Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'M. Hardie' _publ_contact_author_address ; School of Chemistry University of Leeds Woodhouse Lane Leeds LS2 9JT UNITED KINGDOM ; _publ_contact_author_email M.J.HARDIE@LEEDS.AC.UK _publ_section_title ; Flattened trigonal bipyramidal coordination assembly with trans geometry ; loop_ _publ_author_name 'M. Hardie' 'Julie Fisher' 'Lindsay P. Harding' 'Aleema Westcott' data_complex1 _database_code_depnum_ccdc_archive 'CCDC 662140' _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexaacetobis{N,N_,N__-tris(6-methyl-2-pyridyl) benzene-1,3,5-tricarboxamide}dipalladium(II) ; _chemical_name_common ; hexaacetobis(N,N_,N__-tris(6-methyl-2-pyridyl) benzene-1,3,5- tricarboxamide)dipalladium(ii) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H66 N12 O18 Pd3' _chemical_formula_weight 1634.51 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' O O 0.0106 0.0060 '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-31c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 22.9258(8) _cell_length_b 22.9258(8) _cell_length_c 19.4600(7) _cell_angle_alpha 90.000(2) _cell_angle_beta 90.000(2) _cell_angle_gamma 120.000(2) _cell_volume 8857.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3312 _exptl_absorpt_coefficient_mu 0.664 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8463 _exptl_absorpt_correction_T_max 0.9246 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 89830 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.56 _reflns_number_total 7526 _reflns_number_gt 4386 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEXII (Bruker, 2004)' _computing_cell_refinement 'APEXII (Bruker, 2004)' _computing_data_reduction 'APEXII (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7526 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1454 _refine_ls_R_factor_gt 0.0901 _refine_ls_wR_factor_ref 0.3460 _refine_ls_wR_factor_gt 0.2838 _refine_ls_goodness_of_fit_ref 1.245 _refine_ls_restrained_S_all 1.245 _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 0.39080(3) 0.27410(3) 0.94840(3) 0.0523(3) Uani 1 1 d . . . O1 O 0.5181(3) 0.1657(3) 0.8355(4) 0.0716(17) Uani 1 1 d . . . N1 N 0.3626(3) 0.1952(3) 0.8800(3) 0.0548(14) Uani 1 1 d . . . C1 C 0.2941(4) 0.1496(5) 0.8729(5) 0.076(3) Uani 1 1 d . . . O2 O 0.6229(4) 0.4663(3) 1.0367(5) 0.099(3) Uani 1 1 d . . . N2 N 0.4753(3) 0.2364(3) 0.8511(3) 0.0492(13) Uani 1 1 d . . . H2 H 0.4849 0.2778 0.8604 0.059 Uiso 1 1 calc R . . C2 C 0.2732(4) 0.0967(5) 0.8313(6) 0.086(3) Uani 1 1 d . . . H2A H 0.2262 0.0659 0.8273 0.103 Uiso 1 1 calc R . . O3 O 0.4176(5) 0.2257(4) 1.0215(5) 0.108(3) Uani 1 1 d . . . N3 N 0.4148(3) 0.3532(3) 1.0153(3) 0.0547(14) Uani 1 1 d . . . C3 C 0.3189(4) 0.0851(4) 0.7929(5) 0.069(2) Uani 1 1 d . . . H3 H 0.3035 0.0470 0.7636 0.082 Uiso 1 1 calc R . . O4 O 0.3275(7) 0.1954(7) 1.0701(12) 0.231(9) Uani 1 1 d . . . N4 N 0.5219(3) 0.3672(3) 1.0277(4) 0.0614(16) Uani 1 1 d . . . H4 H 0.5038 0.3239 1.0188 0.074 Uiso 1 1 calc R . . C4 C 0.3865(4) 0.1311(4) 0.7996(4) 0.0556(17) Uani 1 1 d . . . H4A H 0.4190 0.1260 0.7741 0.067 Uiso 1 1 calc R . . O5 O 0.3696(4) 0.3236(5) 0.8746(4) 0.106(3) Uani 1 1 d . . . C5 C 0.4066(3) 0.1857(3) 0.8444(4) 0.0471(15) Uani 1 1 d . . . O6 O 0.4714(4) 0.3609(4) 0.8465(6) 0.121(3) Uani 1 1 d . . . C6 C 0.2462(5) 0.1651(8) 0.9094(9) 0.151(8) Uani 1 1 d . . . H6A H 0.2005 0.1264 0.9061 0.227 Uiso 1 1 calc R . . H6B H 0.2475 0.2045 0.8882 0.227 Uiso 1 1 calc R . . H6C H 0.2592 0.1746 0.9579 0.227 Uiso 1 1 calc R . . C7 C 0.5276(3) 0.2237(3) 0.8437(4) 0.0495(15) Uani 1 1 d . . . C8 C 0.5997(3) 0.2824(3) 0.8450(3) 0.0425(13) Uani 1 1 d . . . C9 C 0.6159(3) 0.3501(3) 0.8450(3) 0.0446(14) Uani 1 1 d . . . H9 H 0.5813 0.3612 0.8451 0.054 Uiso 1 1 calc R . . C10 C 0.3648(5) 0.3685(5) 1.0287(4) 0.064(2) Uani 1 1 d . . . C11 C 0.3829(6) 0.4282(5) 1.0653(5) 0.080(3) Uani 1 1 d . . . H11 H 0.3495 0.4397 1.0758 0.096 Uiso 1 1 calc R . . C12 C 0.4473(6) 0.4695(5) 1.0859(6) 0.089(3) Uani 1 1 d . . . H12 H 0.4588 0.5105 1.1085 0.107 Uiso 1 1 calc R . . C13 C 0.4970(5) 0.4524(4) 1.0741(5) 0.078(3) Uani 1 1 d . . . H13 H 0.5419 0.4798 1.0900 0.093 Uiso 1 1 calc R . . C14 C 0.4771(4) 0.3927(4) 1.0377(4) 0.0591(18) Uani 1 1 d . . . C15 C 0.2935(6) 0.3194(8) 1.0083(7) 0.112(5) Uani 1 1 d . . . H15A H 0.2888 0.3208 0.9583 0.167 Uiso 1 1 calc R . . H15B H 0.2629 0.3316 1.0310 0.167 Uiso 1 1 calc R . . H15C H 0.2822 0.2739 1.0221 0.167 Uiso 1 1 calc R . . C16 C 0.5927(4) 0.4054(5) 1.0309(5) 0.065(2) Uani 1 1 d . . . C17 C 0.6284(4) 0.3656(4) 1.0282(4) 0.0539(17) Uani 1 1 d . . . C18 C 0.5962(4) 0.2952(4) 1.0296(4) 0.0534(16) Uani 1 1 d . . . H18 H 0.5484 0.2693 1.0315 0.064 Uiso 1 1 calc R . . C19 C 0.3809(10) 0.1987(7) 1.0724(5) 0.117(5) Uani 1 1 d . . . C20 C 0.4069(10) 0.1679(10) 1.1229(9) 0.151(7) Uani 1 1 d . . . H20A H 0.4371 0.2023 1.1556 0.227 Uiso 1 1 calc R . . H20B H 0.4316 0.1496 1.0984 0.227 Uiso 1 1 calc R . . H20C H 0.3690 0.1315 1.1478 0.227 Uiso 1 1 calc R . . C21 C 0.4223(4) 0.3651(5) 0.8374(4) 0.063(2) Uani 1 1 d . . . C22 C 0.4050(8) 0.4034(6) 0.7863(8) 0.125(5) Uani 1 1 d . . . H22A H 0.4465 0.4427 0.7699 0.187 Uiso 1 1 calc R . . H22B H 0.3764 0.4185 0.8084 0.187 Uiso 1 1 calc R . . H22C H 0.3809 0.3741 0.7473 0.187 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 0.0495(4) 0.0610(4) 0.0495(4) -0.0090(2) 0.0037(2) 0.0301(3) O1 0.051(3) 0.048(3) 0.119(5) 0.020(3) 0.020(3) 0.027(2) N1 0.043(3) 0.057(3) 0.056(3) -0.011(3) 0.001(3) 0.018(3) C1 0.047(4) 0.086(6) 0.081(6) -0.025(5) 0.005(4) 0.023(4) O2 0.074(4) 0.055(4) 0.171(8) 0.016(4) -0.003(4) 0.034(3) N2 0.046(3) 0.041(3) 0.056(3) -0.006(2) 0.006(2) 0.017(2) C2 0.051(5) 0.086(6) 0.086(7) -0.024(5) 0.000(4) 0.008(4) O3 0.115(6) 0.080(5) 0.139(7) -0.006(5) 0.021(5) 0.057(5) N3 0.060(4) 0.060(4) 0.054(3) -0.002(3) 0.006(3) 0.038(3) C3 0.066(5) 0.057(5) 0.072(5) -0.016(4) -0.010(4) 0.022(4) O4 0.131(10) 0.169(12) 0.43(3) -0.026(15) -0.049(13) 0.102(10) N4 0.056(4) 0.057(4) 0.073(4) -0.020(3) -0.004(3) 0.030(3) C4 0.054(4) 0.058(4) 0.058(4) -0.006(3) 0.002(3) 0.030(4) O5 0.085(5) 0.136(7) 0.109(6) -0.029(5) -0.001(4) 0.064(5) C5 0.042(3) 0.043(3) 0.053(4) -0.004(3) -0.002(3) 0.018(3) O6 0.109(6) 0.091(5) 0.192(9) -0.069(6) -0.074(6) 0.073(5) C6 0.045(5) 0.184(15) 0.165(14) -0.103(12) 0.012(7) 0.014(7) C7 0.050(4) 0.045(3) 0.052(4) 0.013(3) 0.010(3) 0.022(3) C8 0.047(3) 0.045(3) 0.035(3) 0.008(2) 0.005(2) 0.023(3) C9 0.047(3) 0.049(3) 0.038(3) -0.005(3) 0.000(3) 0.024(3) C10 0.079(6) 0.074(5) 0.057(5) 0.000(4) 0.012(4) 0.051(5) C11 0.108(8) 0.074(6) 0.082(6) 0.005(5) 0.037(5) 0.063(6) C12 0.090(7) 0.050(5) 0.120(9) -0.018(5) 0.031(6) 0.030(5) C13 0.083(6) 0.060(5) 0.083(6) -0.017(4) 0.017(5) 0.030(5) C14 0.067(5) 0.060(4) 0.053(4) 0.002(3) 0.012(4) 0.035(4) C15 0.091(8) 0.170(13) 0.111(9) -0.056(9) -0.004(7) 0.093(9) C16 0.067(5) 0.064(5) 0.068(5) 0.006(4) -0.002(4) 0.034(4) C17 0.062(4) 0.055(4) 0.044(4) 0.003(3) -0.004(3) 0.029(4) C18 0.060(4) 0.061(4) 0.043(3) -0.003(3) -0.001(3) 0.032(4) C19 0.236(17) 0.113(9) 0.057(6) 0.030(6) 0.042(8) 0.129(11) C20 0.175(16) 0.192(17) 0.126(13) 0.060(12) 0.047(11) 0.121(14) C21 0.065(5) 0.071(5) 0.062(5) -0.014(4) 0.000(4) 0.040(4) C22 0.173(14) 0.089(8) 0.129(12) 0.000(8) 0.021(10) 0.077(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 Pd1 O5 2.033(9) . ? Pd1 N3 2.071(6) . ? Pd1 N1 2.071(6) . ? Pd1 O3 2.076(10) . ? O1 C7 1.243(9) . ? N1 C5 1.329(9) . ? N1 C1 1.391(10) . ? C1 C2 1.332(13) . ? C1 C6 1.492(14) . ? O2 C16 1.215(11) . ? N2 C7 1.376(9) . ? N2 C5 1.421(8) . ? C2 C3 1.417(13) . ? O3 C19 1.247(14) . ? N3 C14 1.326(11) . ? N3 C10 1.381(10) . ? C3 C4 1.378(11) . ? O4 C19 1.189(18) . ? N4 C16 1.408(11) . ? N4 C14 1.427(10) . ? C4 C5 1.401(10) . ? O5 C21 1.318(12) . ? O6 C21 1.190(10) . ? C7 C8 1.524(9) . ? C8 C9 1.381(9) 2_655 ? C8 C9 1.402(9) . ? C9 C8 1.381(9) 3_665 ? C10 C11 1.409(12) . ? C10 C15 1.502(15) . ? C11 C12 1.356(14) . ? C12 C13 1.396(13) . ? C13 C14 1.399(11) . ? C16 C17 1.500(11) . ? C17 C18 1.400(11) . ? C17 C18 1.404(11) 3_665 ? C18 C17 1.404(11) 2_655 ? C19 C20 1.50(2) . ? C21 C22 1.506(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 O5 Pd1 N3 89.3(3) . . ? O5 Pd1 N1 88.6(3) . . ? N3 Pd1 N1 177.1(2) . . ? O5 Pd1 O3 176.9(3) . . ? N3 Pd1 O3 91.0(3) . . ? N1 Pd1 O3 91.1(3) . . ? C5 N1 C1 119.3(6) . . ? C5 N1 Pd1 123.1(5) . . ? C1 N1 Pd1 117.6(5) . . ? C2 C1 N1 120.1(8) . . ? C2 C1 C6 122.3(9) . . ? N1 C1 C6 117.5(8) . . ? C7 N2 C5 123.1(6) . . ? C1 C2 C3 121.9(8) . . ? C19 O3 Pd1 120.3(9) . . ? C14 N3 C10 120.9(7) . . ? C14 N3 Pd1 121.9(5) . . ? C10 N3 Pd1 116.7(6) . . ? C4 C3 C2 117.4(8) . . ? C16 N4 C14 125.5(7) . . ? C3 C4 C5 119.0(7) . . ? C21 O5 Pd1 113.7(6) . . ? N1 C5 C4 122.3(6) . . ? N1 C5 N2 116.2(6) . . ? C4 C5 N2 121.5(6) . . ? O1 C7 N2 122.2(6) . . ? O1 C7 C8 118.7(6) . . ? N2 C7 C8 119.1(6) . . ? C9 C8 C9 120.5(7) 2_655 . ? C9 C8 C7 116.2(6) 2_655 . ? C9 C8 C7 123.3(6) . . ? C8 C9 C8 119.5(7) 3_665 . ? N3 C10 C11 117.5(9) . . ? N3 C10 C15 119.4(8) . . ? C11 C10 C15 122.9(8) . . ? C12 C11 C10 121.2(8) . . ? C11 C12 C13 120.8(8) . . ? C12 C13 C14 116.4(9) . . ? N3 C14 C13 123.2(8) . . ? N3 C14 N4 115.2(7) . . ? C13 C14 N4 121.4(8) . . ? O2 C16 N4 122.3(8) . . ? O2 C16 C17 122.2(8) . . ? N4 C16 C17 115.5(7) . . ? C18 C17 C18 119.9(8) . 3_665 ? C18 C17 C16 124.5(7) . . ? C18 C17 C16 115.4(7) 3_665 . ? C17 C18 C17 120.0(8) . 2_655 ? O4 C19 O3 114.8(15) . . ? O4 C19 C20 129.4(16) . . ? O3 C19 C20 115.3(15) . . ? O6 C21 O5 115.0(10) . . ? O6 C21 C22 132.9(11) . . ? O5 C21 C22 111.8(9) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.56 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.414 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.190 #===END data_complex1a _database_code_depnum_ccdc_archive 'CCDC 662141' _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexaacetobis{N,N_,N__-tris(6-methyl-2-pyridyl) benzene-1,3,5-tricarboxamide}dipalladium(II) ; _chemical_name_common ; hexaacetobis(N,N_,N__-tris(6-methyl-2-pyridyl) benzene-1,3,5- tricarboxamide)dipalladium(ii) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H88 N16 O24 Pd4' _chemical_formula_weight 2179.34 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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-31c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 22.6400(11) _cell_length_b 22.6400(11) _cell_length_c 19.219(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8531.2(15) _cell_formula_units_Z 3 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3312 _exptl_absorpt_coefficient_mu 0.689 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8199 _exptl_absorpt_correction_T_max 0.9037 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62587 _diffrn_reflns_av_R_equivalents 0.1100 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 23.25 _reflns_number_total 4080 _reflns_number_gt 2224 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEXII (Bruker, 2004)' _computing_cell_refinement 'APEXII (Bruker, 2004)' _computing_data_reduction 'APEXII (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1097P)^2^+120.1340P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4080 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1866 _refine_ls_R_factor_gt 0.1046 _refine_ls_wR_factor_ref 0.3427 _refine_ls_wR_factor_gt 0.2704 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.88520(7) 0.27177(7) 0.44900(7) 0.0825(6) Uani 1 1 d . . . O1 O 0.6478(5) 0.1643(6) 0.3307(7) 0.092(4) Uani 1 1 d . . . N1 N 0.8355(7) 0.1931(7) 0.3808(7) 0.079(4) Uani 1 1 d . . . C1 C 0.8564(9) 0.1463(10) 0.3709(10) 0.080(5) Uani 1 1 d . . . O2 O 0.8455(8) 0.4658(8) 0.5462(9) 0.127(5) Uani 1 1 d . . . N2 N 0.7614(6) 0.2349(6) 0.3501(7) 0.070(3) Uani 1 1 d . . . H2 H 0.7935 0.2768 0.3603 0.084 Uiso 1 1 calc R . . C2 C 0.8240(11) 0.0921(10) 0.3292(10) 0.095(6) Uani 1 1 d . . . H2A H 0.8398 0.0604 0.3251 0.114 Uiso 1 1 calc R . . O3 O 0.9569(6) 0.3234(7) 0.3738(7) 0.095(4) Uani 1 1 d . . . N3 N 0.9397(8) 0.3499(8) 0.5150(8) 0.090(4) Uani 1 1 d . . . C3 C 0.7674(10) 0.0822(9) 0.2919(10) 0.092(5) Uani 1 1 d . . . H3 H 0.7440 0.0434 0.2627 0.110 Uiso 1 1 calc R . . O4 O 0.8910(7) 0.3654(6) 0.3431(7) 0.098(4) Uani 1 1 d . . . N4 N 0.8472(8) 0.3670(7) 0.5285(7) 0.085(4) Uani 1 1 d . . . H4 H 0.8218 0.3240 0.5164 0.102 Uiso 1 1 calc R . . C4 C 0.7451(8) 0.1285(7) 0.2970(9) 0.072(4) Uani 1 1 d . . . H4A H 0.7078 0.1238 0.2701 0.086 Uiso 1 1 calc R . . O5 O 0.8125(6) 0.2268(7) 0.5200(7) 0.095(4) Uani 1 1 d . . . C5 C 0.7797(8) 0.1829(8) 0.3435(9) 0.068(4) Uani 1 1 d . . . O6 O 0.8741(10) 0.1880(11) 0.5761(10) 0.156(7) Uani 1 1 d . . . C6 C 0.9192(11) 0.1610(12) 0.4127(12) 0.127(8) Uani 1 1 d . . . H6A H 0.9252 0.1210 0.4115 0.190 Uiso 1 1 calc R . . H6B H 0.9136 0.1711 0.4610 0.190 Uiso 1 1 calc R . . H6C H 0.9595 0.2003 0.3925 0.190 Uiso 1 1 calc R . . C7 C 0.6957(9) 0.2219(9) 0.3410(8) 0.068(4) Uani 1 1 d . . . C8 C 0.6833(7) 0.2819(8) 0.3439(8) 0.063(4) Uani 1 1 d . . . C9 C 0.6154(8) 0.2659(8) 0.3433(7) 0.065(4) Uani 1 1 d . . . H9 H 0.5802 0.2195 0.3425 0.078 Uiso 1 1 calc R . . C10 C 1.0083(10) 0.3679(11) 0.5290(10) 0.093(6) Uani 1 1 d . . . C11 C 1.0485(11) 0.4253(11) 0.5638(11) 0.105(7) Uani 1 1 d . . . H11 H 1.0941 0.4364 0.5733 0.126 Uiso 1 1 calc R . . C12 C 1.0273(11) 0.4684(10) 0.5862(11) 0.105(7) Uani 1 1 d . . . H12 H 1.0578 0.5096 0.6093 0.126 Uiso 1 1 calc R . . C13 C 0.9606(11) 0.4512(10) 0.5746(11) 0.104(6) Uani 1 1 d . . . H13 H 0.9443 0.4801 0.5909 0.125 Uiso 1 1 calc R . . C14 C 0.9176(9) 0.3924(9) 0.5395(10) 0.085(5) Uani 1 1 d . . . C15 C 1.0279(9) 0.3169(10) 0.5074(11) 0.103(6) Uani 1 1 d . . . H15A H 1.0766 0.3353 0.5161 0.155 Uiso 1 1 calc R . . H15B H 1.0185 0.3071 0.4577 0.155 Uiso 1 1 calc R . . H15C H 1.0014 0.2749 0.5342 0.155 Uiso 1 1 calc R . . C16 C 0.8166(11) 0.4040(13) 0.5353(11) 0.104(6) Uani 1 1 d . . . C17 C 0.7387(9) 0.3652(10) 0.5304(9) 0.081(5) Uani 1 1 d . . . C18 C 0.7002(10) 0.2953(9) 0.5306(8) 0.080(5) Uani 1 1 d . . . H18 H 0.7222 0.2690 0.5309 0.096 Uiso 1 1 calc R . . C19 C 0.9449(9) 0.3621(10) 0.3400(10) 0.085(5) Uani 1 1 d . . . C20 C 0.9959(10) 0.4081(11) 0.2845(11) 0.117(7) Uani 1 1 d . . . H20A H 1.0424 0.4228 0.3002 0.176 Uiso 1 1 calc R . . H20B H 0.9908 0.4481 0.2771 0.176 Uiso 1 1 calc R . . H20C H 0.9871 0.3827 0.2408 0.176 Uiso 1 1 calc R . . C21 C 0.8249(13) 0.1967(12) 0.5725(12) 0.111(7) Uani 1 1 d . . . C22 C 0.7651(13) 0.1683(13) 0.6276(13) 0.145(9) Uani 1 1 d . . . H22A H 0.7267 0.1256 0.6105 0.218 Uiso 1 1 calc R . . H22B H 0.7504 0.2019 0.6348 0.218 Uiso 1 1 calc R . . H22C H 0.7813 0.1599 0.6718 0.218 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 0.0723(10) 0.0921(11) 0.0845(10) -0.0067(8) -0.0181(7) 0.0421(8) O1 0.047(6) 0.053(7) 0.168(12) 0.014(7) 0.004(7) 0.017(6) N1 0.072(9) 0.089(10) 0.076(9) 0.001(7) -0.019(7) 0.040(8) C1 0.068(11) 0.086(12) 0.103(14) -0.003(11) -0.012(10) 0.053(10) O2 0.102(11) 0.094(11) 0.188(16) 0.001(11) -0.010(10) 0.051(9) N2 0.059(8) 0.044(7) 0.103(10) -0.009(7) -0.015(7) 0.023(6) C2 0.108(16) 0.090(14) 0.109(15) -0.007(12) -0.005(13) 0.066(13) O3 0.076(8) 0.109(10) 0.099(9) -0.008(8) -0.023(7) 0.046(8) N3 0.093(11) 0.107(12) 0.088(10) -0.001(9) -0.023(8) 0.063(10) C3 0.082(13) 0.070(12) 0.123(16) 0.003(11) -0.010(11) 0.038(11) O4 0.087(9) 0.070(8) 0.126(11) -0.003(7) -0.023(8) 0.031(7) N4 0.088(11) 0.073(10) 0.101(11) -0.025(8) -0.017(8) 0.046(9) C4 0.053(9) 0.045(9) 0.111(13) 0.000(9) -0.004(9) 0.020(7) O5 0.100(9) 0.095(9) 0.079(8) -0.009(7) -0.019(7) 0.040(8) C5 0.054(9) 0.054(9) 0.090(12) 0.010(8) 0.004(8) 0.022(8) O6 0.126(14) 0.20(2) 0.165(16) 0.044(14) 0.001(12) 0.104(14) C6 0.127(18) 0.15(2) 0.15(2) -0.051(17) -0.050(16) 0.111(17) C7 0.069(11) 0.066(11) 0.079(11) -0.001(8) -0.007(8) 0.040(10) C8 0.046(9) 0.065(10) 0.069(10) 0.003(8) -0.003(7) 0.021(8) C9 0.071(11) 0.065(10) 0.069(10) 0.009(8) 0.007(8) 0.042(9) C10 0.083(13) 0.104(15) 0.091(13) 0.013(11) -0.031(11) 0.046(12) C11 0.098(15) 0.104(16) 0.118(17) -0.023(13) -0.055(13) 0.054(14) C12 0.096(15) 0.082(13) 0.138(18) -0.006(12) -0.056(13) 0.046(12) C13 0.108(16) 0.083(14) 0.122(16) -0.005(12) -0.036(13) 0.049(13) C14 0.062(11) 0.070(12) 0.097(13) 0.014(10) -0.020(10) 0.015(10) C15 0.068(12) 0.106(15) 0.136(17) -0.014(13) -0.043(11) 0.043(11) C16 0.097(16) 0.093(16) 0.113(17) -0.008(13) -0.012(12) 0.042(14) C17 0.069(11) 0.097(15) 0.071(11) 0.008(10) -0.004(9) 0.038(12) C18 0.098(14) 0.077(13) 0.065(11) 0.010(9) 0.000(9) 0.043(11) C19 0.059(11) 0.096(15) 0.089(14) -0.022(11) -0.027(10) 0.031(11) C20 0.087(14) 0.112(17) 0.124(17) 0.029(14) 0.007(13) 0.029(13) C21 0.108(18) 0.109(17) 0.089(16) -0.011(13) -0.002(14) 0.033(15) C22 0.14(2) 0.15(2) 0.13(2) 0.049(17) 0.037(17) 0.064(18) _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 O5 1.983(13) . ? Pd1 N3 2.019(16) . ? Pd1 N1 2.037(14) . ? Pd1 O3 2.048(13) . ? O1 C7 1.226(18) . ? N1 C5 1.369(19) . ? N1 C1 1.37(2) . ? C1 C2 1.34(2) . ? C1 C6 1.52(2) . ? O2 C16 1.23(2) . ? N2 C7 1.374(19) . ? N2 C5 1.436(18) . ? C2 C3 1.39(2) . ? O3 C19 1.22(2) . ? N3 C14 1.37(2) . ? N3 C10 1.42(2) . ? C3 C4 1.38(2) . ? O4 C19 1.26(2) . ? N4 C16 1.33(2) . ? N4 C14 1.41(2) . ? C4 C5 1.40(2) . ? O5 C21 1.32(3) . ? O6 C21 1.23(3) . ? C7 C8 1.52(2) . ? C8 C9 1.380(19) 2_655 ? C8 C9 1.391(19) . ? C9 C8 1.380(19) 3_665 ? C10 C11 1.33(3) . ? C10 C15 1.49(3) . ? C11 C12 1.36(3) . ? C12 C13 1.38(3) . ? C13 C14 1.37(2) . ? C16 C17 1.53(3) . ? C17 C18 1.37(2) . ? C17 C18 1.45(2) 2_655 ? C18 C17 1.45(2) 3_665 ? C19 C20 1.53(3) . ? C21 C22 1.58(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Pd1 N3 90.2(6) . . ? O5 Pd1 N1 92.3(5) . . ? N3 Pd1 N1 176.6(6) . . ? O5 Pd1 O3 175.1(6) . . ? N3 Pd1 O3 88.9(6) . . ? N1 Pd1 O3 88.8(5) . . ? C5 N1 C1 116.3(14) . . ? C5 N1 Pd1 122.9(11) . . ? C1 N1 Pd1 120.8(11) . . ? C2 C1 N1 123.4(16) . . ? C2 C1 C6 122.7(17) . . ? N1 C1 C6 113.9(16) . . ? C7 N2 C5 122.5(12) . . ? C1 C2 C3 119.7(17) . . ? C19 O3 Pd1 112.7(13) . . ? C14 N3 C10 117.6(16) . . ? C14 N3 Pd1 123.6(11) . . ? C10 N3 Pd1 118.2(14) . . ? C4 C3 C2 120.2(18) . . ? C16 N4 C14 124.4(17) . . ? C3 C4 C5 117.3(16) . . ? C21 O5 Pd1 116.9(14) . . ? N1 C5 C4 123.0(14) . . ? N1 C5 N2 115.9(14) . . ? C4 C5 N2 120.9(14) . . ? O1 C7 N2 122.4(14) . . ? O1 C7 C8 119.8(14) . . ? N2 C7 C8 117.9(14) . . ? C9 C8 C9 119.2(16) 2_655 . ? C9 C8 C7 124.5(14) 2_655 . ? C9 C8 C7 116.2(14) . . ? C8 C9 C8 120.8(17) 3_665 . ? C11 C10 N3 119(2) . . ? C11 C10 C15 124.9(18) . . ? N3 C10 C15 115.6(17) . . ? C10 C11 C12 123(2) . . ? C11 C12 C13 119(2) . . ? C14 C13 C12 120(2) . . ? N3 C14 C13 121.3(18) . . ? N3 C14 N4 113.4(16) . . ? C13 C14 N4 125(2) . . ? O2 C16 N4 126(2) . . ? O2 C16 C17 118(2) . . ? N4 C16 C17 116(2) . . ? C18 C17 C18 119.2(19) . 2_655 ? C18 C17 C16 123.2(19) . . ? C18 C17 C16 117.5(19) 2_655 . ? C17 C18 C17 120.8(19) . 3_665 ? O3 C19 O4 125.8(19) . . ? O3 C19 C20 119.6(19) . . ? O4 C19 C20 115(2) . . ? O6 C21 O5 125(2) . . ? O6 C21 C22 124(2) . . ? O5 C21 C22 111(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.192 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.147