Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Z.Ciunik' 'J.A. Wolny' 'M.F. Rudolf' 'S. Wolowiec' _publ_contact_author_name 'Dr Juliusz A Wolny' _publ_contact_author_address ; Dr Juliusz A Wolny Faculty of Chemistry University of Wroclaw Joliot-Curie 14 50-383 Wroclaw POLAND ; _publ_contact_author_email 'yool@wchuwr.chem.uni.wroc.pl' _publ_section_title ; Cis - trans isomerism and rotational isomerims in triazene-1-oxide bis-chelates of palladium (II) ; data_cmpd_1 _database_code_CSD 153413 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C22 H32 N6 O2 Pd' _chemical_formula_weight 518.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 28.306(8) _cell_length_b 5.9950(10) _cell_length_c 17.074(4) _cell_angle_alpha 90.00 _cell_angle_beta 122.72(3) _cell_angle_gamma 90.00 _cell_volume 2437.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.790 _exptl_absorpt_correction_T_min 0.7975 _exptl_absorpt_correction_T_max 0.8580 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 1651 _diffrn_reflns_av_R_equivalents 0.0145 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1580 _reflns_number_gt 1580 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+5.1179P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 1580 _refine_ls_number_parameters 206 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.1040 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_restrained_S_all 1.180 _refine_ls_shift/su_max 0.273 _refine_ls_shift/su_mean 0.014 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.5000 0.0000 0.5000 0.03451(19) Uani 1 d S . . O1 O 0.52398(14) 0.1964(6) 0.4340(2) 0.0462(8) Uani 1 d . . . N1 N 0.57941(16) 0.1673(7) 0.4693(3) 0.0442(9) Uani 1 d . . . N2 N 0.60827(17) 0.0181(6) 0.5313(3) 0.0412(9) Uani 1 d . . . N3 N 0.57968(16) -0.0951(7) 0.5580(3) 0.0394(8) Uani 1 d . . . C1 C 0.61325(18) -0.2505(8) 0.6312(3) 0.0363(10) Uani 1 d . . . C2 C 0.5889(2) -0.4463(8) 0.6367(3) 0.0413(11) Uani 1 d . . . C3 C 0.6213(2) -0.6013(10) 0.7074(4) 0.0457(11) Uani 1 d . . . C4 C 0.6777(2) -0.5606(9) 0.7738(3) 0.0443(12) Uani 1 d . . . C5 C 0.7008(2) -0.3634(10) 0.7662(4) 0.0509(13) Uani 1 d . . . C6 C 0.6699(2) -0.2101(10) 0.6969(4) 0.0464(12) Uani 1 d . . . C7 C 0.6031(2) 0.2807(9) 0.4194(4) 0.0483(12) Uani 1 d . . . C8 C 0.5744(5) 0.5051(11) 0.3861(7) 0.082(3) Uani 1 d . . . C9 C 0.6655(4) 0.303(3) 0.4848(8) 0.140(7) Uani 1 d . . . C10 C 0.5885(4) 0.1362(14) 0.3364(6) 0.078(2) Uani 1 d . . . C41 C 0.7130(3) -0.7239(13) 0.8520(4) 0.0630(16) Uani 1 d . . . H2 H 0.549(3) -0.484(8) 0.594(5) 0.062(18) Uiso 1 d . . . H3 H 0.602(2) -0.729(10) 0.708(4) 0.057(16) Uiso 1 d . . . H5 H 0.741(2) -0.339(10) 0.812(4) 0.063(17) Uiso 1 d . . . H6 H 0.685(2) -0.086(11) 0.697(4) 0.047(14) Uiso 1 d . . . H81 H 0.534(7) 0.510(19) 0.351(12) 0.21(8) Uiso 1 d . . . H82 H 0.593(3) 0.578(11) 0.359(4) 0.063(17) Uiso 1 d . . . H83 H 0.580(3) 0.587(14) 0.436(6) 0.09(3) Uiso 1 d . . . H91 H 0.680(4) 0.363(19) 0.450(7) 0.14(4) Uiso 1 d . . . H92 H 0.679(4) 0.250(18) 0.517(7) 0.10(4) Uiso 1 d . . . H93 H 0.672(4) 0.427(18) 0.545(8) 0.13(4) Uiso 1 d . . . H101 H 0.609(5) -0.002(14) 0.356(7) 0.12(4) Uiso 1 d . . . H102 H 0.606(3) 0.191(13) 0.309(5) 0.09(2) Uiso 1 d . . . H103 H 0.547(4) 0.155(19) 0.292(7) 0.15(4) Uiso 1 d . . . H411 H 0.716(3) -0.680(13) 0.916(6) 0.11(3) Uiso 1 d . . . H412 H 0.747(4) -0.742(14) 0.866(6) 0.11(3) Uiso 1 d . . . H413 H 0.692(3) -0.845(15) 0.848(6) 0.10(3) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0355(3) 0.0390(3) 0.0300(3) 0.0036(2) 0.0184(2) 0.0004(2) O1 0.0447(18) 0.049(2) 0.0461(18) 0.0144(16) 0.0256(16) 0.0037(16) N1 0.042(2) 0.055(2) 0.038(2) 0.007(2) 0.0226(18) -0.003(2) N2 0.043(2) 0.047(2) 0.0373(19) 0.002(2) 0.0240(17) -0.002(2) N3 0.041(2) 0.045(2) 0.035(2) 0.0021(18) 0.0217(17) 0.0005(19) C1 0.038(2) 0.042(2) 0.034(2) 0.002(2) 0.0223(19) 0.003(2) C2 0.042(3) 0.042(3) 0.036(2) -0.0006(19) 0.019(2) -0.002(2) C3 0.056(3) 0.041(3) 0.048(3) -0.001(2) 0.032(3) 0.001(3) C4 0.051(3) 0.046(3) 0.039(2) 0.006(2) 0.026(2) 0.014(2) C5 0.040(3) 0.059(4) 0.048(3) 0.004(3) 0.020(2) 0.006(3) C6 0.042(3) 0.050(3) 0.046(3) 0.003(2) 0.022(2) -0.005(2) C7 0.052(3) 0.054(3) 0.045(3) 0.006(2) 0.030(2) -0.010(2) C8 0.144(8) 0.047(3) 0.103(6) 0.017(4) 0.098(7) 0.006(4) C9 0.060(5) 0.244(17) 0.086(7) 0.073(10) 0.021(5) -0.044(7) C10 0.124(7) 0.069(5) 0.086(5) 0.001(4) 0.086(6) 0.000(5) C41 0.066(4) 0.066(4) 0.054(4) 0.019(3) 0.030(3) 0.021(4) 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 O1 1.987(3) 5_656 ? Pd1 O1 1.987(3) . ? Pd1 N3 1.994(4) 5_656 ? Pd1 N3 1.994(4) . ? O1 N1 1.354(5) . ? N1 N2 1.285(5) . ? N1 C7 1.501(6) . ? N2 N3 1.313(6) . ? N3 C1 1.431(6) . ? C1 C2 1.390(7) . ? C1 C6 1.394(7) . ? C2 C3 1.401(8) . ? C3 C4 1.393(7) . ? C4 C5 1.390(8) . ? C4 C41 1.515(7) . ? C5 C6 1.375(7) . ? C7 C9 1.500(11) . ? C7 C10 1.516(9) . ? C7 C8 1.514(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 O1 Pd1 O1 180.0 5_656 . ? O1 Pd1 N3 79.04(15) 5_656 5_656 ? O1 Pd1 N3 100.96(15) . 5_656 ? O1 Pd1 N3 100.96(15) 5_656 . ? O1 Pd1 N3 79.04(15) . . ? N3 Pd1 N3 180.000(1) 5_656 . ? N1 O1 Pd1 109.9(2) . . ? N2 N1 O1 121.6(4) . . ? N2 N1 C7 120.1(4) . . ? O1 N1 C7 117.0(4) . . ? N1 N2 N3 114.2(4) . . ? N2 N3 C1 113.4(4) . . ? N2 N3 Pd1 115.1(3) . . ? C1 N3 Pd1 131.2(3) . . ? C2 C1 C6 119.3(4) . . ? C2 C1 N3 119.3(4) . . ? C6 C1 N3 121.4(4) . . ? C1 C2 C3 120.0(5) . . ? C4 C3 C2 120.9(5) . . ? C5 C4 C3 117.5(5) . . ? C5 C4 C41 120.9(5) . . ? C3 C4 C41 121.6(6) . . ? C6 C5 C4 122.4(5) . . ? C5 C6 C1 119.8(5) . . ? N1 C7 C9 109.0(5) . . ? N1 C7 C10 107.0(5) . . ? C9 C7 C10 111.3(10) . . ? N1 C7 C8 107.6(5) . . ? C9 C7 C8 112.2(10) . . ? C10 C7 C8 109.7(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Pd1 O1 N1 -77(100) 5_656 . . . ? N3 Pd1 O1 N1 175.6(3) 5_656 . . . ? N3 Pd1 O1 N1 -4.4(3) . . . . ? Pd1 O1 N1 N2 5.0(5) . . . . ? Pd1 O1 N1 C7 172.3(3) . . . . ? O1 N1 N2 N3 -1.9(6) . . . . ? C7 N1 N2 N3 -168.9(4) . . . . ? N1 N2 N3 C1 -176.3(4) . . . . ? N1 N2 N3 Pd1 -2.3(5) . . . . ? O1 Pd1 N3 N2 -176.2(3) 5_656 . . . ? O1 Pd1 N3 N2 3.8(3) . . . . ? N3 Pd1 N3 N2 50(100) 5_656 . . . ? O1 Pd1 N3 C1 -3.5(4) 5_656 . . . ? O1 Pd1 N3 C1 176.5(4) . . . . ? N3 Pd1 N3 C1 -137(100) 5_656 . . . ? N2 N3 C1 C2 -149.1(4) . . . . ? Pd1 N3 C1 C2 38.1(6) . . . . ? N2 N3 C1 C6 30.6(6) . . . . ? Pd1 N3 C1 C6 -142.1(4) . . . . ? C6 C1 C2 C3 -0.3(7) . . . . ? N3 C1 C2 C3 179.5(4) . . . . ? C1 C2 C3 C4 1.0(8) . . . . ? C2 C3 C4 C5 -1.2(7) . . . . ? C2 C3 C4 C41 178.6(5) . . . . ? C3 C4 C5 C6 0.7(8) . . . . ? C41 C4 C5 C6 -179.1(5) . . . . ? C4 C5 C6 C1 0.0(8) . . . . ? C2 C1 C6 C5 -0.2(7) . . . . ? N3 C1 C6 C5 -180.0(5) . . . . ? N2 N1 C7 C9 -33.4(11) . . . . ? O1 N1 C7 C9 159.1(10) . . . . ? N2 N1 C7 C10 87.0(6) . . . . ? O1 N1 C7 C10 -80.5(6) . . . . ? N2 N1 C7 C8 -155.3(6) . . . . ? O1 N1 C7 C8 37.2(7) . . . . ? _diffrn_measured_fraction_theta_max 0.367 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.367 _refine_diff_density_max 0.879 _refine_diff_density_min -0.843 _refine_diff_density_rms 0.087 #===END data_cmpd_2 _database_code_CSD 153414 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C20 H28 N6 O2 Pd' _chemical_formula_weight 490.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 8.2540(10) _cell_length_b 11.666(2) _cell_length_c 12.134(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.620(10) _cell_angle_gamma 90.00 _cell_volume 1155.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 0.829 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7890 _exptl_absorpt_correction_T_max 0.8517 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 2188 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 27.91 _reflns_number_total 2029 _reflns_number_gt 1570 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.6013P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2029 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0699 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.062 _refine_ls_shift/su_mean 0.006 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.5000 0.5000 0.5000 0.03505(12) Uani 1 d S . . O1 O 0.3044(2) 0.59239(19) 0.52174(16) 0.0521(5) Uani 1 d . . . N1 N 0.2977(3) 0.6035(2) 0.6313(2) 0.0490(6) Uani 1 d . . . N2 N 0.4026(3) 0.5582(2) 0.7060(2) 0.0466(6) Uani 1 d . . . N3 N 0.5176(3) 0.49949(17) 0.6662(2) 0.0418(5) Uani 1 d . . . C1 C 0.6396(3) 0.4553(3) 0.7513(2) 0.0432(6) Uani 1 d . . . C2 C 0.7276(4) 0.3595(3) 0.7263(3) 0.0507(7) Uani 1 d . . . H2 H 0.707(4) 0.330(3) 0.651(3) 0.064(9) Uiso 1 d . . . C3 C 0.8434(4) 0.3123(3) 0.8084(3) 0.0647(9) Uani 1 d . . . H3 H 0.896(4) 0.252(3) 0.790(3) 0.069(11) Uiso 1 d . . . C4 C 0.8724(5) 0.3573(4) 0.9134(3) 0.0724(11) Uani 1 d . . . H4 H 0.952(4) 0.326(3) 0.968(3) 0.067(10) Uiso 1 d . . . C5 C 0.7864(5) 0.4533(4) 0.9367(3) 0.0717(11) Uani 1 d . . . H5 H 0.799(6) 0.481(3) 0.999(4) 0.078(14) Uiso 1 d . . . C6 C 0.6716(5) 0.5028(3) 0.8571(3) 0.0589(8) Uani 1 d . . . H6 H 0.614(4) 0.571(3) 0.881(3) 0.077(12) Uiso 1 d . . . C7 C 0.1520(4) 0.6683(3) 0.6617(3) 0.0550(8) Uani 1 d . . . C8 C 0.2054(9) 0.7225(7) 0.7781(5) 0.105(3) Uani 0.754(11) d P A 1 H81 H 0.1175 0.7636 0.8016 0.120 Uiso 0.75 d P A 1 H82 H 0.2966 0.7745 0.7745 0.120 Uiso 0.75 d P A 1 H83 H 0.2425 0.6631 0.8315 0.120 Uiso 0.75 d P A 1 C9 C 0.1121(12) 0.7615(7) 0.5826(7) 0.129(4) Uani 0.754(11) d P A 1 H91 H 0.0408 0.8145 0.6116 0.120 Uiso 0.75 d P A 1 H92 H 0.0607 0.7314 0.5129 0.120 Uiso 0.75 d P A 1 H93 H 0.2121 0.8002 0.5723 0.120 Uiso 0.75 d P A 1 C10 C 0.0247(9) 0.5822(6) 0.6682(10) 0.144(5) Uani 0.754(11) d P A 1 H101 H 0.0049 0.5416 0.5965 0.120 Uiso 0.75 d P A 1 H102 H -0.0761 0.6209 0.6772 0.120 Uiso 0.75 d P A 1 H103 H 0.0563 0.5306 0.7257 0.120 Uiso 0.75 d P A 1 C8' C 0.117(2) 0.6423(16) 0.7747(14) 0.073(5) Uiso 0.246(11) d P A 2 C9' C 0.190(3) 0.790(2) 0.644(2) 0.101(8) Uiso 0.246(11) d P A 2 C10' C -0.015(2) 0.6314(17) 0.5769(15) 0.074(5) Uiso 0.246(11) d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03385(17) 0.03434(18) 0.03867(17) -0.00175(12) 0.01102(11) 0.00388(11) O1 0.0540(12) 0.0624(13) 0.0420(11) 0.0004(9) 0.0142(9) 0.0167(10) N1 0.0529(14) 0.0500(15) 0.0479(14) 0.0039(11) 0.0196(11) 0.0123(12) N2 0.0523(14) 0.0437(14) 0.0468(13) 0.0016(11) 0.0172(11) 0.0067(11) N3 0.0432(13) 0.0394(13) 0.0449(12) 0.0008(10) 0.0128(10) 0.0058(10) C1 0.0423(15) 0.0401(14) 0.0476(16) 0.0073(13) 0.0079(12) -0.0043(13) C2 0.0474(16) 0.0536(19) 0.0526(18) 0.0027(15) 0.0118(13) 0.0040(14) C3 0.0527(19) 0.057(2) 0.084(3) 0.0099(19) 0.0108(18) 0.0144(17) C4 0.060(2) 0.079(3) 0.072(2) 0.020(2) -0.0114(18) 0.001(2) C5 0.082(3) 0.075(3) 0.052(2) -0.001(2) -0.0095(19) -0.009(2) C6 0.068(2) 0.0482(19) 0.059(2) -0.0033(16) 0.0044(16) 0.0008(16) C7 0.0505(17) 0.0576(19) 0.0634(19) 0.0044(15) 0.0297(15) 0.0190(15) C8 0.099(5) 0.129(6) 0.087(4) -0.033(4) 0.014(3) 0.059(5) C9 0.168(8) 0.136(7) 0.101(5) 0.056(5) 0.078(6) 0.120(6) C10 0.082(5) 0.086(5) 0.290(14) -0.025(6) 0.111(7) -0.009(4) 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 O1 1.9914(19) . ? Pd1 O1 1.9914(19) 3_666 ? Pd1 N3 2.000(2) . ? Pd1 N3 2.000(2) 3_666 ? O1 N1 1.345(3) . ? N1 N2 1.271(3) . ? N1 C7 1.513(3) . ? N2 N3 1.320(3) . ? N3 C1 1.427(4) . ? C1 C6 1.386(5) . ? C1 C2 1.392(4) . ? C2 C3 1.386(5) . ? C3 C4 1.366(5) . ? C4 C5 1.378(6) . ? C5 C6 1.374(6) . ? C7 C9 1.455(6) . ? C7 C8' 1.475(17) . ? C7 C10 1.463(7) . ? C7 C9' 1.48(3) . ? C7 C8 1.550(7) . ? C7 C10' 1.650(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pd1 O1 180.0 . 3_666 ? O1 Pd1 N3 78.81(8) . . ? O1 Pd1 N3 101.19(8) 3_666 . ? O1 Pd1 N3 101.19(8) . 3_666 ? O1 Pd1 N3 78.81(8) 3_666 3_666 ? N3 Pd1 N3 180.0 . 3_666 ? N1 O1 Pd1 109.70(15) . . ? N2 N1 O1 122.7(2) . . ? N2 N1 C7 121.0(2) . . ? O1 N1 C7 116.2(2) . . ? N1 N2 N3 113.9(2) . . ? N2 N3 C1 113.0(2) . . ? N2 N3 Pd1 114.83(18) . . ? C1 N3 Pd1 131.94(19) . . ? C6 C1 C2 119.3(3) . . ? C6 C1 N3 122.8(3) . . ? C2 C1 N3 117.9(3) . . ? C3 C2 C1 119.3(3) . . ? C4 C3 C2 121.5(4) . . ? C3 C4 C5 118.7(4) . . ? C6 C5 C4 121.3(4) . . ? C5 C6 C1 119.9(4) . . ? C9 C7 C8' 135.3(7) . . ? C9 C7 C10 117.1(6) . . ? C8' C7 C10 64.3(8) . . ? C9 C7 C9' 38.6(9) . . ? C8' C7 C9' 113.9(12) . . ? C10 C7 C9' 146.7(10) . . ? C9 C7 N1 108.8(3) . . ? C8' C7 N1 113.5(7) . . ? C10 C7 N1 105.9(3) . . ? C9' C7 N1 104.8(10) . . ? C9 C7 C8 107.5(5) . . ? C8' C7 C8 46.0(7) . . ? C10 C7 C8 109.8(5) . . ? C9' C7 C8 72.5(10) . . ? N1 C7 C8 107.3(3) . . ? C9 C7 C10' 72.5(8) . . ? C8' C7 C10' 105.2(9) . . ? C10 C7 C10' 46.7(7) . . ? C9' C7 C10' 109.7(11) . . ? N1 C7 C10' 109.8(6) . . ? C8 C7 C10' 140.5(7) . . ? 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 O1 Pd1 O1 N1 84(100) 3_666 . . . ? N3 Pd1 O1 N1 1.26(18) . . . . ? N3 Pd1 O1 N1 -178.74(18) 3_666 . . . ? Pd1 O1 N1 N2 -1.1(3) . . . . ? Pd1 O1 N1 C7 -177.9(2) . . . . ? O1 N1 N2 N3 -0.2(4) . . . . ? C7 N1 N2 N3 176.6(2) . . . . ? N1 N2 N3 C1 176.4(2) . . . . ? N1 N2 N3 Pd1 1.3(3) . . . . ? O1 Pd1 N3 N2 -1.45(18) . . . . ? O1 Pd1 N3 N2 178.55(18) 3_666 . . . ? N3 Pd1 N3 N2 -148(100) 3_666 . . . ? O1 Pd1 N3 C1 -175.4(3) . . . . ? O1 Pd1 N3 C1 4.6(3) 3_666 . . . ? N3 Pd1 N3 C1 38(100) 3_666 . . . ? N2 N3 C1 C6 -23.4(4) . . . . ? Pd1 N3 C1 C6 150.6(3) . . . . ? N2 N3 C1 C2 155.8(2) . . . . ? Pd1 N3 C1 C2 -30.2(4) . . . . ? C6 C1 C2 C3 1.2(5) . . . . ? N3 C1 C2 C3 -178.0(3) . . . . ? C1 C2 C3 C4 0.4(5) . . . . ? C2 C3 C4 C5 -1.4(6) . . . . ? C3 C4 C5 C6 0.9(6) . . . . ? C4 C5 C6 C1 0.7(6) . . . . ? C2 C1 C6 C5 -1.7(5) . . . . ? N3 C1 C6 C5 177.4(3) . . . . ? N2 N1 C7 C9 146.6(6) . . . . ? O1 N1 C7 C9 -36.5(6) . . . . ? N2 N1 C7 C8' -18.3(10) . . . . ? O1 N1 C7 C8' 158.6(9) . . . . ? N2 N1 C7 C10 -86.7(6) . . . . ? O1 N1 C7 C10 90.2(6) . . . . ? N2 N1 C7 C9' 106.5(11) . . . . ? O1 N1 C7 C9' -76.6(11) . . . . ? N2 N1 C7 C8 30.5(5) . . . . ? O1 N1 C7 C8 -152.5(4) . . . . ? N2 N1 C7 C10' -135.8(8) . . . . ? O1 N1 C7 C10' 41.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.701 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.701 _refine_diff_density_max 0.511 _refine_diff_density_min -0.211 _refine_diff_density_rms 0.060 #===END data_cmpd_3 _database_code_CSD 178675 _audit_creation_method SHELXL _chemical_formula_sum 'C24 H36 N6 O2 Pd' _chemical_formula_weight 546.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 8.7850(10) _cell_length_b 16.359(2) _cell_length_c 9.3340(10) _cell_angle_alpha 90.00 _cell_angle_beta 98.550(10) _cell_angle_gamma 90.00 _cell_volume 1326.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.369 _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 0.730 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 2480 _diffrn_reflns_av_R_equivalents 0.0129 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2336 _reflns_number_observed 1705 _reflns_observed_criterion >2sigma(I) _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1407P)^2^+0.3458P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_extinction_method none _refine_ls_number_reflns 2336 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_obs 0.0500 _refine_ls_wR_factor_all 0.1939 _refine_ls_wR_factor_obs 0.1689 _refine_ls_goodness_of_fit_all 1.119 _refine_ls_goodness_of_fit_obs 1.152 _refine_ls_restrained_S_all 1.119 _refine_ls_restrained_S_obs 1.152 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.5000 0.5000 0.5000 0.0322(3) Uani 1 d S . O1 O 0.3494(4) 0.5865(2) 0.4260(5) 0.0449(10) Uani 1 d . . N1 N 0.2333(5) 0.5878(3) 0.5071(5) 0.0378(11) Uani 1 d . . N2 N 0.2314(5) 0.5418(3) 0.6171(5) 0.0383(11) Uani 1 d . . N3 N 0.3515(6) 0.4927(2) 0.6421(7) 0.0375(12) Uani 1 d . . C1 C 0.3510(6) 0.4398(3) 0.7655(6) 0.0348(12) Uani 1 d . . C2 C 0.3086(6) 0.4654(4) 0.8987(7) 0.0376(13) Uani 1 d . . C3 C 0.2980(6) 0.4067(4) 1.0037(7) 0.0451(15) Uani 1 d . . C4 C 0.3413(7) 0.3257(4) 0.9821(7) 0.051(2) Uani 1 d . . H4 H 0.3352 0.2871 1.0539 0.060 Uiso 1 d . . C5 C 0.3926(7) 0.3028(4) 0.8566(7) 0.0486(15) Uani 1 d . . H5 H 0.4237 0.2492 0.8440 0.080 Uiso 1 d . . C6 C 0.3974(6) 0.3591(4) 0.7475(6) 0.0404(13) Uani 1 d . . H6 H 0.4304 0.3433 0.6617 0.040 Uiso 1 d . . C21 C 0.2756(8) 0.5548(4) 0.9261(8) 0.051(2) Uani 1 d . . H211 H 0.3026 0.5664 1.0276 0.080 Uiso 1 d . . H212 H 0.1669 0.5651 0.8979 0.080 Uiso 1 d . . H213 H 0.3332 0.5888 0.8710 0.080 Uiso 1 d . . C31 C 0.2440(10) 0.4292(5) 1.1463(9) 0.073(2) Uani 1 d . . H311 H 0.1448 0.4544 1.1274 0.080 Uiso 1 d . . H312 H 0.3163 0.4670 1.1988 0.080 Uiso 1 d . . H313 H 0.2387 0.3809 1.2037 0.080 Uiso 1 d . . C7 C 0.1090(6) 0.6487(4) 0.4591(7) 0.0408(13) Uani 1 d . . C8 C -0.0150(8) 0.6409(5) 0.5578(9) 0.058(2) Uani 1 d . . H81 H -0.0925 0.6826 0.5319 0.080 Uiso 1 d . . H82 H 0.0302 0.6484 0.6566 0.080 Uiso 1 d . . H83 H -0.0630 0.5882 0.5458 0.080 Uiso 1 d . . C9 C 0.1833(8) 0.7325(4) 0.4704(9) 0.067(2) Uani 1 d . . H91 H 0.1075 0.7730 0.4354 0.070 Uiso 1 d . . H92 H 0.2653 0.7339 0.4132 0.070 Uiso 1 d . . H93 H 0.2232 0.7437 0.5698 0.070 Uiso 1 d . . C10 C 0.0428(8) 0.6282(5) 0.3022(8) 0.058(2) Uani 1 d . . H101 H -0.0369 0.6669 0.2681 0.080 Uiso 1 d . . H102 H -0.0009 0.5741 0.2981 0.080 Uiso 1 d . . H103 H 0.1223 0.6308 0.2431 0.080 Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0273(4) 0.0362(4) 0.0342(4) 0.0035(2) 0.0086(3) 0.0041(2) O1 0.034(2) 0.054(2) 0.051(2) 0.016(2) 0.019(2) 0.012(2) N1 0.029(2) 0.041(3) 0.045(3) 0.004(2) 0.011(2) 0.006(2) N2 0.030(2) 0.037(3) 0.048(3) 0.003(2) 0.009(2) 0.002(2) N3 0.029(3) 0.036(3) 0.048(3) 0.006(2) 0.006(2) 0.005(2) C1 0.027(2) 0.037(3) 0.041(3) 0.002(2) 0.008(2) -0.001(2) C2 0.030(3) 0.038(3) 0.042(3) -0.003(3) -0.001(2) -0.002(2) C3 0.033(3) 0.054(4) 0.048(4) 0.005(3) 0.005(3) -0.002(3) C4 0.054(4) 0.053(4) 0.045(4) 0.015(3) 0.006(3) -0.004(3) C5 0.053(4) 0.035(3) 0.056(4) 0.003(3) 0.004(3) 0.001(3) C6 0.036(3) 0.044(3) 0.043(3) 0.002(3) 0.011(2) 0.002(2) C21 0.055(4) 0.050(4) 0.048(4) -0.011(3) 0.008(3) 0.007(3) C31 0.078(5) 0.086(5) 0.056(5) 0.002(4) 0.015(4) -0.010(4) C7 0.031(3) 0.043(3) 0.050(3) 0.009(3) 0.009(2) 0.009(2) C8 0.048(4) 0.070(5) 0.059(4) 0.014(4) 0.021(3) 0.018(3) C9 0.061(4) 0.041(4) 0.099(6) 0.006(4) 0.010(4) 0.002(3) C10 0.043(3) 0.077(5) 0.054(4) 0.006(4) 0.004(3) 0.012(3) 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 O1 1.990(4) . ? Pd1 O1 1.990(4) 3_666 ? Pd1 N3 1.997(6) 3_666 ? Pd1 N3 1.997(6) . ? O1 N1 1.358(6) . ? N1 N2 1.275(7) . ? N1 C7 1.497(7) . ? N2 N3 1.319(7) . ? N3 C1 1.442(8) . ? C1 C6 1.399(8) . ? C1 C2 1.413(8) . ? C2 C3 1.385(9) . ? C2 C21 1.521(10) . ? C3 C4 1.402(9) . ? C3 C31 1.523(10) . ? C4 C5 1.368(9) . ? C5 C6 1.378(8) . ? C7 C9 1.515(9) . ? C7 C10 1.531(9) . ? C7 C8 1.533(8) . ? 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 O1 Pd1 O1 180.0 . 3_666 ? O1 Pd1 N3 101.1(2) . 3_666 ? O1 Pd1 N3 78.9(2) 3_666 3_666 ? O1 Pd1 N3 78.9(2) . . ? O1 Pd1 N3 101.1(2) 3_666 . ? N3 Pd1 N3 179.999(1) 3_666 . ? N1 O1 Pd1 109.4(3) . . ? N2 N1 O1 122.8(4) . . ? N2 N1 C7 122.5(4) . . ? O1 N1 C7 114.7(4) . . ? N1 N2 N3 113.3(5) . . ? N2 N3 C1 114.1(5) . . ? N2 N3 Pd1 115.6(4) . . ? C1 N3 Pd1 130.3(4) . . ? C6 C1 C2 120.3(5) . . ? C6 C1 N3 115.8(5) . . ? C2 C1 N3 123.9(5) . . ? C3 C2 C1 118.2(6) . . ? C3 C2 C21 120.8(6) . . ? C1 C2 C21 121.0(6) . . ? C2 C3 C4 120.3(6) . . ? C2 C3 C31 120.9(6) . . ? C4 C3 C31 118.7(6) . . ? C5 C4 C3 120.9(6) . . ? C4 C5 C6 120.0(6) . . ? C5 C6 C1 120.0(5) . . ? N1 C7 C9 107.1(5) . . ? N1 C7 C10 107.3(5) . . ? C9 C7 C10 111.3(6) . . ? N1 C7 C8 108.4(5) . . ? C9 C7 C8 111.8(6) . . ? C10 C7 C8 110.7(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 O1 Pd1 O1 N1 156.5(294) 3_666 . . . ? N3 Pd1 O1 N1 177.0(3) 3_666 . . . ? N3 Pd1 O1 N1 -3.0(3) . . . . ? Pd1 O1 N1 N2 3.2(6) . . . . ? Pd1 O1 N1 C7 -178.1(4) . . . . ? O1 N1 N2 N3 -0.9(8) . . . . ? C7 N1 N2 N3 -179.6(5) . . . . ? N1 N2 N3 C1 -179.6(5) . . . . ? N1 N2 N3 Pd1 -1.9(6) . . . . ? O1 Pd1 N3 N2 2.8(4) . . . . ? O1 Pd1 N3 N2 -177.2(4) 3_666 . . . ? N3 Pd1 N3 N2 -147.3(50) 3_666 . . . ? O1 Pd1 N3 C1 180.0(5) . . . . ? O1 Pd1 N3 C1 0.0(5) 3_666 . . . ? N3 Pd1 N3 C1 29.9(50) 3_666 . . . ? N2 N3 C1 C6 138.4(5) . . . . ? Pd1 N3 C1 C6 -38.8(7) . . . . ? N2 N3 C1 C2 -42.1(8) . . . . ? Pd1 N3 C1 C2 140.6(5) . . . . ? C6 C1 C2 C3 -7.0(8) . . . . ? N3 C1 C2 C3 173.6(5) . . . . ? C6 C1 C2 C21 172.9(5) . . . . ? N3 C1 C2 C21 -6.5(8) . . . . ? C1 C2 C3 C4 5.4(8) . . . . ? C21 C2 C3 C4 -174.6(5) . . . . ? C1 C2 C3 C31 -176.5(6) . . . . ? C21 C2 C3 C31 3.6(9) . . . . ? C2 C3 C4 C5 -0.9(9) . . . . ? C31 C3 C4 C5 -179.1(6) . . . . ? C3 C4 C5 C6 -2.1(10) . . . . ? C4 C5 C6 C1 0.5(9) . . . . ? C2 C1 C6 C5 4.1(8) . . . . ? N3 C1 C6 C5 -176.4(5) . . . . ? N2 N1 C7 C9 117.8(6) . . . . ? O1 N1 C7 C9 -60.9(7) . . . . ? N2 N1 C7 C10 -122.6(6) . . . . ? O1 N1 C7 C10 58.7(6) . . . . ? N2 N1 C7 C8 -2.9(7) . . . . ? O1 N1 C7 C8 178.3(5) . . . . ? _refine_diff_density_max 2.071 _refine_diff_density_min -1.406 _refine_diff_density_rms 0.164 #===END data_cmpd_4 _database_code_CSD 153406 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C22 H32 N6 O2 Pd' _chemical_formula_weight 518.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 14.138(3) _cell_length_b 9.568(2) _cell_length_c 17.685(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.49(3) _cell_angle_gamma 90.00 _cell_volume 2385.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.808 _exptl_absorpt_correction_T_min 0.7652 _exptl_absorpt_correction_T_max 0.7937 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 2683 _diffrn_reflns_av_R_equivalents 0.0143 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max -3 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 6.50 _diffrn_reflns_theta_max 25.06 _reflns_number_total 2557 _reflns_number_gt 1794 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+1.4455P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2557 _refine_ls_number_parameters 408 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0196 _refine_ls_wR_factor_ref 0.0559 _refine_ls_wR_factor_gt 0.0456 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.102 _refine_ls_shift/su_mean 0.004 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.836358(19) -0.002966(19) 0.403152(12) 0.02756(10) Uani 1 d . . . O1 O 0.8016(2) 0.13200(17) 0.32075(14) 0.0409(7) Uani 1 d . . . O1' O 0.8810(2) -0.13266(17) 0.48574(13) 0.0389(7) Uani 1 d . . . N1 N 0.7992(3) 0.0644(2) 0.25350(19) 0.0401(10) Uani 1 d . . . N2 N 0.8173(3) -0.0648(2) 0.24828(19) 0.0375(9) Uani 1 d . . . N3 N 0.8367(3) -0.1250(2) 0.31293(17) 0.0331(8) Uani 1 d . . . N1' N 0.8849(3) -0.0627(2) 0.55291(19) 0.0379(9) Uani 1 d . . . N2' N 0.8588(3) 0.0646(2) 0.55730(19) 0.0361(9) Uani 1 d . . . N3' N 0.8271(3) 0.1170(2) 0.49271(17) 0.0332(8) Uani 1 d . . . C1 C 0.8534(3) -0.2726(3) 0.3087(2) 0.0298(9) Uani 1 d . . . C2 C 0.7790(3) -0.3693(3) 0.2909(2) 0.0357(9) Uani 1 d . . . C3 C 0.8103(4) -0.5095(3) 0.2919(2) 0.0504(13) Uani 1 d . . . C4 C 0.9003(5) -0.5507(4) 0.3084(3) 0.0498(15) Uani 1 d . . . C5 C 0.9700(5) -0.4542(4) 0.3271(3) 0.0479(14) Uani 1 d . . . C6 C 0.9441(4) -0.3143(3) 0.3280(2) 0.0412(11) Uani 1 d . . . C7 C 0.6756(4) -0.3338(3) 0.2701(3) 0.0476(11) Uani 1 d . . . C8 C 0.6103(6) -0.4614(6) 0.2771(5) 0.0768(19) Uani 1 d . . . C9 C 0.6625(7) -0.2844(6) 0.1879(5) 0.0721(19) Uani 1 d . . . C10 C 0.6374(6) -0.2229(6) 0.3236(5) 0.0712(18) Uani 1 d . . . C11 C 0.7737(5) 0.1479(4) 0.1874(3) 0.0580(15) Uani 1 d . . . C1' C 0.8011(3) 0.2629(2) 0.49676(19) 0.0291(8) Uani 1 d . . . C2' C 0.7090(3) 0.3092(3) 0.4921(2) 0.0346(10) Uani 1 d . . . C3' C 0.6971(4) 0.4552(3) 0.4921(3) 0.0434(12) Uani 1 d . . . C4' C 0.7730(5) 0.5450(3) 0.4978(3) 0.0446(13) Uani 1 d . . . C5' C 0.8621(4) 0.4970(4) 0.5028(2) 0.0453(13) Uani 1 d . . . C6' C 0.8787(4) 0.3542(3) 0.5023(3) 0.0396(11) Uani 1 d . . . C7' C 0.6204(3) 0.2159(3) 0.4868(3) 0.0424(10) Uani 1 d . . . C8' C 0.5303(6) 0.2976(7) 0.4991(7) 0.084(2) Uani 1 d . . . C9' C 0.6043(5) 0.1543(6) 0.4075(4) 0.0645(15) Uani 1 d . . . C10' C 0.6312(6) 0.0973(8) 0.5453(5) 0.094(3) Uani 1 d . . . C11' C 0.9219(5) -0.1393(4) 0.6185(3) 0.0479(11) Uani 1 d . . . H111 H 0.704(6) 0.178(4) 0.199(4) 0.074(15) Uiso 1 d . . . H114 H 0.926(4) -0.079(3) 0.661(3) 0.044(10) Uiso 1 d . . . H115 H 0.884(5) -0.208(4) 0.617(3) 0.063(16) Uiso 1 d . . . H116 H 0.974(6) -0.175(4) 0.609(3) 0.066(16) Uiso 1 d . . . H112 H 0.819(5) 0.217(4) 0.189(3) 0.058(14) Uiso 1 d . . . H3A H 0.752(4) -0.577(3) 0.282(3) 0.046(11) Uiso 1 d . . . H4A H 0.922(7) -0.639(5) 0.307(5) 0.10(2) Uiso 1 d . . . H5A H 1.026(4) -0.481(4) 0.340(3) 0.043(11) Uiso 1 d . . . H6A H 0.998(4) -0.242(4) 0.345(3) 0.053(12) Uiso 1 d . . . H8A H 0.631(8) -0.538(6) 0.235(6) 0.12(2) Uiso 1 d . . . H8B H 0.625(6) -0.505(5) 0.325(5) 0.087(19) Uiso 1 d . . . H8C H 0.552(6) -0.434(4) 0.266(4) 0.073(18) Uiso 1 d . . . H9A H 0.702(7) -0.200(6) 0.178(5) 0.09(2) Uiso 1 d . . . H9B H 0.679(7) -0.359(6) 0.158(5) 0.08(2) Uiso 1 d . . . H9C H 0.606(8) -0.265(6) 0.180(5) 0.10(3) Uiso 1 d . . . H10A H 0.670(9) -0.138(7) 0.324(6) 0.12(3) Uiso 1 d . . . H10B H 0.568(7) -0.209(5) 0.323(4) 0.089(18) Uiso 1 d . . . H10C H 0.660(6) -0.246(5) 0.382(5) 0.10(2) Uiso 1 d . . . H113 H 0.773(4) 0.085(4) 0.144(3) 0.063(13) Uiso 1 d . . . H3'A H 0.630(5) 0.497(3) 0.492(3) 0.053(11) Uiso 1 d . . . H4'A H 0.765(6) 0.628(5) 0.499(4) 0.074(17) Uiso 1 d . . . H5'A H 0.920(5) 0.561(4) 0.505(3) 0.062(14) Uiso 1 d . . . H6'A H 0.936(4) 0.317(3) 0.505(3) 0.037(10) Uiso 1 d . . . H8'A H 0.485(7) 0.232(6) 0.495(4) 0.09(2) Uiso 1 d . . . H8'B H 0.541(7) 0.315(6) 0.548(6) 0.10(2) Uiso 1 d . . . H8'C H 0.513(8) 0.373(7) 0.464(5) 0.10(3) Uiso 1 d . . . H9'A H 0.658(6) 0.097(5) 0.394(4) 0.085(18) Uiso 1 d . . . H9'B H 0.547(6) 0.105(5) 0.399(4) 0.079(16) Uiso 1 d . . . H9'C H 0.599(7) 0.232(5) 0.370(5) 0.09(2) Uiso 1 d . . . H10D H 0.682(10) 0.025(7) 0.528(6) 0.13(3) Uiso 1 d . . . H10E H 0.661(9) 0.123(7) 0.589(6) 0.13(3) Uiso 1 d . . . H10F H 0.569(7) 0.062(5) 0.550(4) 0.080(16) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03930(17) 0.02387(13) 0.01942(14) -0.00307(7) 0.00164(10) -0.00205(8) O1 0.070(2) 0.0263(10) 0.0267(14) -0.0018(7) 0.0029(13) 0.0015(9) O1' 0.060(2) 0.0310(10) 0.0250(14) -0.0021(7) -0.0005(13) 0.0041(9) N1 0.064(3) 0.0324(14) 0.023(2) -0.0015(10) 0.0025(17) 0.0053(12) N2 0.053(3) 0.0274(13) 0.032(2) -0.0015(10) 0.0013(17) 0.0006(11) N3 0.049(3) 0.0255(12) 0.0249(18) -0.0003(9) 0.0011(15) -0.0017(10) N1' 0.054(3) 0.0355(14) 0.024(2) -0.0011(10) 0.0037(17) 0.0024(12) N2' 0.047(3) 0.0299(13) 0.032(2) -0.0024(10) 0.0038(17) 0.0012(11) N3' 0.044(2) 0.0259(12) 0.0297(18) -0.0002(10) 0.0014(15) 0.0012(10) C1 0.039(3) 0.0251(14) 0.025(2) -0.0033(10) 0.0003(17) 0.0004(12) C2 0.044(3) 0.0314(16) 0.031(2) -0.0043(11) -0.0024(19) -0.0003(13) C3 0.075(4) 0.0311(17) 0.045(3) -0.0076(14) 0.004(2) -0.012(2) C4 0.065(5) 0.0320(17) 0.052(3) -0.0020(14) -0.001(3) 0.0107(17) C5 0.052(4) 0.046(2) 0.045(3) 0.0011(15) -0.003(3) 0.020(2) C6 0.051(4) 0.0372(18) 0.035(2) -0.0049(13) 0.001(2) -0.0008(16) C7 0.046(3) 0.0481(19) 0.048(3) -0.0074(14) -0.001(2) -0.0094(15) C8 0.054(5) 0.073(3) 0.102(6) -0.002(3) -0.008(4) -0.023(3) C9 0.070(6) 0.074(4) 0.067(4) -0.003(2) -0.024(4) -0.007(3) C10 0.050(5) 0.082(3) 0.084(5) -0.025(3) 0.015(4) 0.006(2) C11 0.099(5) 0.040(2) 0.034(3) 0.0069(15) 0.000(3) 0.012(2) C1' 0.038(3) 0.0246(13) 0.025(2) -0.0057(10) 0.0042(17) -0.0033(13) C2' 0.045(3) 0.0276(15) 0.031(2) -0.0018(11) 0.0036(18) -0.0045(13) C3' 0.047(4) 0.0339(17) 0.048(3) 0.0012(12) -0.003(2) 0.0036(15) C4' 0.064(4) 0.0251(16) 0.044(3) 0.0018(12) -0.003(2) -0.0040(15) C5' 0.062(4) 0.0357(16) 0.039(2) -0.0045(15) 0.011(2) -0.020(2) C6' 0.044(4) 0.0345(17) 0.041(3) -0.0064(13) 0.007(2) -0.0072(17) C7' 0.038(3) 0.0396(17) 0.049(3) 0.0001(13) 0.002(2) -0.0064(13) C8' 0.050(5) 0.075(4) 0.130(7) -0.031(4) 0.033(4) -0.015(3) C9' 0.041(4) 0.075(3) 0.075(4) -0.021(2) -0.007(3) -0.014(2) C10' 0.079(6) 0.105(5) 0.095(6) 0.053(4) -0.022(5) -0.057(5) C11' 0.060(4) 0.045(2) 0.037(3) 0.0062(16) -0.001(2) 0.006(2) 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 N3' 1.969(3) . ? Pd1 N3 1.978(3) . ? Pd1 O1 1.980(2) . ? Pd1 O1' 1.982(2) . ? O1 N1 1.352(4) . ? O1' N1' 1.361(4) . ? N1 N2 1.268(3) . ? N1 C11 1.438(5) . ? N2 N3 1.290(4) . ? N3 C1 1.434(3) . ? N1' N2' 1.277(3) . ? N1' C11' 1.435(5) . ? N2' N3' 1.295(4) . ? N3' C1' 1.447(4) . ? C1 C6 1.362(7) . ? C1 C2 1.417(5) . ? C2 C3 1.413(5) . ? C2 C7 1.517(7) . ? C3 C4 1.341(8) . ? C4 C5 1.373(9) . ? C5 C6 1.388(5) . ? C7 C9 1.526(9) . ? C7 C8 1.541(7) . ? C7 C10 1.547(7) . ? C1' C2' 1.372(6) . ? C1' C6' 1.399(6) . ? C2' C3' 1.407(4) . ? C2' C7' 1.535(5) . ? C3' C4' 1.372(8) . ? C4' C5' 1.337(9) . ? C5' C6' 1.387(6) . ? C7' C9' 1.522(7) . ? C7' C8' 1.525(9) . ? C7' C10' 1.535(7) . ? 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 N3' Pd1 N3 176.32(15) . . ? N3' Pd1 O1 100.58(10) . . ? N3 Pd1 O1 78.91(9) . . ? N3' Pd1 O1' 79.02(9) . . ? N3 Pd1 O1' 101.77(10) . . ? O1 Pd1 O1' 175.70(12) . . ? N1 O1 Pd1 108.85(15) . . ? N1' O1' Pd1 108.90(15) . . ? N2 N1 O1 122.7(3) . . ? N2 N1 C11 121.5(3) . . ? O1 N1 C11 115.9(2) . . ? N1 N2 N3 113.6(3) . . ? N2 N3 C1 114.7(2) . . ? N2 N3 Pd1 115.94(17) . . ? C1 N3 Pd1 129.4(2) . . ? N2' N1' O1' 122.0(3) . . ? N2' N1' C11' 121.8(3) . . ? O1' N1' C11' 116.2(3) . . ? N1' N2' N3' 113.4(3) . . ? N2' N3' C1' 113.7(2) . . ? N2' N3' Pd1 116.35(18) . . ? C1' N3' Pd1 129.5(2) . . ? C6 C1 C2 122.2(3) . . ? C6 C1 N3 115.5(3) . . ? C2 C1 N3 122.1(4) . . ? C3 C2 C1 113.0(4) . . ? C3 C2 C7 120.7(3) . . ? C1 C2 C7 126.3(3) . . ? C4 C3 C2 125.0(4) . . ? C3 C4 C5 120.4(3) . . ? C4 C5 C6 117.8(6) . . ? C1 C6 C5 121.6(4) . . ? C2 C7 C9 110.0(5) . . ? C2 C7 C8 112.1(4) . . ? C9 C7 C8 107.0(5) . . ? C2 C7 C10 112.4(4) . . ? C9 C7 C10 110.3(5) . . ? C8 C7 C10 104.8(5) . . ? C2' C1' C6' 122.5(3) . . ? C2' C1' N3' 123.5(3) . . ? C6' C1' N3' 113.9(4) . . ? C1' C2' C3' 115.7(3) . . ? C1' C2' C7' 125.7(3) . . ? C3' C2' C7' 118.7(4) . . ? C4' C3' C2' 122.0(5) . . ? C5' C4' C3' 121.1(3) . . ? C4' C5' C6' 119.8(4) . . ? C5' C6' C1' 118.9(5) . . ? C9' C7' C8' 105.3(6) . . ? C9' C7' C2' 110.1(4) . . ? C8' C7' C2' 112.4(3) . . ? C9' C7' C10' 109.5(5) . . ? C8' C7' C10' 108.9(7) . . ? C2' C7' C10' 110.6(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3' Pd1 O1 N1 -176.7(3) . . . . ? N3 Pd1 O1 N1 -0.4(3) . . . . ? O1' Pd1 O1 N1 99.0(11) . . . . ? N3' Pd1 O1' N1' -3.8(3) . . . . ? N3 Pd1 O1' N1' 179.9(3) . . . . ? O1 Pd1 O1' N1' 81.3(12) . . . . ? Pd1 O1 N1 N2 -0.1(4) . . . . ? Pd1 O1 N1 C11 179.2(4) . . . . ? O1 N1 N2 N3 0.9(5) . . . . ? C11 N1 N2 N3 -178.4(5) . . . . ? N1 N2 N3 C1 177.4(3) . . . . ? N1 N2 N3 Pd1 -1.2(4) . . . . ? N3' Pd1 N3 N2 83.2(16) . . . . ? O1 Pd1 N3 N2 0.9(3) . . . . ? O1' Pd1 N3 N2 -174.7(3) . . . . ? N3' Pd1 N3 C1 -95.2(16) . . . . ? O1 Pd1 N3 C1 -177.5(4) . . . . ? O1' Pd1 N3 C1 6.9(4) . . . . ? Pd1 O1' N1' N2' 2.6(4) . . . . ? Pd1 O1' N1' C11' -176.1(4) . . . . ? O1' N1' N2' N3' 1.5(5) . . . . ? C11' N1' N2' N3' -179.9(5) . . . . ? N1' N2' N3' C1' -177.6(3) . . . . ? N1' N2' N3' Pd1 -5.0(4) . . . . ? N3 Pd1 N3' N2' 107.8(16) . . . . ? O1 Pd1 N3' N2' -170.6(3) . . . . ? O1' Pd1 N3' N2' 5.0(3) . . . . ? N3 Pd1 N3' C1' -81.0(16) . . . . ? O1 Pd1 N3' C1' 0.5(3) . . . . ? O1' Pd1 N3' C1' 176.2(3) . . . . ? N2 N3 C1 C6 111.8(4) . . . . ? Pd1 N3 C1 C6 -69.8(4) . . . . ? N2 N3 C1 C2 -72.5(4) . . . . ? Pd1 N3 C1 C2 105.9(4) . . . . ? C6 C1 C2 C3 -2.9(5) . . . . ? N3 C1 C2 C3 -178.3(3) . . . . ? C6 C1 C2 C7 178.9(4) . . . . ? N3 C1 C2 C7 3.4(6) . . . . ? C1 C2 C3 C4 0.7(6) . . . . ? C7 C2 C3 C4 179.0(5) . . . . ? C2 C3 C4 C5 0.8(7) . . . . ? C3 C4 C5 C6 -0.1(7) . . . . ? C2 C1 C6 C5 3.7(6) . . . . ? N3 C1 C6 C5 179.4(3) . . . . ? C4 C5 C6 C1 -2.1(6) . . . . ? C3 C2 C7 C9 -100.4(4) . . . . ? C1 C2 C7 C9 77.8(5) . . . . ? C3 C2 C7 C8 18.6(6) . . . . ? C1 C2 C7 C8 -163.3(5) . . . . ? C3 C2 C7 C10 136.2(4) . . . . ? C1 C2 C7 C10 -45.6(6) . . . . ? N2' N3' C1' C2' -106.6(4) . . . . ? Pd1 N3' C1' C2' 82.1(4) . . . . ? N2' N3' C1' C6' 76.3(4) . . . . ? Pd1 N3' C1' C6' -95.0(4) . . . . ? C6' C1' C2' C3' 0.9(5) . . . . ? N3' C1' C2' C3' -176.0(3) . . . . ? C6' C1' C2' C7' -179.3(4) . . . . ? N3' C1' C2' C7' 3.9(6) . . . . ? C1' C2' C3' C4' -1.1(5) . . . . ? C7' C2' C3' C4' 179.0(4) . . . . ? C2' C3' C4' C5' 0.8(6) . . . . ? C3' C4' C5' C6' -0.1(6) . . . . ? C4' C5' C6' C1' -0.2(5) . . . . ? C2' C1' C6' C5' -0.2(5) . . . . ? N3' C1' C6' C5' 176.9(3) . . . . ? C1' C2' C7' C9' -75.0(5) . . . . ? C3' C2' C7' C9' 104.8(4) . . . . ? C1' C2' C7' C8' 168.0(6) . . . . ? C3' C2' C7' C8' -12.2(7) . . . . ? C1' C2' C7' C10' 46.1(7) . . . . ? C3' C2' C7' C10' -134.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.568 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.568 _refine_diff_density_max 0.214 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.042 #===END data_cmpd_5 _database_code_CSD 153407 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C18 H28 N6 O2 Pd' _chemical_formula_weight 466.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 10.307(2) _cell_length_b 7.982(2) _cell_length_c 13.628(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.12(3) _cell_angle_gamma 90.00 _cell_volume 1112.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 0.857 _exptl_absorpt_correction_T_min 0.8473 _exptl_absorpt_correction_T_max 0.8822 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 7074 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0152 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 29.10 _reflns_number_total 2708 _reflns_number_gt 2454 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+2.0843P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0073(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2708 _refine_ls_number_parameters 135 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1166 _refine_ls_wR_factor_gt 0.1138 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.003 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.5000 0.0000 0.5000 0.03191(15) Uani 1 d S . . O1 O 0.3273(2) -0.1151(3) 0.49214(17) 0.0452(6) Uani 1 d . . . N1 N 0.2774(3) -0.0885(5) 0.5782(2) 0.0491(7) Uani 1 d . . . N2 N 0.3380(3) -0.0077(4) 0.6507(2) 0.0437(7) Uani 1 d . . . N3 N 0.4499(3) 0.0540(4) 0.6328(2) 0.0387(6) Uani 1 d . . . C1 C 0.5268(3) 0.1250(4) 0.7174(2) 0.0386(6) Uani 1 d . . . C2 C 0.5607(4) 0.2953(5) 0.7145(3) 0.0476(8) Uani 1 d . . . C3 C 0.6409(4) 0.3607(6) 0.7958(3) 0.0589(10) Uani 1 d . . . H3 H 0.6659 0.4726 0.7952 0.071 Uiso 1 calc R . . C4 C 0.6835(4) 0.2638(7) 0.8762(4) 0.0679(13) Uani 1 d . . . H4 H 0.7352 0.3105 0.9300 0.081 Uiso 1 calc R . . C5 C 0.6497(4) 0.0979(6) 0.8773(3) 0.0615(11) Uani 1 d . . . H5 H 0.6795 0.0330 0.9322 0.074 Uiso 1 calc R . . C6 C 0.5718(4) 0.0240(5) 0.7980(3) 0.0466(8) Uani 1 d . . . C7 C 0.5437(5) -0.1600(6) 0.8009(3) 0.0667(12) Uani 1 d . . . H71 H 0.6205 -0.2192 0.8318 0.080 Uiso 1 d . . . H72 H 0.5254 -0.2035 0.7346 0.080 Uiso 1 d . . . H73 H 0.4713 -0.1830 0.8371 0.080 Uiso 0.63 d P . . C8 C 0.5111(6) 0.4049(6) 0.6287(4) 0.0689(13) Uani 1 d . . . H81 H 0.5144 0.3429 0.5679 0.080 Uiso 1 d . . . H82 H 0.5676 0.5002 0.6266 0.080 Uiso 1 d . . . H83 H 0.4234 0.4401 0.6332 0.080 Uiso 0.37 d P . . C9 C 0.3793(9) 0.4622(12) 0.6323(7) 0.072(3) Uiso 0.628(14) d P . . H91 H 0.3515 0.5302 0.5761 0.080 Uiso 0.63 d P . . H92 H 0.3222 0.3661 0.6326 0.080 Uiso 0.63 d P . . H93 H 0.3759 0.5249 0.6919 0.080 Uiso 0.63 d P . . C10 C 0.1502(4) -0.1622(8) 0.5840(4) 0.0743(15) Uani 1 d . . . H101 H 0.1214 -0.1335 0.6462 0.111 Uiso 1 calc R . . H102 H 0.1562 -0.2818 0.5787 0.111 Uiso 1 calc R . . H103 H 0.0889 -0.1201 0.5310 0.111 Uiso 1 calc R . . C11 C 0.4370(16) -0.200(2) 0.8530(12) 0.084(5) Uiso 0.372(14) d P . . H111 H 0.4256 -0.3177 0.8523 0.080 Uiso 0.37 d P . . H112 H 0.4585 -0.1599 0.9193 0.080 Uiso 0.37 d P . . H113 H 0.3624 -0.1440 0.8212 0.080 Uiso 0.37 d P . . 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 0.0325(2) 0.0369(2) 0.0270(2) -0.00006(11) 0.00649(12) 0.00008(11) O1 0.0431(12) 0.0588(15) 0.0350(11) -0.0042(10) 0.0096(9) -0.0078(11) N1 0.0415(15) 0.069(2) 0.0383(15) -0.0080(14) 0.0125(12) -0.0118(14) N2 0.0389(15) 0.0589(19) 0.0352(15) -0.0059(11) 0.0128(12) -0.0067(11) N3 0.0376(13) 0.0476(14) 0.0321(13) -0.0032(12) 0.0086(10) -0.0014(12) C1 0.0387(15) 0.0422(16) 0.0363(15) -0.0061(13) 0.0104(12) -0.0030(12) C2 0.053(2) 0.0450(18) 0.0483(19) -0.0060(15) 0.0185(16) -0.0038(15) C3 0.055(2) 0.056(2) 0.068(3) -0.024(2) 0.020(2) -0.0160(18) C4 0.054(2) 0.086(3) 0.063(3) -0.034(2) 0.003(2) -0.011(2) C5 0.057(2) 0.078(3) 0.047(2) -0.009(2) -0.0038(17) 0.005(2) C6 0.048(2) 0.053(2) 0.0392(18) -0.0063(15) 0.0047(15) 0.0024(15) C7 0.092(3) 0.051(2) 0.054(2) 0.0067(19) -0.002(2) 0.002(2) C8 0.103(4) 0.048(2) 0.060(3) 0.0090(19) 0.030(2) 0.000(2) C10 0.051(2) 0.110(4) 0.066(3) -0.018(3) 0.022(2) -0.027(2) 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 N3 1.990(3) 3_656 ? Pd1 N3 1.990(3) . ? Pd1 O1 1.994(2) 3_656 ? Pd1 O1 1.994(2) . ? O1 N1 1.355(4) . ? N1 N2 1.276(4) . ? N1 C10 1.448(5) . ? N2 N3 1.304(4) . ? N3 C1 1.432(4) . ? C1 C6 1.395(5) . ? C1 C2 1.406(5) . ? C2 C3 1.398(6) . ? C2 C8 1.499(6) . ? C3 C4 1.368(7) . ? C4 C5 1.369(7) . ? C5 C6 1.394(6) . ? C6 C7 1.499(6) . ? C7 C11 1.417(17) . ? C8 C9 1.441(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Pd1 N3 180.0 3_656 . ? N3 Pd1 O1 79.53(11) 3_656 3_656 ? N3 Pd1 O1 100.47(11) . 3_656 ? N3 Pd1 O1 100.47(11) 3_656 . ? N3 Pd1 O1 79.53(11) . . ? O1 Pd1 O1 180.0 3_656 . ? N1 O1 Pd1 108.24(19) . . ? N2 N1 O1 123.2(3) . . ? N2 N1 C10 121.5(3) . . ? O1 N1 C10 115.3(3) . . ? N1 N2 N3 113.9(3) . . ? N2 N3 C1 114.4(3) . . ? N2 N3 Pd1 115.0(2) . . ? C1 N3 Pd1 129.6(2) . . ? C6 C1 C2 121.4(3) . . ? C6 C1 N3 120.1(3) . . ? C2 C1 N3 118.4(3) . . ? C3 C2 C1 117.6(4) . . ? C3 C2 C8 120.8(4) . . ? C1 C2 C8 121.6(4) . . ? C4 C3 C2 121.5(4) . . ? C3 C4 C5 119.9(4) . . ? C4 C5 C6 121.6(4) . . ? C1 C6 C5 118.0(4) . . ? C1 C6 C7 122.7(4) . . ? C5 C6 C7 119.3(4) . . ? C11 C7 C6 113.4(8) . . ? C9 C8 C2 113.0(5) . . ? _diffrn_measured_fraction_theta_max 0.852 _diffrn_reflns_theta_full 29.10 _diffrn_measured_fraction_theta_full 0.852 _refine_diff_density_max 1.878 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.095 #===END data_cmpd_6 _database_code_CSD 178676 _audit_creation_method SHELXL _chemical_name_systematic ? _chemical_formula_sum 'C16 H20 N6 O2 Pd' _chemical_formula_weight 434.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.223(2) _cell_length_b 8.536(2) _cell_length_c 14.290(3) _cell_angle_alpha 103.96(3) _cell_angle_beta 95.80(3) _cell_angle_gamma 107.42(3) _cell_volume 912.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.583 _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 1.039 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 3458 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3215 _reflns_number_observed 2929 _reflns_observed_criterion >2sigma(I) _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+0.2015P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_extinction_method none _refine_ls_number_reflns 3215 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_obs 0.0211 _refine_ls_wR_factor_all 0.0586 _refine_ls_wR_factor_obs 0.0573 _refine_ls_goodness_of_fit_all 1.086 _refine_ls_goodness_of_fit_obs 1.119 _refine_ls_restrained_S_all 1.086 _refine_ls_restrained_S_obs 1.119 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.05285(2) 0.34580(2) 0.406007(11) 0.03240(7) Uani 1 d . . O1 O 0.3022(2) 0.4948(2) 0.43937(13) 0.0467(4) Uani 1 d . . O1' O 0.0573(2) 0.2660(2) 0.52718(12) 0.0432(4) Uani 1 d . . N1 N 0.3403(3) 0.5692(3) 0.3675(2) 0.0448(5) Uani 1 d . . N1' N -0.1045(3) 0.1708(3) 0.52923(15) 0.0428(4) Uani 1 d . . N2 N 0.2279(3) 0.5476(3) 0.29319(15) 0.0434(5) Uani 1 d . . N2' N -0.2327(3) 0.1281(2) 0.45837(14) 0.0409(4) Uani 1 d . . N3 N 0.0721(2) 0.4416(3) 0.29153(14) 0.0386(4) Uani 1 d . . N3' N -0.1910(2) 0.1873(2) 0.38370(14) 0.0377(4) Uani 1 d . . C1 C -0.0560(3) 0.4284(3) 0.2110(2) 0.0378(5) Uani 1 d . . C1' C -0.3382(3) 0.1413(3) 0.3074(2) 0.0374(5) Uani 1 d . . C2 C -0.0425(3) 0.3667(3) 0.1127(2) 0.0463(5) Uani 1 d . . C2' C -0.3398(3) 0.0415(3) 0.2140(2) 0.0428(5) Uani 1 d . . C3 C -0.1741(4) 0.3604(4) 0.0409(2) 0.0566(7) Uani 1 d . . C3' C -0.4854(4) 0.0011(4) 0.1415(2) 0.0559(7) Uani 1 d . . C4 C -0.3141(4) 0.4084(4) 0.0637(2) 0.0585(7) Uani 1 d . . C4' C -0.6239(4) 0.0554(4) 0.1617(2) 0.0610(7) Uani 1 d . . C5 C -0.3270(4) 0.4653(4) 0.1607(2) 0.0527(6) Uani 1 d . . C5' C -0.6204(4) 0.1544(4) 0.2549(2) 0.0526(6) Uani 1 d . . C6 C -0.1986(3) 0.4755(3) 0.2339(2) 0.0439(5) Uani 1 d . . C6' C -0.4766(3) 0.1987(3) 0.3281(2) 0.0445(5) Uani 1 d . . C7 C 0.1042(5) 0.3051(6) 0.0841(2) 0.0651(8) Uani 1 d . . C7' C -0.1945(4) -0.0257(4) 0.1910(2) 0.0575(7) Uani 1 d . . C8 C 0.5145(4) 0.6937(5) 0.3852(3) 0.0650(8) Uani 1 d . . C8' C -0.1265(5) 0.0987(4) 0.6120(2) 0.0528(6) Uani 1 d . . H3 H -0.1754(45) 0.3235(45) -0.0172(26) 0.073(10) Uiso 1 d . . H4 H -0.3961(44) 0.4063(41) 0.0146(24) 0.068(9) Uiso 1 d . . H5 H -0.4167(43) 0.4904(40) 0.1718(23) 0.064(9) Uiso 1 d . . H6 H -0.2028(34) 0.5114(34) 0.2996(20) 0.045(7) Uiso 1 d . . H71 H 0.0950(64) 0.2470(63) 0.0107(39) 0.130(17) Uiso 1 d . . H72 H 0.1329(59) 0.2412(61) 0.1275(34) 0.118(15) Uiso 1 d . . H73 H 0.2015(49) 0.3974(49) 0.0987(26) 0.073(11) Uiso 1 d . . H81 H 0.5126(46) 0.7971(48) 0.4373(28) 0.081(11) Uiso 1 d . . H82 H 0.5218(47) 0.7353(47) 0.3284(28) 0.077(11) Uiso 1 d . . H83 H 0.5881(56) 0.6505(52) 0.4100(30) 0.093(14) Uiso 1 d . . H2' H -0.4711(35) 0.2637(37) 0.3891(21) 0.046(7) Uiso 1 d . . H3' H -0.4880(42) -0.0708(42) 0.0782(25) 0.068(9) Uiso 1 d . . H4' H -0.7167(47) 0.0211(43) 0.1098(25) 0.078(10) Uiso 1 d . . H5' H -0.7105(45) 0.1943(42) 0.2647(23) 0.069(9) Uiso 1 d . . H71' H -0.2191(62) -0.0846(60) 0.1286(36) 0.118(16) Uiso 1 d . . H72' H -0.1914(50) -0.0939(52) 0.2233(28) 0.084(13) Uiso 1 d . . H73' H -0.0810(47) 0.0622(45) 0.2139(24) 0.068(9) Uiso 1 d . . H81' H -0.0810(45) 0.0144(47) 0.6118(25) 0.075(10) Uiso 1 d . . H82' H -0.2513(57) 0.0510(52) 0.6078(28) 0.095(13) Uiso 1 d . . H83' H -0.0742(48) 0.1870(50) 0.6708(28) 0.084(11) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02854(10) 0.03201(11) 0.03334(11) 0.00655(7) 0.00181(7) 0.00891(7) O1 0.0328(8) 0.0526(10) 0.0457(9) 0.0112(8) 0.0005(7) 0.0063(7) O1' 0.0408(9) 0.0460(9) 0.0402(9) 0.0131(7) 0.0011(7) 0.0124(7) N1 0.0324(10) 0.0452(11) 0.0488(12) 0.0083(9) 0.0075(9) 0.0056(9) N1' 0.0458(11) 0.0414(11) 0.0396(10) 0.0154(8) 0.0045(9) 0.0103(9) N2 0.0389(11) 0.0411(11) 0.0472(11) 0.0115(9) 0.0110(9) 0.0090(9) N2' 0.0428(11) 0.0363(10) 0.0408(10) 0.0129(8) 0.0046(8) 0.0088(8) N3 0.0333(10) 0.0397(10) 0.0399(10) 0.0120(8) 0.0061(8) 0.0077(8) N3' 0.0354(10) 0.0358(10) 0.0368(10) 0.0100(8) 0.0011(8) 0.0067(8) C1 0.0388(12) 0.0318(11) 0.0420(12) 0.0141(9) 0.0052(9) 0.0085(9) C1' 0.0338(11) 0.0320(11) 0.0405(11) 0.0115(9) 0.0006(9) 0.0038(9) C2 0.0554(14) 0.0449(13) 0.0429(13) 0.0173(10) 0.0095(11) 0.0189(11) C2' 0.0448(12) 0.0344(11) 0.0436(12) 0.0073(9) 0.0009(10) 0.0106(10) C3 0.073(2) 0.058(2) 0.0388(14) 0.0142(12) 0.0019(13) 0.0235(14) C3' 0.062(2) 0.0496(15) 0.0441(14) 0.0007(12) -0.0073(12) 0.0168(13) C4 0.058(2) 0.056(2) 0.060(2) 0.0207(14) -0.0078(14) 0.0191(13) C4' 0.048(2) 0.059(2) 0.062(2) 0.0087(14) -0.0162(13) 0.0135(13) C5 0.0450(15) 0.0468(15) 0.068(2) 0.0165(13) 0.0040(12) 0.0196(12) C5' 0.0368(13) 0.057(2) 0.063(2) 0.0186(13) 0.0038(12) 0.0148(12) C6 0.0429(13) 0.0375(12) 0.0476(14) 0.0093(10) 0.0061(10) 0.0113(10) C6' 0.0378(12) 0.0481(14) 0.0458(13) 0.0132(11) 0.0085(10) 0.0118(10) C7 0.075(2) 0.086(2) 0.051(2) 0.024(2) 0.020(2) 0.045(2) C7' 0.061(2) 0.053(2) 0.053(2) 0.0004(14) 0.0011(14) 0.0267(15) C8 0.0372(15) 0.069(2) 0.070(2) 0.011(2) 0.0106(14) -0.0035(14) C8' 0.072(2) 0.0464(15) 0.0448(15) 0.0212(12) 0.0094(13) 0.0206(14) 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 N3 1.998(2) . ? Pd1 N3' 1.998(2) . ? Pd1 O1 1.999(2) . ? Pd1 O1' 2.009(2) . ? O1 N1 1.348(3) . ? O1' N1' 1.344(3) . ? N1 N2 1.273(3) . ? N1 C8 1.459(3) . ? N1' N2' 1.283(3) . ? N1' C8' 1.463(3) . ? N2 N3 1.323(3) . ? N2' N3' 1.320(3) . ? N3 C1 1.438(3) . ? N3' C1' 1.432(3) . ? C1 C6 1.394(3) . ? C1 C2 1.404(3) . ? C1' C2' 1.395(3) . ? C1' C6' 1.399(3) . ? C2 C3 1.394(4) . ? C2 C7 1.508(4) . ? C2' C3' 1.399(4) . ? C2' C7' 1.504(4) . ? C3 C4 1.375(4) . ? C3' C4' 1.383(4) . ? C4 C5 1.380(4) . ? C4' C5' 1.387(4) . ? C5 C6 1.376(4) . ? C5' C6' 1.388(4) . ? 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 N3 Pd1 N3' 106.67(8) . . ? N3 Pd1 O1 79.00(8) . . ? N3' Pd1 O1 174.22(7) . . ? N3 Pd1 O1' 174.29(7) . . ? N3' Pd1 O1' 78.99(8) . . ? O1 Pd1 O1' 95.34(8) . . ? N1 O1 Pd1 109.32(13) . . ? N1' O1' Pd1 108.81(13) . . ? N2 N1 O1 122.9(2) . . ? N2 N1 C8 120.9(2) . . ? O1 N1 C8 115.8(2) . . ? N2' N1' O1' 123.0(2) . . ? N2' N1' C8' 119.9(2) . . ? O1' N1' C8' 116.7(2) . . ? N1 N2 N3 113.9(2) . . ? N1' N2' N3' 113.8(2) . . ? N2 N3 C1 113.1(2) . . ? N2 N3 Pd1 114.9(2) . . ? C1 N3 Pd1 131.77(15) . . ? N2' N3' C1' 112.1(2) . . ? N2' N3' Pd1 114.75(15) . . ? C1' N3' Pd1 132.54(15) . . ? C6 C1 C2 120.4(2) . . ? C6 C1 N3 117.3(2) . . ? C2 C1 N3 122.2(2) . . ? C2' C1' C6' 121.5(2) . . ? C2' C1' N3' 119.4(2) . . ? C6' C1' N3' 119.1(2) . . ? C3 C2 C1 117.1(2) . . ? C3 C2 C7 120.4(3) . . ? C1 C2 C7 122.5(2) . . ? C1' C2' C3' 117.4(2) . . ? C1' C2' C7' 122.3(2) . . ? C3' C2' C7' 120.3(2) . . ? C4 C3 C2 122.3(3) . . ? C4' C3' C2' 121.5(3) . . ? C3 C4 C5 119.8(3) . . ? C3' C4' C5' 120.4(3) . . ? C6 C5 C4 119.7(3) . . ? C4' C5' C6' 119.5(3) . . ? C5 C6 C1 120.6(3) . . ? C5' C6' C1' 119.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Pd1 O1 N1 -1.16(14) . . . . ? N3' Pd1 O1 N1 168.3(6) . . . . ? O1' Pd1 O1 N1 179.69(14) . . . . ? N3 Pd1 O1' N1' 166.1(6) . . . . ? N3' Pd1 O1' N1' -6.63(14) . . . . ? O1 Pd1 O1' N1' 174.53(14) . . . . ? Pd1 O1 N1 N2 2.1(3) . . . . ? Pd1 O1 N1 C8 175.0(2) . . . . ? Pd1 O1' N1' N2' 6.2(3) . . . . ? Pd1 O1' N1' C8' 179.1(2) . . . . ? O1 N1 N2 N3 -2.0(3) . . . . ? C8 N1 N2 N3 -174.5(3) . . . . ? O1' N1' N2' N3' -0.4(3) . . . . ? C8' N1' N2' N3' -173.1(2) . . . . ? N1 N2 N3 C1 175.8(2) . . . . ? N1 N2 N3 Pd1 0.7(3) . . . . ? N3' Pd1 N3 N2 -178.6(2) . . . . ? O1 Pd1 N3 N2 0.3(2) . . . . ? O1' Pd1 N3 N2 8.8(8) . . . . ? N3' Pd1 N3 C1 7.5(2) . . . . ? O1 Pd1 N3 C1 -173.6(2) . . . . ? O1' Pd1 N3 C1 -165.1(6) . . . . ? N1' N2' N3' C1' -178.3(2) . . . . ? N1' N2' N3' Pd1 -5.9(2) . . . . ? N3 Pd1 N3' N2' -172.2(2) . . . . ? O1 Pd1 N3' N2' 18.6(8) . . . . ? O1' Pd1 N3' N2' 7.1(2) . . . . ? N3 Pd1 N3' C1' -1.7(2) . . . . ? O1 Pd1 N3' C1' -171.0(6) . . . . ? O1' Pd1 N3' C1' 177.5(2) . . . . ? N2 N3 C1 C6 -119.8(2) . . . . ? Pd1 N3 C1 C6 54.2(3) . . . . ? N2 N3 C1 C2 61.8(3) . . . . ? Pd1 N3 C1 C2 -124.3(2) . . . . ? N2' N3' C1' C2' -119.2(2) . . . . ? Pd1 N3' C1' C2' 70.1(3) . . . . ? N2' N3' C1' C6' 61.2(3) . . . . ? Pd1 N3' C1' C6' -109.4(2) . . . . ? C6 C1 C2 C3 1.9(3) . . . . ? N3 C1 C2 C3 -179.7(2) . . . . ? C6 C1 C2 C7 -176.6(3) . . . . ? N3 C1 C2 C7 1.8(4) . . . . ? C6' C1' C2' C3' 0.2(4) . . . . ? N3' C1' C2' C3' -179.4(2) . . . . ? C6' C1' C2' C7' -178.2(3) . . . . ? N3' C1' C2' C7' 2.3(4) . . . . ? C1 C2 C3 C4 -1.4(4) . . . . ? C7 C2 C3 C4 177.2(3) . . . . ? C1' C2' C3' C4' -1.0(4) . . . . ? C7' C2' C3' C4' 177.4(3) . . . . ? C2 C3 C4 C5 0.1(5) . . . . ? C2' C3' C4' C5' 1.0(5) . . . . ? C3 C4 C5 C6 0.8(4) . . . . ? C3' C4' C5' C6' -0.1(5) . . . . ? C4 C5 C6 C1 -0.2(4) . . . . ? C2 C1 C6 C5 -1.1(4) . . . . ? N3 C1 C6 C5 -179.6(2) . . . . ? C4' C5' C6' C1' -0.8(4) . . . . ? C2' C1' C6' C5' 0.7(4) . . . . ? N3' C1' C6' C5' -179.7(2) . . . . ? _refine_diff_density_max 0.520 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.057 #===END data_cmpd_7 _database_code_CSD 153415 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C18 H24 N6 O2 Pd' _chemical_formula_weight 462.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.098(2) _cell_length_b 9.918(2) _cell_length_c 13.036(3) _cell_angle_alpha 88.08(3) _cell_angle_beta 74.01(3) _cell_angle_gamma 65.39(3) _cell_volume 1023.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 0.931 _exptl_absorpt_correction_T_min 0.7071 _exptl_absorpt_correction_T_max 0.8357 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 7009 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 28.90 _reflns_number_total 4659 _reflns_number_gt 3952 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1038P)^2^+2.1631P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.028(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4659 _refine_ls_number_parameters 251 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.1907 _refine_ls_wR_factor_gt 0.1772 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.08127(4) 0.70058(4) 0.14853(3) 0.0485(2) Uani 1 d . . . O1 O 0.3178(5) 0.5440(4) 0.0913(4) 0.0529(9) Uani 1 d . . . O1' O 0.1380(5) 0.8740(4) 0.1071(4) 0.0514(9) Uani 1 d . . . N1 N 0.3187(6) 0.4091(5) 0.1040(4) 0.0502(10) Uani 1 d . . . N2 N 0.1854(6) 0.3909(5) 0.1470(4) 0.0518(10) Uani 1 d . . . N3 N 0.0466(5) 0.5157(5) 0.1781(4) 0.0464(9) Uani 1 d . . . N1' N -0.0067(6) 1.0011(4) 0.1356(4) 0.0494(10) Uani 1 d . . . N2' N -0.1492(6) 1.0032(5) 0.1820(4) 0.0502(10) Uani 1 d . . . N3' N -0.1460(5) 0.8711(5) 0.2030(4) 0.0476(10) Uani 1 d . . . C1 C -0.0997(6) 0.4907(5) 0.2228(5) 0.0471(11) Uani 1 d . . . C2 C -0.1216(8) 0.4220(7) 0.3174(5) 0.0564(13) Uani 1 d . . . C3 C -0.2678(9) 0.3983(9) 0.3536(5) 0.0668(16) Uani 1 d . . . H3 H -0.2819 0.3495 0.4153 0.080 Uiso 1 calc R . . C4 C -0.3931(8) 0.4440(8) 0.3019(5) 0.0605(14) Uani 1 d . . . C5 C -0.3679(7) 0.5138(7) 0.2082(5) 0.0556(13) Uani 1 d . . . H5 H -0.4490 0.5451 0.1715 0.067 Uiso 1 calc R . . C6 C -0.2237(7) 0.5368(6) 0.1695(5) 0.0525(12) Uani 1 d . . . H6 H -0.2090 0.5837 0.1070 0.063 Uiso 1 calc R . . C7 C 0.0092(11) 0.3686(11) 0.3777(7) 0.083(2) Uani 1 d . . . H71 H -0.0438 0.3637 0.4515 0.124 Uiso 1 calc R . . H72 H 0.0605 0.4367 0.3731 0.124 Uiso 1 calc R . . H73 H 0.0942 0.2715 0.3468 0.124 Uiso 1 calc R . . C8 C -0.5483(11) 0.4146(13) 0.3443(7) 0.095(3) Uani 1 d . . . H81 H -0.5192 0.3113 0.3284 0.143 Uiso 1 calc R . . H82 H -0.6330 0.4747 0.3110 0.143 Uiso 1 calc R . . H83 H -0.5914 0.4393 0.4205 0.143 Uiso 1 calc R . . C9 C 0.4828(8) 0.2818(7) 0.0619(7) 0.0713(18) Uani 1 d . . . H91 H 0.4687 0.1910 0.0704 0.107 Uiso 1 calc R . . H92 H 0.5585 0.2822 0.1005 0.107 Uiso 1 calc R . . H93 H 0.5285 0.2888 -0.0128 0.107 Uiso 1 calc R . . C1' C -0.3107(6) 0.8771(6) 0.2494(5) 0.0508(12) Uani 1 d . . . C2' C -0.3564(7) 0.8422(7) 0.3543(5) 0.0564(13) Uani 1 d . . . C3' C -0.5175(9) 0.8465(8) 0.3934(5) 0.0648(15) Uani 1 d . . . H3' H -0.5509 0.8234 0.4633 0.078 Uiso 1 calc R . . C4' C -0.6306(8) 0.8839(8) 0.3325(6) 0.0689(17) Uani 1 d . . . C5' C -0.5815(8) 0.9166(8) 0.2294(6) 0.0652(16) Uani 1 d . . . H5' H -0.6549 0.9414 0.1872 0.078 Uiso 1 calc R . . C6' C -0.4214(7) 0.9126(7) 0.1876(6) 0.0594(14) Uani 1 d . . . H6' H -0.3882 0.9340 0.1173 0.071 Uiso 1 calc R . . C7' C -0.2383(9) 0.8015(9) 0.4237(6) 0.0742(19) Uani 1 d . . . H71' H -0.3007 0.8068 0.4972 0.111 Uiso 1 calc R . . H72' H -0.1869 0.8698 0.4168 0.111 Uiso 1 calc R . . H73' H -0.1521 0.7020 0.4012 0.111 Uiso 1 calc R . . C8' C -0.8025(10) 0.8830(13) 0.3788(8) 0.100(3) Uani 1 d . . . H81' H -0.8875 0.9718 0.3633 0.150 Uiso 1 calc R . . H82' H -0.8253 0.8795 0.4551 0.150 Uiso 1 calc R . . H83' H -0.8034 0.7972 0.3475 0.150 Uiso 1 calc R . . C9' C 0.0136(8) 1.1383(6) 0.1104(6) 0.0606(14) Uani 1 d . . . H91' H -0.0953 1.2215 0.1282 0.091 Uiso 1 calc R . . H92' H 0.0690 1.1318 0.0354 0.091 Uiso 1 calc R . . H93' H 0.0805 1.1517 0.1513 0.091 Uiso 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 0.0387(3) 0.0333(3) 0.0751(3) 0.00661(18) -0.01690(19) -0.01663(18) O1 0.0359(17) 0.0316(17) 0.086(3) 0.0085(17) -0.0137(17) -0.0124(14) O1' 0.0384(17) 0.0286(16) 0.087(3) 0.0070(16) -0.0183(17) -0.0140(14) N1 0.037(2) 0.0278(19) 0.080(3) 0.0046(19) -0.014(2) -0.0093(16) N2 0.043(2) 0.032(2) 0.080(3) 0.008(2) -0.015(2) -0.0175(17) N3 0.0370(19) 0.0290(19) 0.075(3) 0.0087(18) -0.0174(19) -0.0149(16) N1' 0.042(2) 0.0249(18) 0.082(3) 0.0059(18) -0.019(2) -0.0132(16) N2' 0.041(2) 0.029(2) 0.077(3) 0.0033(19) -0.017(2) -0.0119(16) N3' 0.0362(19) 0.0275(19) 0.072(3) 0.0045(18) -0.0118(18) -0.0096(15) C1 0.041(2) 0.033(2) 0.069(3) 0.001(2) -0.015(2) -0.0170(19) C2 0.056(3) 0.056(3) 0.065(3) 0.007(3) -0.021(3) -0.029(3) C3 0.069(4) 0.080(5) 0.063(3) 0.011(3) -0.016(3) -0.045(4) C4 0.059(3) 0.067(4) 0.069(3) 0.012(3) -0.019(3) -0.039(3) C5 0.047(3) 0.057(3) 0.070(3) 0.012(3) -0.017(2) -0.029(3) C6 0.048(3) 0.038(3) 0.074(3) 0.007(2) -0.021(2) -0.018(2) C7 0.082(5) 0.104(6) 0.089(5) 0.029(4) -0.046(4) -0.053(5) C8 0.073(5) 0.142(9) 0.095(5) 0.017(5) -0.018(4) -0.072(6) C9 0.048(3) 0.034(3) 0.116(5) 0.007(3) -0.011(3) -0.010(2) C1' 0.040(2) 0.032(2) 0.076(3) 0.004(2) -0.015(2) -0.0117(19) C2' 0.049(3) 0.051(3) 0.065(3) -0.003(2) -0.011(2) -0.020(2) C3' 0.057(3) 0.068(4) 0.062(3) 0.000(3) -0.003(3) -0.028(3) C4' 0.042(3) 0.069(4) 0.088(4) -0.008(3) -0.004(3) -0.024(3) C5' 0.043(3) 0.063(4) 0.087(4) 0.005(3) -0.024(3) -0.016(3) C6' 0.044(3) 0.050(3) 0.078(4) 0.015(3) -0.017(3) -0.015(2) C7' 0.061(4) 0.084(5) 0.077(4) -0.007(4) -0.022(3) -0.027(4) C8' 0.053(4) 0.137(9) 0.110(6) 0.002(6) -0.013(4) -0.046(5) C9' 0.062(3) 0.032(3) 0.091(4) 0.004(3) -0.025(3) -0.021(2) 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 N3 1.994(4) . ? Pd1 N3' 2.000(4) . ? Pd1 O1 2.002(4) . ? Pd1 O1' 2.010(4) . ? O1 N1 1.340(6) . ? O1' N1' 1.356(6) . ? N1 N2 1.272(6) . ? N1 C9 1.466(7) . ? N2 N3 1.320(6) . ? N3 C1 1.418(6) . ? N1' N2' 1.263(6) . ? N1' C9' 1.463(7) . ? N2' N3' 1.319(6) . ? N3' C1' 1.429(7) . ? C1 C2 1.395(8) . ? C1 C6 1.395(8) . ? C2 C3 1.398(9) . ? C2 C7 1.509(9) . ? C3 C4 1.390(9) . ? C4 C5 1.394(9) . ? C4 C8 1.512(9) . ? C5 C6 1.380(8) . ? C1' C6' 1.386(8) . ? C1' C2' 1.391(9) . ? C2' C3' 1.396(9) . ? C2' C7' 1.513(9) . ? C3' C4' 1.393(10) . ? C4' C5' 1.368(10) . ? C4' C8' 1.517(9) . ? C5' C6' 1.391(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 N3 Pd1 N3' 106.32(17) . . ? N3 Pd1 O1 79.01(16) . . ? N3' Pd1 O1 174.64(15) . . ? N3 Pd1 O1' 174.13(16) . . ? N3' Pd1 O1' 79.11(16) . . ? O1 Pd1 O1' 95.58(15) . . ? N1 O1 Pd1 109.4(3) . . ? N1' O1' Pd1 108.5(3) . . ? N2 N1 O1 122.6(4) . . ? N2 N1 C9 121.4(5) . . ? O1 N1 C9 115.9(4) . . ? N1 N2 N3 114.5(4) . . ? N2 N3 C1 112.8(4) . . ? N2 N3 Pd1 114.5(3) . . ? C1 N3 Pd1 132.7(3) . . ? N2' N1' O1' 123.3(4) . . ? N2' N1' C9' 121.6(4) . . ? O1' N1' C9' 115.1(4) . . ? N1' N2' N3' 114.4(4) . . ? N2' N3' C1' 112.7(4) . . ? N2' N3' Pd1 114.6(3) . . ? C1' N3' Pd1 132.2(3) . . ? C2 C1 C6 119.9(5) . . ? C2 C1 N3 121.9(5) . . ? C6 C1 N3 118.2(5) . . ? C1 C2 C3 117.7(6) . . ? C1 C2 C7 122.1(6) . . ? C3 C2 C7 120.1(6) . . ? C4 C3 C2 123.1(6) . . ? C3 C4 C5 117.6(5) . . ? C3 C4 C8 120.9(6) . . ? C5 C4 C8 121.5(6) . . ? C6 C5 C4 120.7(6) . . ? C5 C6 C1 120.9(6) . . ? C6' C1' C2' 120.6(5) . . ? C6' C1' N3' 119.2(5) . . ? C2' C1' N3' 120.1(5) . . ? C1' C2' C3' 117.0(6) . . ? C1' C2' C7' 122.0(6) . . ? C3' C2' C7' 120.9(6) . . ? C4' C3' C2' 122.9(6) . . ? C5' C4' C3' 118.7(6) . . ? C5' C4' C8' 120.9(7) . . ? C3' C4' C8' 120.3(7) . . ? C4' C5' C6' 119.9(6) . . ? C1' C6' C5' 120.9(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Pd1 O1 N1 0.4(4) . . . . ? N3' Pd1 O1 N1 174.6(17) . . . . ? O1' Pd1 O1 N1 -177.3(4) . . . . ? N3 Pd1 O1' N1' 156.0(15) . . . . ? N3' Pd1 O1' N1' -2.1(3) . . . . ? O1 Pd1 O1' N1' 178.6(3) . . . . ? Pd1 O1 N1 N2 -0.4(7) . . . . ? Pd1 O1 N1 C9 177.6(5) . . . . ? O1 N1 N2 N3 -0.1(8) . . . . ? C9 N1 N2 N3 -177.9(6) . . . . ? N1 N2 N3 C1 178.3(5) . . . . ? N1 N2 N3 Pd1 0.5(7) . . . . ? N3' Pd1 N3 N2 -179.9(4) . . . . ? O1 Pd1 N3 N2 -0.5(4) . . . . ? O1' Pd1 N3 N2 22.5(18) . . . . ? N3' Pd1 N3 C1 2.7(6) . . . . ? O1 Pd1 N3 C1 -177.9(5) . . . . ? O1' Pd1 N3 C1 -154.9(14) . . . . ? Pd1 O1' N1' N2' 1.2(7) . . . . ? Pd1 O1' N1' C9' -179.9(4) . . . . ? O1' N1' N2' N3' 1.4(8) . . . . ? C9' N1' N2' N3' -177.4(5) . . . . ? N1' N2' N3' C1' -176.4(5) . . . . ? N1' N2' N3' Pd1 -3.3(6) . . . . ? N3 Pd1 N3' N2' -174.7(4) . . . . ? O1 Pd1 N3' N2' 11(2) . . . . ? O1' Pd1 N3' N2' 3.0(4) . . . . ? N3 Pd1 N3' C1' -3.3(6) . . . . ? O1 Pd1 N3' C1' -177.3(16) . . . . ? O1' Pd1 N3' C1' 174.4(6) . . . . ? N2 N3 C1 C2 64.4(7) . . . . ? Pd1 N3 C1 C2 -118.2(6) . . . . ? N2 N3 C1 C6 -115.5(6) . . . . ? Pd1 N3 C1 C6 61.9(7) . . . . ? C6 C1 C2 C3 1.8(9) . . . . ? N3 C1 C2 C3 -178.2(6) . . . . ? C6 C1 C2 C7 179.4(6) . . . . ? N3 C1 C2 C7 -0.6(9) . . . . ? C1 C2 C3 C4 -2.1(10) . . . . ? C7 C2 C3 C4 -179.8(7) . . . . ? C2 C3 C4 C5 1.5(11) . . . . ? C2 C3 C4 C8 179.7(8) . . . . ? C3 C4 C5 C6 -0.4(10) . . . . ? C8 C4 C5 C6 -178.6(7) . . . . ? C4 C5 C6 C1 0.2(9) . . . . ? C2 C1 C6 C5 -0.8(8) . . . . ? N3 C1 C6 C5 179.1(5) . . . . ? N2' N3' C1' C6' 68.3(7) . . . . ? Pd1 N3' C1' C6' -103.2(6) . . . . ? N2' N3' C1' C2' -114.1(6) . . . . ? Pd1 N3' C1' C2' 74.4(7) . . . . ? C6' C1' C2' C3' -0.8(9) . . . . ? N3' C1' C2' C3' -178.3(5) . . . . ? C6' C1' C2' C7' 179.4(6) . . . . ? N3' C1' C2' C7' 1.9(9) . . . . ? C1' C2' C3' C4' -0.1(10) . . . . ? C7' C2' C3' C4' 179.7(7) . . . . ? C2' C3' C4' C5' 0.6(11) . . . . ? C2' C3' C4' C8' 178.5(8) . . . . ? C3' C4' C5' C6' -0.3(11) . . . . ? C8' C4' C5' C6' -178.2(8) . . . . ? C2' C1' C6' C5' 1.1(9) . . . . ? N3' C1' C6' C5' 178.7(5) . . . . ? C4' C5' C6' C1' -0.6(10) . . . . ? _diffrn_measured_fraction_theta_max 0.862 _diffrn_reflns_theta_full 28.90 _diffrn_measured_fraction_theta_full 0.862 _refine_diff_density_max 2.625 _refine_diff_density_min -1.644 _refine_diff_density_rms 0.135 #===END