . ? Pt1 N2 C5 C6 -179.61(18) . . . . ? N3 C5 C6 C7 179.8(3) . . . . ? N2 C5 C6 C7 -0.5(3) . . . . ? C5 C6 C7 C8 -0.1(3) . . . . ? C5 N2 C8 C9 178.1(3) . . . . ? Pt1 N2 C8 C9 -1.3(4) . . . . ? C5 N2 C8 C7 -1.0(3) . . . . ? Pt1 N2 C8 C7 179.54(17) . . . . ? C6 C7 C8 N2 0.7(3) . . . . ? C6 C7 C8 C9 -178.4(3) . . . . ? N2 C8 C9 C1 2.9(4) . . . 4_676 ? C7 C8 C9 C1 -178.1(3) . . . 4_676 ? N2 C8 C9 C10 -173.2(2) . . . . ? C7 C8 C9 C10 5.8(4) . . . . ? C8 C9 C10 C11 -95.0(3) . . . . ? C1 C9 C10 C11 88.7(3) 4_676 . . . ? C8 C9 C10 C15 85.9(3) . . . . ? C1 C9 C10 C15 -90.5(3) 4_676 . . . ? C15 C10 C11 C12 2.3(4) . . . . ? C9 C10 C11 C12 -176.9(3) . . . . ? C15 C10 C11 C16 -176.6(3) . . . . ? C9 C10 C11 C16 4.3(4) . . . . ? C10 C11 C12 C13 0.4(4) . . . . ? C16 C11 C12 C13 179.2(3) . . . . ? C11 C12 C13 C14 -2.0(4) . . . . ? C11 C12 C13 C17 178.1(3) . . . . ? C12 C13 C14 C15 1.0(4) . . . . ? C17 C13 C14 C15 -179.1(3) . . . . ? C13 C14 C15 C10 1.5(4) . . . . ? C13 C14 C15 C18 -177.3(3) . . . . ? C11 C10 C15 C14 -3.2(4) . . . . ? C9 C10 C15 C14 175.9(3) . . . . ? C11 C10 C15 C18 175.6(3) . . . . ? C9 C10 C15 C18 -5.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.691 _refine_diff_density_min -2.110 _refine_diff_density_rms 0.100 #===END data_shelxl_4Ni _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H32 N4 Ni' _chemical_formula_sum 'C38 H32 N4 Ni' _chemical_formula_weight 603.39 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 monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 13.345(3) _cell_length_b 13.790(3) _cell_length_c 8.1213(16) _cell_angle_alpha 90.00 _cell_angle_beta 101.114(2) _cell_angle_gamma 90.00 _cell_volume 1466.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 3703 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 27.48 _exptl_crystal_description platelet _exptl_crystal_colour purple _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8733 _exptl_absorpt_correction_T_max 0.9660 _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.629 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11220 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3242 _reflns_number_gt 2669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_structure_solution 'SIR92 (Altomare, et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _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^)+(0.0550P)^2^+0.5000P] 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 3242 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _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 0.5000 0.0000 0.0000 0.01681(13) Uani 1 2 d S . . N1 N 0.37649(12) -0.07091(12) 0.0223(2) 0.0196(3) Uani 1 1 d . . . N2 N 0.54449(12) -0.10726(12) -0.12501(19) 0.0192(3) Uani 1 1 d . . . C1 C 0.34661(15) -0.16126(15) -0.0435(3) 0.0231(4) Uani 1 1 d . . . C2 C 0.25137(16) -0.18913(16) -0.0022(3) 0.0290(5) Uani 1 1 d . . . H2 H 0.2148 -0.2472 -0.0354 0.035 Uiso 1 1 calc R . . C3 C 0.22307(15) -0.11789(16) 0.0923(3) 0.0265(5) Uani 1 1 d . . . H3 H 0.1635 -0.1167 0.1401 0.032 Uiso 1 1 calc R . . C4 C 0.30008(14) -0.04400(15) 0.1074(2) 0.0201(4) Uani 1 1 d . . . C5 C 0.29585(15) 0.04263(15) 0.1911(2) 0.0212(4) Uani 1 1 d . . . C6 C 0.36796(15) 0.11420(14) 0.1920(2) 0.0207(4) Uani 1 1 d . . . C7 C 0.36222(16) 0.20821(15) 0.2680(3) 0.0258(4) Uani 1 1 d . . . H7 H 0.3091 0.2309 0.3210 0.031 Uiso 1 1 calc R . . C8 C 0.44616(17) 0.25754(15) 0.2497(3) 0.0261(5) Uani 1 1 d . . . H8 H 0.4636 0.3217 0.2870 0.031 Uiso 1 1 calc R . . C9 C 0.49568(16) -0.19494(14) -0.1634(2) 0.0223(4) Uani 1 1 d . . . C10 C 0.40252(16) -0.21952(15) -0.1289(3) 0.0247(4) Uani 1 1 d . . . H10 H 0.3748 -0.2809 -0.1665 0.030 Uiso 1 1 calc R . . C11 C 0.21192(15) 0.06131(14) 0.2864(2) 0.0216(4) Uani 1 1 d . . . C12 C 0.11691(15) 0.09598(15) 0.2034(2) 0.0230(4) Uani 1 1 d . . . C13 C 0.04314(16) 0.11906(15) 0.2972(3) 0.0256(4) Uani 1 1 d . . . H13 H -0.0218 0.1412 0.2407 0.031 Uiso 1 1 calc R . . C14 C 0.06173(17) 0.11065(15) 0.4708(3) 0.0271(5) Uani 1 1 d . . . C15 C 0.15632(17) 0.07495(16) 0.5506(3) 0.0276(5) Uani 1 1 d . . . H15 H 0.1700 0.0683 0.6693 0.033 Uiso 1 1 calc R . . C16 C 0.23144(16) 0.04873(16) 0.4615(3) 0.0253(4) Uani 1 1 d . . . C17 C 0.09467(18) 0.11086(18) 0.0154(3) 0.0329(5) Uani 1 1 d . . . H17A H 0.1047 0.0496 -0.0405 0.039 Uiso 1 1 calc R . . H17B H 0.1410 0.1601 -0.0144 0.039 Uiso 1 1 calc R . . H17C H 0.0239 0.1325 -0.0207 0.039 Uiso 1 1 calc R . . C18 C -0.01813(19) 0.13943(18) 0.5696(3) 0.0362(6) Uani 1 1 d . . . H18A H -0.0300 0.0855 0.6422 0.043 Uiso 1 1 calc R . . H18B H -0.0819 0.1552 0.4923 0.043 Uiso 1 1 calc R . . H18C H 0.0055 0.1963 0.6388 0.043 Uiso 1 1 calc R . . C19 C 0.33184(18) 0.00798(18) 0.5534(3) 0.0339(5) Uani 1 1 d . . . H19A H 0.3305 0.0029 0.6734 0.041 Uiso 1 1 calc R . . H19B H 0.3876 0.0510 0.5376 0.041 Uiso 1 1 calc R . . H19C H 0.3425 -0.0565 0.5090 0.041 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 0.01638(19) 0.01721(19) 0.0174(2) -0.00061(13) 0.00469(14) -0.00108(13) N1 0.0190(8) 0.0192(8) 0.0210(8) -0.0016(6) 0.0049(7) -0.0010(6) N2 0.0197(8) 0.0208(8) 0.0172(8) 0.0002(6) 0.0039(6) -0.0009(7) C1 0.0207(10) 0.0225(10) 0.0259(10) -0.0012(8) 0.0038(8) -0.0053(8) C2 0.0238(10) 0.0260(11) 0.0384(12) -0.0028(9) 0.0088(9) -0.0077(9) C3 0.0180(10) 0.0295(11) 0.0330(11) 0.0022(9) 0.0076(9) -0.0017(8) C4 0.0158(9) 0.0237(10) 0.0203(10) 0.0019(8) 0.0024(8) -0.0011(8) C5 0.0196(9) 0.0253(10) 0.0193(9) 0.0029(8) 0.0054(8) 0.0022(8) C6 0.0203(9) 0.0241(10) 0.0185(9) 0.0006(8) 0.0055(8) 0.0017(8) C7 0.0281(11) 0.0251(10) 0.0269(11) -0.0033(9) 0.0117(9) 0.0024(9) C8 0.0321(11) 0.0219(10) 0.0260(11) -0.0058(8) 0.0099(9) -0.0009(9) C9 0.0265(10) 0.0195(9) 0.0217(10) -0.0031(8) 0.0067(8) -0.0027(8) C10 0.0267(10) 0.0211(10) 0.0263(10) -0.0052(8) 0.0055(9) -0.0053(8) C11 0.0209(10) 0.0219(10) 0.0235(10) 0.0000(8) 0.0077(8) -0.0002(8) C12 0.0233(10) 0.0232(10) 0.0237(10) 0.0010(8) 0.0072(8) -0.0002(8) C13 0.0223(10) 0.0235(10) 0.0326(11) 0.0024(9) 0.0094(9) 0.0039(8) C14 0.0305(11) 0.0241(10) 0.0307(11) -0.0027(9) 0.0160(9) -0.0001(9) C15 0.0333(12) 0.0303(11) 0.0212(10) 0.0001(9) 0.0100(9) -0.0014(9) C16 0.0256(10) 0.0270(11) 0.0237(10) 0.0000(9) 0.0060(9) -0.0010(9) C17 0.0317(12) 0.0422(13) 0.0262(11) 0.0060(10) 0.0094(9) 0.0085(10) C18 0.0416(13) 0.0348(12) 0.0382(13) -0.0029(10) 0.0223(11) 0.0061(11) C19 0.0291(12) 0.0464(14) 0.0254(12) 0.0027(10) 0.0030(10) 0.0048(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 N2 1.9502(16) . ? Ni1 N2 1.9502(16) 3_655 ? Ni1 N1 1.9548(16) 3_655 ? Ni1 N1 1.9548(16) . ? N1 C1 1.384(2) . ? N1 C4 1.388(2) . ? N2 C9 1.380(2) . ? N2 C6 1.384(2) 3_655 ? C1 C10 1.372(3) . ? C1 C2 1.428(3) . ? C2 C3 1.345(3) . ? C2 H2 0.9500 . ? C3 C4 1.436(3) . ? C3 H3 0.9500 . ? C4 C5 1.381(3) . ? C5 C6 1.378(3) . ? C5 C11 1.501(3) . ? C6 N2 1.384(2) 3_655 ? C6 C7 1.445(3) . ? C7 C8 1.343(3) . ? C7 H7 0.9500 . ? C8 C9 1.431(3) 3_655 ? C8 H8 0.9500 . ? C9 C10 1.369(3) . ? C9 C8 1.431(3) 3_655 ? C10 H10 0.9500 . ? C11 C12 1.400(3) . ? C11 C16 1.407(3) . ? C12 C13 1.393(3) . ? C12 C17 1.512(3) . ? C13 C14 1.388(3) . ? C13 H13 0.9500 . ? C14 C15 1.393(3) . ? C14 C18 1.506(3) . ? C15 C16 1.392(3) . ? C15 H15 0.9500 . ? C16 C19 1.511(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 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 N2 Ni1 N2 180.0 . 3_655 ? N2 Ni1 N1 89.10(7) . 3_655 ? N2 Ni1 N1 90.90(7) 3_655 3_655 ? N2 Ni1 N1 90.90(7) . . ? N2 Ni1 N1 89.11(7) 3_655 . ? N1 Ni1 N1 180.0 3_655 . ? C1 N1 C4 104.38(16) . . ? C1 N1 Ni1 126.87(13) . . ? C4 N1 Ni1 128.75(13) . . ? C9 N2 C6 104.37(16) . 3_655 ? C9 N2 Ni1 127.17(13) . . ? C6 N2 Ni1 128.45(13) 3_655 . ? C10 C1 N1 125.32(18) . . ? C10 C1 C2 123.80(19) . . ? N1 C1 C2 110.79(18) . . ? C3 C2 C1 107.33(19) . . ? C3 C2 H2 126.3 . . ? C1 C2 H2 126.3 . . ? C2 C3 C4 106.97(18) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? C5 C4 N1 125.46(17) . . ? C5 C4 C3 124.01(18) . . ? N1 C4 C3 110.51(17) . . ? C6 C5 C4 121.82(18) . . ? C6 C5 C11 117.67(18) . . ? C4 C5 C11 120.50(18) . . ? C5 C6 N2 126.19(18) . 3_655 ? C5 C6 C7 123.41(18) . . ? N2 C6 C7 110.40(17) 3_655 . ? C8 C7 C6 107.05(18) . . ? C8 C7 H7 126.5 . . ? C6 C7 H7 126.5 . . ? C7 C8 C9 106.93(18) . 3_655 ? C7 C8 H8 126.5 . . ? C9 C8 H8 126.5 3_655 . ? C10 C9 N2 125.34(18) . . ? C10 C9 C8 123.40(19) . 3_655 ? N2 C9 C8 111.23(18) . 3_655 ? C9 C10 C1 124.22(19) . . ? C9 C10 H10 117.9 . . ? C1 C10 H10 117.9 . . ? C12 C11 C16 120.17(18) . . ? C12 C11 C5 120.47(18) . . ? C16 C11 C5 119.27(18) . . ? C13 C12 C11 119.01(19) . . ? C13 C12 C17 119.95(19) . . ? C11 C12 C17 121.02(18) . . ? C14 C13 C12 121.96(19) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 118.08(18) . . ? C13 C14 C18 120.9(2) . . ? C15 C14 C18 121.1(2) . . ? C16 C15 C14 121.90(19) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C15 C16 C11 118.81(19) . . ? C15 C16 C19 119.91(19) . . ? C11 C16 C19 121.28(19) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 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 N2 Ni1 N1 C1 -2.20(17) . . . . ? N2 Ni1 N1 C1 177.79(17) 3_655 . . . ? N1 Ni1 N1 C1 -73(6) 3_655 . . . ? N2 Ni1 N1 C4 177.02(17) . . . . ? N2 Ni1 N1 C4 -2.99(17) 3_655 . . . ? N1 Ni1 N1 C4 106(6) 3_655 . . . ? N2 Ni1 N2 C9 -143(3) 3_655 . . . ? N1 Ni1 N2 C9 178.24(16) 3_655 . . . ? N1 Ni1 N2 C9 -1.76(16) . . . . ? N2 Ni1 N2 C6 39(3) 3_655 . . 3_655 ? N1 Ni1 N2 C6 -0.25(16) 3_655 . . 3_655 ? N1 Ni1 N2 C6 179.75(16) . . . 3_655 ? C4 N1 C1 C10 -175.4(2) . . . . ? Ni1 N1 C1 C10 4.0(3) . . . . ? C4 N1 C1 C2 1.2(2) . . . . ? Ni1 N1 C1 C2 -179.47(14) . . . . ? C10 C1 C2 C3 175.1(2) . . . . ? N1 C1 C2 C3 -1.5(2) . . . . ? C1 C2 C3 C4 1.2(2) . . . . ? C1 N1 C4 C5 -178.57(19) . . . . ? Ni1 N1 C4 C5 2.1(3) . . . . ? C1 N1 C4 C3 -0.4(2) . . . . ? Ni1 N1 C4 C3 -179.76(13) . . . . ? C2 C3 C4 C5 177.68(19) . . . . ? C2 C3 C4 N1 -0.5(2) . . . . ? N1 C4 C5 C6 2.7(3) . . . . ? C3 C4 C5 C6 -175.27(19) . . . . ? N1 C4 C5 C11 -176.78(18) . . . . ? C3 C4 C5 C11 5.3(3) . . . . ? C4 C5 C6 N2 -5.7(3) . . . 3_655 ? C11 C5 C6 N2 173.77(18) . . . 3_655 ? C4 C5 C6 C7 175.52(19) . . . . ? C11 C5 C6 C7 -5.0(3) . . . . ? C5 C6 C7 C8 178.11(19) . . . . ? N2 C6 C7 C8 -0.9(2) 3_655 . . . ? C6 C7 C8 C9 -0.2(2) . . . 3_655 ? C6 N2 C9 C10 -176.63(19) 3_655 . . . ? Ni1 N2 C9 C10 4.6(3) . . . . ? C6 N2 C9 C8 1.7(2) 3_655 . . 3_655 ? Ni1 N2 C9 C8 -177.11(13) . . . 3_655 ? N2 C9 C10 C1 -3.2(3) . . . . ? C8 C9 C10 C1 178.7(2) 3_655 . . . ? N1 C1 C10 C9 -1.2(3) . . . . ? C2 C1 C10 C9 -177.4(2) . . . . ? C6 C5 C11 C12 96.7(2) . . . . ? C4 C5 C11 C12 -83.8(3) . . . . ? C6 C5 C11 C16 -79.8(2) . . . . ? C4 C5 C11 C16 99.7(2) . . . . ? C16 C11 C12 C13 1.0(3) . . . . ? C5 C11 C12 C13 -175.50(19) . . . . ? C16 C11 C12 C17 179.5(2) . . . . ? C5 C11 C12 C17 3.0(3) . . . . ? C11 C12 C13 C14 1.4(3) . . . . ? C17 C12 C13 C14 -177.1(2) . . . . ? C12 C13 C14 C15 -2.1(3) . . . . ? C12 C13 C14 C18 177.8(2) . . . . ? C13 C14 C15 C16 0.5(3) . . . . ? C18 C14 C15 C16 -179.4(2) . . . . ? C14 C15 C16 C11 1.8(3) . . . . ? C14 C15 C16 C19 -178.5(2) . . . . ? C12 C11 C16 C15 -2.5(3) . . . . ? C5 C11 C16 C15 174.01(19) . . . . ? C12 C11 C16 C19 177.7(2) . . . . ? C5 C11 C16 C19 -5.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.389 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.065 #===END