# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name J.Vicente _publ_contact_author_email jvs1@um.es _publ_author_name J.Vicente data_aab16s _database_code_depnum_ccdc_archive 'CCDC 837023' #TrackingRef '- 2d_aab16s.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H15 Cl N2 O Pd' _chemical_formula_weight 369.13 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' Cl Cl 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1285(4) _cell_length_b 9.2016(4) _cell_length_c 10.0426(4) _cell_angle_alpha 90.108(2) _cell_angle_beta 108.795(2) _cell_angle_gamma 114.271(2) _cell_volume 719.11(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7402 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 28.03 _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 1.468 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7001 _exptl_absorpt_correction_T_max 0.7577 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8249 _diffrn_reflns_av_R_equivalents 0.0133 _diffrn_reflns_av_sigmaI/netI 0.0154 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 28.03 _reflns_number_total 3197 _reflns_number_gt 3155 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. OH free, rigid methyls, other riding ; _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^)+(0.0236P)^2^+0.4874P] 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 0.0164(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3197 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0175 _refine_ls_R_factor_gt 0.0172 _refine_ls_wR_factor_ref 0.0448 _refine_ls_wR_factor_gt 0.0446 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 0.766055(14) 0.276499(13) 1.103599(11) 0.01216(6) Uani 1 1 d . . . Cl1 Cl 1.04575(5) 0.30474(5) 1.26100(4) 0.01932(9) Uani 1 1 d . . . N1 N 0.73034(17) 0.36338(16) 1.26660(14) 0.0147(3) Uani 1 1 d . . . O1 O 0.84981(16) 0.41000(16) 1.40436(12) 0.0204(2) Uani 1 1 d . . . H01 H 0.926(4) 0.395(3) 1.390(3) 0.043(7) Uiso 1 1 d . . . C1 C 0.5333(2) 0.26411(18) 1.00536(17) 0.0149(3) Uani 1 1 d . . . C2 C 0.4788(2) 0.33169(18) 1.09621(16) 0.0137(3) Uani 1 1 d . . . C3 C 0.3235(2) 0.34240(19) 1.04538(17) 0.0163(3) Uani 1 1 d . . . H3 H 0.2898 0.3900 1.1071 0.020 Uiso 1 1 calc R . . C4 C 0.2173(2) 0.2831(2) 0.90355(18) 0.0190(3) Uani 1 1 d . . . H4 H 0.1125 0.2929 0.8673 0.023 Uiso 1 1 calc R . . C5 C 0.2654(2) 0.2096(2) 0.81563(17) 0.0199(3) Uani 1 1 d . . . H5 H 0.1906 0.1653 0.7199 0.024 Uiso 1 1 calc R . . C6 C 0.4224(2) 0.1997(2) 0.86575(17) 0.0181(3) Uani 1 1 d . . . H6 H 0.4532 0.1488 0.8041 0.022 Uiso 1 1 calc R . . C7 C 0.5947(2) 0.38598(18) 1.24523(16) 0.0147(3) Uani 1 1 d . . . C8 C 0.5603(2) 0.4562(2) 1.35966(18) 0.0204(3) Uani 1 1 d . . . H8A H 0.4762 0.3696 1.3895 0.031 Uiso 1 1 calc R . . H8B H 0.5146 0.5335 1.3232 0.031 Uiso 1 1 calc R . . H8C H 0.6674 0.5115 1.4413 0.031 Uiso 1 1 calc R . . N2 N 0.78231(17) 0.19740(16) 0.92177(14) 0.0138(3) Uani 1 1 d . . . C11 C 0.7797(2) 0.2823(2) 0.81228(18) 0.0180(3) Uani 1 1 d . . . H11 H 0.7789 0.3845 0.8239 0.022 Uiso 1 1 calc R . . C12 C 0.7780(2) 0.2259(2) 0.68402(18) 0.0208(3) Uani 1 1 d . . . H12 H 0.7751 0.2886 0.6090 0.025 Uiso 1 1 calc R . . C13 C 0.7806(2) 0.0770(2) 0.66454(17) 0.0201(3) Uani 1 1 d . . . C14 C 0.7894(2) -0.0064(2) 0.77984(19) 0.0200(3) Uani 1 1 d . . . H14 H 0.7951 -0.1067 0.7723 0.024 Uiso 1 1 calc R . . C15 C 0.7899(2) 0.05584(19) 0.90521(17) 0.0162(3) Uani 1 1 d . . . H15 H 0.7958 -0.0034 0.9826 0.019 Uiso 1 1 calc R . . C16 C 0.7754(3) 0.0094(3) 0.5254(2) 0.0338(4) Uani 1 1 d . . . H16A H 0.8218 -0.0705 0.5418 0.051 Uiso 1 1 calc R . . H16B H 0.8446 0.0970 0.4850 0.051 Uiso 1 1 calc R . . H16C H 0.6563 -0.0421 0.4588 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01378(8) 0.01418(8) 0.01095(8) 0.00129(4) 0.00610(5) 0.00707(5) Cl1 0.01784(18) 0.0260(2) 0.01799(18) 0.00215(15) 0.00628(14) 0.01316(16) N1 0.0164(6) 0.0175(6) 0.0097(6) 0.0001(5) 0.0044(5) 0.0072(5) O1 0.0184(6) 0.0318(7) 0.0106(5) -0.0022(5) 0.0025(4) 0.0126(5) C1 0.0158(7) 0.0145(7) 0.0173(7) 0.0042(6) 0.0090(6) 0.0068(6) C2 0.0155(7) 0.0130(7) 0.0132(7) 0.0021(5) 0.0067(6) 0.0054(6) C3 0.0164(7) 0.0154(7) 0.0195(8) 0.0038(6) 0.0093(6) 0.0070(6) C4 0.0146(7) 0.0197(8) 0.0225(8) 0.0054(6) 0.0062(6) 0.0076(6) C5 0.0158(7) 0.0243(8) 0.0138(7) 0.0013(6) 0.0026(6) 0.0054(6) C6 0.0188(8) 0.0210(8) 0.0162(8) 0.0009(6) 0.0089(6) 0.0081(6) C7 0.0167(7) 0.0148(7) 0.0142(7) 0.0022(6) 0.0078(6) 0.0065(6) C8 0.0221(8) 0.0264(8) 0.0163(8) -0.0014(6) 0.0096(6) 0.0119(7) N2 0.0148(6) 0.0155(6) 0.0136(6) 0.0019(5) 0.0073(5) 0.0073(5) C11 0.0220(8) 0.0211(8) 0.0181(8) 0.0065(6) 0.0106(6) 0.0135(7) C12 0.0239(8) 0.0295(9) 0.0149(8) 0.0071(6) 0.0082(6) 0.0161(7) C13 0.0180(8) 0.0261(8) 0.0148(8) -0.0025(6) 0.0071(6) 0.0073(7) C14 0.0223(8) 0.0153(7) 0.0237(8) -0.0006(6) 0.0117(7) 0.0069(6) C15 0.0181(7) 0.0150(7) 0.0173(7) 0.0033(6) 0.0091(6) 0.0066(6) C16 0.0425(12) 0.0403(11) 0.0202(9) -0.0037(8) 0.0156(8) 0.0162(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 C1 1.9873(16) . ? Pd1 N1 1.9945(13) . ? Pd1 N2 2.0358(13) . ? Pd1 Cl1 2.4367(4) . ? N1 C7 1.290(2) . ? N1 O1 1.3887(17) . ? C1 C6 1.390(2) . ? C1 C2 1.419(2) . ? C2 C3 1.389(2) . ? C2 C7 1.467(2) . ? C3 C4 1.392(2) . ? C4 C5 1.386(2) . ? C5 C6 1.399(2) . ? C7 C8 1.495(2) . ? N2 C15 1.345(2) . ? N2 C11 1.350(2) . ? C11 C12 1.381(2) . ? C12 C13 1.395(2) . ? C13 C14 1.390(2) . ? C13 C16 1.507(2) . ? C14 C15 1.380(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N1 80.00(6) . . ? C1 Pd1 N2 93.74(6) . . ? N1 Pd1 N2 173.05(5) . . ? C1 Pd1 Cl1 170.23(5) . . ? N1 Pd1 Cl1 90.29(4) . . ? N2 Pd1 Cl1 96.01(4) . . ? C7 N1 O1 116.75(13) . . ? C7 N1 Pd1 119.93(11) . . ? O1 N1 Pd1 123.23(10) . . ? C6 C1 C2 118.15(14) . . ? C6 C1 Pd1 129.45(12) . . ? C2 C1 Pd1 112.40(11) . . ? C3 C2 C1 121.16(14) . . ? C3 C2 C7 122.98(14) . . ? C1 C2 C7 115.85(14) . . ? C2 C3 C4 119.70(15) . . ? C5 C4 C3 119.62(15) . . ? C4 C5 C6 120.96(15) . . ? C1 C6 C5 120.28(15) . . ? N1 C7 C2 111.53(13) . . ? N1 C7 C8 123.69(14) . . ? C2 C7 C8 124.77(14) . . ? C15 N2 C11 117.95(14) . . ? C15 N2 Pd1 120.89(11) . . ? C11 N2 Pd1 121.12(11) . . ? N2 C11 C12 122.31(15) . . ? C11 C12 C13 120.06(16) . . ? C14 C13 C12 116.97(15) . . ? C14 C13 C16 121.24(17) . . ? C12 C13 C16 121.79(17) . . ? C15 C14 C13 120.30(15) . . ? N2 C15 C14 122.35(15) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H01 Cl1 0.82(3) 2.29(3) 3.0476(13) 156(3) . C12 H12 O1 0.95 2.49 3.388(2) 156.7 1_554 _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.398 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.070 # Attachment '- 7bH2O_aab341s.cif' data_aab341s _database_code_depnum_ccdc_archive 'CCDC 837024' #TrackingRef '- 7bH2O_aab341s.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H34 N4 O3 Pd2' _chemical_formula_weight 663.37 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 monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.9117(12) _cell_length_b 11.4690(5) _cell_length_c 18.9722(8) _cell_angle_alpha 90.00 _cell_angle_beta 116.729(2) _cell_angle_gamma 90.00 _cell_volume 5424.4(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6991 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 28.16 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 1.359 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7527 _exptl_absorpt_correction_T_max 0.8539 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30421 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0139 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 28.16 _reflns_number_total 6181 _reflns_number_gt 5961 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Water hydrogens free with dfix, rigid methyls others riding ; _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^)+(0.0291P)^2^+6.9418P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6181 _refine_ls_number_parameters 332 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0208 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0513 _refine_ls_wR_factor_gt 0.0507 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.006 _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 0.851632(5) 0.790971(11) 0.363375(7) 0.01684(4) Uani 1 1 d . . . Pd2 Pd 0.928732(5) 0.762185(11) 0.252405(7) 0.01482(4) Uani 1 1 d . . . N1 N 0.87942(6) 0.64328(12) 0.33552(8) 0.0183(3) Uani 1 1 d . . . N2 N 0.92210(5) 0.90504(12) 0.31089(8) 0.0174(3) Uani 1 1 d . . . O1 O 0.92750(5) 0.63617(11) 0.33472(7) 0.0201(2) Uani 1 1 d . . . O2 O 0.91652(5) 0.90092(11) 0.37824(7) 0.0213(2) Uani 1 1 d . . . C1 C 0.79225(7) 0.68267(16) 0.34935(10) 0.0203(3) Uani 1 1 d . . . C2 C 0.79997(7) 0.56871(15) 0.32708(9) 0.0202(3) Uani 1 1 d . . . C3 C 0.76118(7) 0.48263(16) 0.31133(10) 0.0241(4) Uani 1 1 d . . . H3 H 0.7664 0.4070 0.2955 0.029 Uiso 1 1 calc R . . C4 C 0.71492(8) 0.50745(18) 0.31882(11) 0.0295(4) Uani 1 1 d . . . H4 H 0.6883 0.4491 0.3077 0.035 Uiso 1 1 calc R . . C5 C 0.70779(8) 0.61726(19) 0.34246(12) 0.0313(4) Uani 1 1 d . . . H5 H 0.6765 0.6336 0.3486 0.038 Uiso 1 1 calc R . . C6 C 0.74598(7) 0.70437(17) 0.35737(11) 0.0262(4) Uani 1 1 d . . . H6 H 0.7403 0.7796 0.3732 0.031 Uiso 1 1 calc R . . C7 C 0.84985(7) 0.54995(15) 0.32069(9) 0.0192(3) Uani 1 1 d . . . C8 C 0.86658(8) 0.43717(15) 0.29934(11) 0.0241(4) Uani 1 1 d . . . H8A H 0.8854 0.4524 0.2674 0.036 Uiso 1 1 calc R . . H8B H 0.8348 0.3893 0.2691 0.036 Uiso 1 1 calc R . . H8C H 0.8906 0.3957 0.3476 0.036 Uiso 1 1 calc R . . C9 C 0.81963(7) 0.92488(16) 0.38967(10) 0.0220(3) Uani 1 1 d . . . N3 N 0.80147(6) 1.00488(13) 0.40461(9) 0.0231(3) Uani 1 1 d . . . C10 C 0.78159(7) 1.10703(15) 0.42944(10) 0.0231(4) Uani 1 1 d . . . C11 C 0.78824(8) 1.07982(19) 0.51199(11) 0.0301(4) Uani 1 1 d . . . H11A H 0.7676 1.0098 0.5101 0.045 Uiso 1 1 calc R . . H11B H 0.7752 1.1457 0.5313 0.045 Uiso 1 1 calc R . . H11C H 0.8262 1.0664 0.5476 0.045 Uiso 1 1 calc R . . C12 C 0.72277(8) 1.1243(2) 0.37098(12) 0.0366(5) Uani 1 1 d . . . H12A H 0.7200 1.1428 0.3188 0.055 Uiso 1 1 calc R . . H12B H 0.7078 1.1886 0.3888 0.055 Uiso 1 1 calc R . . H12C H 0.7028 1.0526 0.3677 0.055 Uiso 1 1 calc R . . C13 C 0.81582(9) 1.21022(18) 0.42916(15) 0.0370(5) Uani 1 1 d . . . H13A H 0.8532 1.1965 0.4675 0.056 Uiso 1 1 calc R . . H13B H 0.8027 1.2813 0.4434 0.056 Uiso 1 1 calc R . . H13C H 0.8135 1.2192 0.3764 0.056 Uiso 1 1 calc R . . C21 C 0.93274(6) 0.88594(14) 0.18198(9) 0.0170(3) Uani 1 1 d . . . C22 C 0.92992(6) 0.99968(14) 0.20927(10) 0.0186(3) Uani 1 1 d . . . C23 C 0.93225(7) 1.09676(15) 0.16648(11) 0.0237(4) Uani 1 1 d . . . H23 H 0.9306 1.1729 0.1850 0.028 Uiso 1 1 calc R . . C24 C 0.93693(7) 1.08294(16) 0.09718(11) 0.0257(4) Uani 1 1 d . . . H24 H 0.9374 1.1494 0.0676 0.031 Uiso 1 1 calc R . . C25 C 0.94092(7) 0.97213(16) 0.07111(11) 0.0238(4) Uani 1 1 d . . . H25 H 0.9447 0.9628 0.0241 0.029 Uiso 1 1 calc R . . C26 C 0.93942(7) 0.87409(15) 0.11394(10) 0.0199(3) Uani 1 1 d . . . H26 H 0.9430 0.7985 0.0964 0.024 Uiso 1 1 calc R . . C27 C 0.92453(6) 1.00655(14) 0.28250(10) 0.0190(3) Uani 1 1 d . . . C28 C 0.92095(8) 1.11643(15) 0.32229(11) 0.0250(4) Uani 1 1 d . . . H28A H 0.8870 1.1176 0.3260 0.038 Uiso 1 1 calc R . . H28B H 0.9225 1.1838 0.2916 0.038 Uiso 1 1 calc R . . H28C H 0.9510 1.1200 0.3754 0.038 Uiso 1 1 calc R . . C29 C 0.93009(7) 0.63655(15) 0.18407(10) 0.0193(3) Uani 1 1 d . . . N4 N 0.92829(6) 0.56268(13) 0.14205(9) 0.0219(3) Uani 1 1 d . . . C30 C 0.92828(8) 0.47054(15) 0.08856(10) 0.0238(4) Uani 1 1 d . . . C31 C 0.87935(8) 0.39322(18) 0.06973(14) 0.0372(5) Uani 1 1 d . . . H31A H 0.8813 0.3612 0.1188 0.056 Uiso 1 1 calc R . . H31B H 0.8788 0.3293 0.0351 0.056 Uiso 1 1 calc R . . H31C H 0.8466 0.4397 0.0432 0.056 Uiso 1 1 calc R . . C32 C 0.98108(8) 0.40442(17) 0.13147(12) 0.0285(4) Uani 1 1 d . . . H32A H 1.0111 0.4593 0.1480 0.043 Uiso 1 1 calc R . . H32B H 0.9841 0.3461 0.0959 0.043 Uiso 1 1 calc R . . H32C H 0.9819 0.3654 0.1780 0.043 Uiso 1 1 calc R . . C33 C 0.92389(11) 0.5290(2) 0.01429(12) 0.0429(6) Uani 1 1 d . . . H33A H 0.8901 0.5725 -0.0107 0.064 Uiso 1 1 calc R . . H33B H 0.9246 0.4696 -0.0224 0.064 Uiso 1 1 calc R . . H33C H 0.9541 0.5827 0.0279 0.064 Uiso 1 1 calc R . . O3 O 0.99199(7) 0.74887(14) 0.48448(9) 0.0365(3) Uani 1 1 d D . . H03A H 0.9771(12) 0.8158(18) 0.4656(18) 0.070(10) Uiso 1 1 d D . . H03B H 0.9771(13) 0.702(2) 0.4436(14) 0.073(11) Uiso 1 1 d 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 0.01914(7) 0.01640(7) 0.01640(7) -0.00014(4) 0.00924(5) 0.00263(4) Pd2 0.01632(7) 0.01302(7) 0.01519(7) -0.00174(4) 0.00715(5) 0.00076(4) N1 0.0206(7) 0.0181(7) 0.0169(6) 0.0015(5) 0.0093(6) 0.0030(5) N2 0.0176(6) 0.0172(7) 0.0179(7) -0.0037(5) 0.0085(6) 0.0002(5) O1 0.0207(6) 0.0190(6) 0.0234(6) 0.0024(5) 0.0123(5) 0.0042(5) O2 0.0253(6) 0.0219(6) 0.0190(6) -0.0056(5) 0.0121(5) -0.0028(5) C1 0.0200(8) 0.0239(8) 0.0158(7) 0.0040(6) 0.0069(6) 0.0017(6) C2 0.0212(8) 0.0231(8) 0.0147(7) 0.0032(6) 0.0065(6) 0.0010(6) C3 0.0249(9) 0.0241(9) 0.0195(8) 0.0028(7) 0.0067(7) -0.0015(7) C4 0.0234(9) 0.0338(10) 0.0280(9) 0.0051(8) 0.0088(8) -0.0048(7) C5 0.0219(9) 0.0420(12) 0.0314(10) 0.0069(8) 0.0133(8) 0.0017(8) C6 0.0238(9) 0.0301(10) 0.0253(9) 0.0040(7) 0.0116(8) 0.0046(7) C7 0.0215(8) 0.0192(8) 0.0143(7) 0.0019(6) 0.0057(6) 0.0018(6) C8 0.0295(9) 0.0174(8) 0.0252(9) -0.0020(7) 0.0123(8) -0.0004(7) C9 0.0231(8) 0.0245(9) 0.0189(8) -0.0001(7) 0.0099(7) 0.0006(7) N3 0.0261(8) 0.0231(8) 0.0222(7) -0.0030(6) 0.0129(6) 0.0033(6) C10 0.0252(9) 0.0223(8) 0.0215(8) -0.0047(7) 0.0101(7) 0.0064(7) C11 0.0338(10) 0.0357(11) 0.0231(9) -0.0035(8) 0.0147(8) 0.0069(8) C12 0.0273(10) 0.0449(12) 0.0286(10) -0.0126(9) 0.0045(8) 0.0113(9) C13 0.0383(12) 0.0238(10) 0.0473(13) 0.0042(9) 0.0178(10) 0.0055(8) C21 0.0135(7) 0.0168(8) 0.0186(7) 0.0000(6) 0.0054(6) 0.0002(6) C22 0.0157(7) 0.0173(8) 0.0218(8) -0.0008(6) 0.0076(6) -0.0007(6) C23 0.0238(8) 0.0158(8) 0.0329(9) 0.0004(7) 0.0140(8) 0.0001(6) C24 0.0252(9) 0.0227(9) 0.0321(10) 0.0078(7) 0.0155(8) 0.0010(7) C25 0.0212(8) 0.0285(9) 0.0236(8) 0.0031(7) 0.0118(7) 0.0004(7) C26 0.0178(8) 0.0197(8) 0.0210(8) -0.0010(6) 0.0077(7) 0.0002(6) C27 0.0162(7) 0.0165(8) 0.0233(8) -0.0030(6) 0.0080(6) -0.0004(6) C28 0.0295(9) 0.0171(8) 0.0301(9) -0.0056(7) 0.0148(8) -0.0005(7) C29 0.0212(8) 0.0179(8) 0.0183(8) 0.0014(6) 0.0086(7) 0.0001(6) N4 0.0285(8) 0.0166(7) 0.0206(7) -0.0018(6) 0.0111(6) 0.0011(6) C30 0.0333(10) 0.0160(8) 0.0211(8) -0.0065(6) 0.0113(7) 0.0018(7) C31 0.0285(10) 0.0272(10) 0.0466(12) -0.0132(9) 0.0085(9) -0.0014(8) C32 0.0286(9) 0.0237(9) 0.0313(10) -0.0074(7) 0.0119(8) 0.0020(7) C33 0.0763(17) 0.0303(11) 0.0263(10) -0.0016(8) 0.0267(11) 0.0048(11) O3 0.0406(9) 0.0358(9) 0.0291(8) 0.0042(6) 0.0122(7) -0.0004(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C9 1.9510(18) . ? Pd1 C1 1.9909(18) . ? Pd1 N1 2.0296(14) . ? Pd1 O2 2.1191(12) . ? Pd2 C29 1.9501(17) . ? Pd2 C21 1.9867(16) . ? Pd2 N2 2.0334(13) . ? Pd2 O1 2.1395(12) . ? N1 C7 1.303(2) . ? N1 O1 1.3512(18) . ? N2 C27 1.297(2) . ? N2 O2 1.3558(17) . ? C1 C6 1.389(2) . ? C1 C2 1.420(2) . ? C2 C3 1.395(2) . ? C2 C7 1.467(2) . ? C3 C4 1.391(3) . ? C4 C5 1.381(3) . ? C5 C6 1.394(3) . ? C7 C8 1.492(2) . ? C9 N3 1.144(2) . ? N3 C10 1.462(2) . ? C10 C13 1.523(3) . ? C10 C12 1.526(3) . ? C10 C11 1.524(2) . ? C21 C26 1.392(2) . ? C21 C22 1.419(2) . ? C22 C23 1.397(2) . ? C22 C27 1.465(2) . ? C23 C24 1.388(3) . ? C24 C25 1.386(3) . ? C25 C26 1.399(2) . ? C27 C28 1.495(2) . ? C29 N4 1.149(2) . ? N4 C30 1.465(2) . ? C30 C33 1.515(3) . ? C30 C32 1.527(3) . ? C30 C31 1.530(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 C9 Pd1 C1 94.35(7) . . ? C9 Pd1 N1 174.98(7) . . ? C1 Pd1 N1 80.63(7) . . ? C9 Pd1 O2 87.69(6) . . ? C1 Pd1 O2 177.91(6) . . ? N1 Pd1 O2 97.32(5) . . ? C29 Pd2 C21 93.26(7) . . ? C29 Pd2 N2 172.72(6) . . ? C21 Pd2 N2 80.67(6) . . ? C29 Pd2 O1 89.87(6) . . ? C21 Pd2 O1 176.22(6) . . ? N2 Pd2 O1 96.35(5) . . ? C7 N1 O1 118.95(14) . . ? C7 N1 Pd1 117.56(11) . . ? O1 N1 Pd1 123.44(10) . . ? C27 N2 O2 118.18(13) . . ? C27 N2 Pd2 117.50(11) . . ? O2 N2 Pd2 124.30(10) . . ? N1 O1 Pd2 108.03(9) . . ? N2 O2 Pd1 110.41(9) . . ? C6 C1 C2 118.07(16) . . ? C6 C1 Pd1 129.25(14) . . ? C2 C1 Pd1 112.68(12) . . ? C3 C2 C1 120.56(16) . . ? C3 C2 C7 123.55(16) . . ? C1 C2 C7 115.88(15) . . ? C2 C3 C4 120.02(18) . . ? C5 C4 C3 119.72(18) . . ? C4 C5 C6 120.73(18) . . ? C1 C6 C5 120.87(18) . . ? N1 C7 C2 113.23(15) . . ? N1 C7 C8 121.72(15) . . ? C2 C7 C8 125.05(16) . . ? N3 C9 Pd1 178.58(16) . . ? C9 N3 C10 175.82(18) . . ? N3 C10 C13 106.97(15) . . ? N3 C10 C12 108.07(15) . . ? C13 C10 C12 111.61(17) . . ? N3 C10 C11 106.18(15) . . ? C13 C10 C11 112.10(17) . . ? C12 C10 C11 111.57(16) . . ? C26 C21 C22 118.75(15) . . ? C26 C21 Pd2 128.74(13) . . ? C22 C21 Pd2 112.48(12) . . ? C23 C22 C21 119.75(15) . . ? C23 C22 C27 124.04(15) . . ? C21 C22 C27 116.21(14) . . ? C24 C23 C22 120.57(16) . . ? C23 C24 C25 119.98(17) . . ? C24 C25 C26 120.10(16) . . ? C21 C26 C25 120.78(16) . . ? N2 C27 C22 113.10(14) . . ? N2 C27 C28 121.24(15) . . ? C22 C27 C28 125.65(15) . . ? N4 C29 Pd2 176.75(16) . . ? C29 N4 C30 177.35(18) . . ? N4 C30 C33 107.46(15) . . ? N4 C30 C32 106.83(14) . . ? C33 C30 C32 111.76(17) . . ? N4 C30 C31 107.56(15) . . ? C33 C30 C31 110.43(18) . . ? C32 C30 C31 112.52(16) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H03B O1 0.877(15) 2.047(18) 2.895(2) 163(3) . O3 H03A O2 0.869(15) 2.01(2) 2.779(2) 147(3) . O3 H03B N1 0.877(15) 2.66(3) 3.367(2) 139(3) . C32 H32A O1 0.98 2.58 3.538(2) 165.7 2_755 C33 H33C O3 0.98 2.50 3.439(3) 159.3 2_755 C32 H32B O3 0.98 2.47 3.424(2) 163.0 6_565 _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.729 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.072 # Attachment '- 8_aaj33c2si.cif' data_aaj33c2si _database_code_depnum_ccdc_archive 'CCDC 837025' #TrackingRef '- 8_aaj33c2si.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H32 Cl N3 O4 Pd' _chemical_formula_weight 628.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M 'P 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.1876(11) _cell_length_b 18.0675(14) _cell_length_c 12.4618(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.989(2) _cell_angle_gamma 90.00 _cell_volume 2854.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9585 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 28.52 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.782 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8188 _exptl_absorpt_correction_T_max 0.9330 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18582 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.66 _reflns_number_total 6757 _reflns_number_gt 6182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One methyl is disordered over two positions, ca 57:43%. OH free, ordered methyls rigid, others riding ; _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^)+(0.0422P)^2^+2.5977P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6757 _refine_ls_number_parameters 354 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0865 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.101 _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 0.231968(13) 0.574460(9) 0.360367(14) 0.01576(6) Uani 1 1 d . . . Cl1 Cl 0.26386(5) 0.67244(3) 0.23880(5) 0.02694(14) Uani 1 1 d . . . N1 N 0.15591(15) 0.65171(10) 0.43324(16) 0.0178(4) Uani 1 1 d . . . O1 O 0.10131(15) 0.70673(9) 0.36265(15) 0.0259(4) Uani 1 1 d . . . H01A H 0.131(3) 0.708(2) 0.308(3) 0.065(13) Uiso 1 1 d . . . N2 N 0.12435(15) 0.44767(11) 0.42610(17) 0.0193(4) Uani 1 1 d . . . N3 N 0.34557(16) 0.44989(11) 0.26959(17) 0.0216(4) Uani 1 1 d . . . C1 C 0.22254(17) 0.52446(12) 0.57581(19) 0.0173(4) Uani 1 1 d . . . C2 C 0.19777(17) 0.59446(12) 0.61034(19) 0.0169(4) Uani 1 1 d . . . C3 C 0.22868(17) 0.61448(13) 0.72241(19) 0.0189(4) Uani 1 1 d . . . H3 H 0.2078 0.6610 0.7449 0.023 Uiso 1 1 calc R . . C4 C 0.29000(19) 0.56683(13) 0.80154(19) 0.0194(5) Uani 1 1 d . . . C5 C 0.31907(18) 0.49789(13) 0.76833(19) 0.0196(5) Uani 1 1 d . A . C6 C 0.28406(17) 0.47678(13) 0.65656(19) 0.0185(4) Uani 1 1 d . . . C7 C 0.13848(17) 0.64989(12) 0.52923(19) 0.0170(4) Uani 1 1 d . . . C8 C 0.06569(19) 0.70335(13) 0.5620(2) 0.0216(5) Uani 1 1 d . . . H8A H 0.1023 0.7505 0.5840 0.032 Uiso 1 1 calc R . . H8B H 0.0434 0.6831 0.6248 0.032 Uiso 1 1 calc R . . H8C H 0.0036 0.7115 0.4985 0.032 Uiso 1 1 calc R . . C9 C 0.18516(17) 0.50208(12) 0.45717(19) 0.0169(4) Uani 1 1 d . . . C11 C 0.08677(19) 0.42664(12) 0.3120(2) 0.0199(5) Uani 1 1 d . . . C12 C 0.12320(19) 0.35945(13) 0.2794(2) 0.0228(5) Uani 1 1 d . . . C13 C 0.0848(2) 0.33717(14) 0.1689(2) 0.0278(5) Uani 1 1 d . . . H13 H 0.1094 0.2922 0.1454 0.033 Uiso 1 1 calc R . . C14 C 0.0113(2) 0.37924(15) 0.0923(2) 0.0302(6) Uani 1 1 d . . . H14 H -0.0136 0.3635 0.0169 0.036 Uiso 1 1 calc R . . C15 C -0.0257(2) 0.44409(15) 0.1263(2) 0.0277(5) Uani 1 1 d . . . H15 H -0.0766 0.4725 0.0737 0.033 Uiso 1 1 calc R . . C16 C 0.01036(18) 0.46890(13) 0.2366(2) 0.0225(5) Uani 1 1 d . . . C17 C -0.03493(19) 0.53896(14) 0.2705(2) 0.0262(5) Uani 1 1 d . . . H17A H -0.0347 0.5355 0.3490 0.039 Uiso 1 1 calc R . . H17B H -0.1075 0.5456 0.2239 0.039 Uiso 1 1 calc R . . H17C H 0.0080 0.5813 0.2605 0.039 Uiso 1 1 calc R . . C18 C 0.2023(2) 0.31223(14) 0.3627(2) 0.0280(5) Uani 1 1 d . . . H18A H 0.1665 0.2859 0.4106 0.042 Uiso 1 1 calc R . . H18B H 0.2577 0.3439 0.4087 0.042 Uiso 1 1 calc R . . H18C H 0.2339 0.2763 0.3225 0.042 Uiso 1 1 calc R . . C19 C 0.30282(18) 0.49623(13) 0.30235(19) 0.0202(5) Uani 1 1 d . . . C21 C 0.39359(18) 0.39106(13) 0.2290(2) 0.0217(5) Uani 1 1 d . . . C22 C 0.47696(19) 0.35476(14) 0.3052(2) 0.0280(5) Uani 1 1 d . . . C23 C 0.5224(2) 0.29625(16) 0.2628(3) 0.0379(7) Uani 1 1 d . . . H23 H 0.5786 0.2694 0.3111 0.045 Uiso 1 1 calc R . . C24 C 0.4873(2) 0.27641(16) 0.1519(3) 0.0418(8) Uani 1 1 d . . . H24 H 0.5195 0.2360 0.1251 0.050 Uiso 1 1 calc R . . C25 C 0.4060(2) 0.31443(16) 0.0792(3) 0.0372(7) Uani 1 1 d . . . H25 H 0.3836 0.3002 0.0029 0.045 Uiso 1 1 calc R . . C26 C 0.3562(2) 0.37344(14) 0.1160(2) 0.0266(5) Uani 1 1 d . . . C27 C 0.2682(2) 0.41634(17) 0.0399(2) 0.0354(6) Uani 1 1 d . . . H27A H 0.2934 0.4659 0.0280 0.053 Uiso 1 1 calc R . . H27B H 0.2096 0.4206 0.0737 0.053 Uiso 1 1 calc R . . H27C H 0.2441 0.3906 -0.0319 0.053 Uiso 1 1 calc R . . C28 C 0.5150(2) 0.37909(19) 0.4245(3) 0.0397(7) Uani 1 1 d . . . H28A H 0.5731 0.3471 0.4645 0.060 Uiso 1 1 calc R . . H28B H 0.4570 0.3757 0.4594 0.060 Uiso 1 1 calc R . . H28C H 0.5397 0.4304 0.4276 0.060 Uiso 1 1 calc R . . C29 C 0.2898(2) 0.65079(14) 0.9488(2) 0.0255(5) Uani 1 1 d . . . H29A H 0.3197 0.6923 0.9171 0.038 Uiso 1 1 calc R . . H29B H 0.3133 0.6535 1.0305 0.038 Uiso 1 1 calc R . . H29C H 0.2126 0.6533 0.9237 0.038 Uiso 1 1 calc R . . O2 O 0.32443(14) 0.58246(9) 0.91259(14) 0.0249(4) Uani 1 1 d . . . C30 C 0.4841(4) 0.4351(3) 0.8410(5) 0.0261(15) Uiso 0.573(17) 1 d PD A 1 H30A H 0.5186 0.4001 0.8999 0.031 Uiso 0.573(17) 1 calc PR A 1 H30B H 0.5239 0.4816 0.8514 0.031 Uiso 0.573(17) 1 calc PR A 1 H30C H 0.4819 0.4140 0.7680 0.031 Uiso 0.573(17) 1 calc PR A 1 C30' C 0.4826(5) 0.4572(5) 0.8775(8) 0.030(2) Uiso 0.427(17) 1 d PD A 2 H30D H 0.5142 0.4199 0.9338 0.036 Uiso 0.427(17) 1 calc PR A 2 H30E H 0.5015 0.5067 0.9085 0.036 Uiso 0.427(17) 1 calc PR A 2 H30F H 0.5089 0.4504 0.8119 0.036 Uiso 0.427(17) 1 calc PR A 2 O3 O 0.37523(14) 0.44954(10) 0.84697(15) 0.0276(4) Uani 1 1 d D . . C31 C 0.2553(2) 0.34872(13) 0.6585(2) 0.0289(6) Uani 1 1 d . . . H31A H 0.2672 0.3502 0.7397 0.043 Uiso 1 1 calc R . . H31B H 0.2806 0.3014 0.6372 0.043 Uiso 1 1 calc R . . H31C H 0.1797 0.3538 0.6217 0.043 Uiso 1 1 calc R . . O4 O 0.31169(13) 0.40859(9) 0.62467(14) 0.0211(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01548(10) 0.01531(10) 0.01737(10) 0.00019(6) 0.00600(7) -0.00141(6) Cl1 0.0345(3) 0.0227(3) 0.0276(3) 0.0047(2) 0.0153(3) -0.0038(2) N1 0.0186(9) 0.0145(9) 0.0191(9) 0.0022(7) 0.0033(7) 0.0008(7) O1 0.0310(10) 0.0203(9) 0.0249(9) 0.0069(7) 0.0054(8) 0.0054(7) N2 0.0193(9) 0.0170(9) 0.0237(10) -0.0003(7) 0.0091(8) 0.0001(7) N3 0.0197(10) 0.0219(10) 0.0256(11) 0.0005(8) 0.0103(8) -0.0011(8) C1 0.0169(10) 0.0169(10) 0.0202(11) 0.0014(8) 0.0084(9) 0.0001(8) C2 0.0164(10) 0.0153(10) 0.0201(11) 0.0014(8) 0.0069(8) 0.0005(8) C3 0.0177(10) 0.0179(11) 0.0216(11) -0.0003(9) 0.0063(9) 0.0003(8) C4 0.0198(11) 0.0233(11) 0.0158(11) 0.0008(8) 0.0059(9) -0.0018(9) C5 0.0179(10) 0.0207(11) 0.0211(11) 0.0061(9) 0.0068(9) 0.0027(9) C6 0.0179(10) 0.0156(10) 0.0253(12) 0.0024(8) 0.0111(9) 0.0011(8) C7 0.0153(10) 0.0139(10) 0.0203(11) -0.0002(8) 0.0026(8) 0.0000(8) C8 0.0245(12) 0.0188(11) 0.0216(12) 0.0010(9) 0.0066(9) 0.0044(9) C9 0.0166(10) 0.0163(10) 0.0197(11) 0.0012(8) 0.0080(8) 0.0035(8) C11 0.0193(11) 0.0166(11) 0.0266(12) -0.0027(9) 0.0113(9) -0.0054(8) C12 0.0198(11) 0.0200(11) 0.0303(13) -0.0042(9) 0.0099(10) -0.0045(9) C13 0.0280(13) 0.0216(12) 0.0361(15) -0.0104(10) 0.0124(11) -0.0052(10) C14 0.0298(13) 0.0314(14) 0.0283(14) -0.0114(11) 0.0061(11) -0.0100(11) C15 0.0217(12) 0.0285(13) 0.0307(14) -0.0015(10) 0.0036(10) -0.0053(10) C16 0.0183(11) 0.0210(11) 0.0292(13) -0.0034(9) 0.0081(9) -0.0061(9) C17 0.0177(11) 0.0264(13) 0.0331(14) -0.0026(10) 0.0044(10) 0.0021(9) C18 0.0298(13) 0.0201(12) 0.0360(15) -0.0037(10) 0.0122(11) 0.0004(10) C19 0.0162(10) 0.0249(12) 0.0210(11) 0.0028(9) 0.0074(9) -0.0027(9) C21 0.0193(11) 0.0181(11) 0.0313(13) 0.0001(9) 0.0130(10) -0.0001(9) C22 0.0194(12) 0.0257(12) 0.0414(15) 0.0028(11) 0.0128(11) -0.0006(10) C23 0.0233(13) 0.0289(14) 0.066(2) 0.0055(13) 0.0192(14) 0.0053(11) C24 0.0371(16) 0.0263(14) 0.074(2) -0.0101(14) 0.0347(16) -0.0004(12) C25 0.0394(16) 0.0354(15) 0.0461(17) -0.0155(13) 0.0273(14) -0.0139(13) C26 0.0255(12) 0.0276(13) 0.0312(14) -0.0034(10) 0.0156(11) -0.0077(10) C27 0.0306(14) 0.0498(18) 0.0264(14) 0.0039(12) 0.0086(11) -0.0055(12) C28 0.0257(14) 0.0511(19) 0.0402(17) 0.0078(14) 0.0055(12) -0.0005(13) C29 0.0287(13) 0.0288(13) 0.0196(12) -0.0039(10) 0.0076(10) 0.0031(10) O2 0.0286(9) 0.0249(9) 0.0202(9) 0.0000(7) 0.0051(7) 0.0038(7) O3 0.0279(9) 0.0309(9) 0.0246(9) 0.0112(7) 0.0083(7) 0.0120(8) C31 0.0373(15) 0.0149(11) 0.0389(15) 0.0029(10) 0.0177(12) 0.0008(10) O4 0.0232(8) 0.0165(8) 0.0267(9) 0.0021(6) 0.0119(7) 0.0045(6) _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 C19 1.941(2) . ? Pd1 C9 1.989(2) . ? Pd1 N1 2.0689(19) . ? Pd1 Cl1 2.4406(6) . ? N1 C7 1.279(3) . ? N1 O1 1.390(2) . ? N2 C9 1.260(3) . ? N2 C11 1.422(3) . ? N3 C19 1.146(3) . ? N3 C21 1.401(3) . ? C1 C6 1.401(3) . ? C1 C2 1.403(3) . ? C1 C9 1.480(3) . ? C2 C3 1.391(3) . ? C2 C7 1.483(3) . ? C3 C4 1.389(3) . ? C4 O2 1.362(3) . ? C4 C5 1.399(3) . ? C5 O3 1.368(3) . ? C5 C6 1.394(3) . ? C6 O4 1.374(3) . ? C7 C8 1.496(3) . ? C11 C16 1.400(3) . ? C11 C12 1.406(3) . ? C12 C13 1.390(4) . ? C12 C18 1.515(4) . ? C13 C14 1.385(4) . ? C14 C15 1.379(4) . ? C15 C16 1.399(4) . ? C16 C17 1.509(3) . ? C21 C26 1.394(4) . ? C21 C22 1.402(4) . ? C22 C23 1.389(4) . ? C22 C28 1.498(4) . ? C23 C24 1.379(5) . ? C24 C25 1.381(5) . ? C25 C26 1.395(4) . ? C26 C27 1.497(4) . ? C29 O2 1.432(3) . ? C30 O3 1.481(5) . ? C30' O3 1.368(6) . ? C31 O4 1.440(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 C19 Pd1 C9 90.50(9) . . ? C19 Pd1 N1 175.06(8) . . ? C9 Pd1 N1 84.74(8) . . ? C19 Pd1 Cl1 96.55(7) . . ? C9 Pd1 Cl1 171.35(6) . . ? N1 Pd1 Cl1 88.30(5) . . ? C7 N1 O1 114.52(19) . . ? C7 N1 Pd1 128.82(15) . . ? O1 N1 Pd1 115.72(14) . . ? C9 N2 C11 122.2(2) . . ? C19 N3 C21 177.3(2) . . ? C6 C1 C2 118.1(2) . . ? C6 C1 C9 121.1(2) . . ? C2 C1 C9 120.7(2) . . ? C3 C2 C1 120.9(2) . . ? C3 C2 C7 117.5(2) . . ? C1 C2 C7 121.5(2) . . ? C4 C3 C2 120.3(2) . . ? O2 C4 C3 124.0(2) . . ? O2 C4 C5 116.3(2) . . ? C3 C4 C5 119.7(2) . . ? O3 C5 C6 120.4(2) . . ? O3 C5 C4 119.7(2) . . ? C6 C5 C4 119.8(2) . . ? O4 C6 C5 119.5(2) . . ? O4 C6 C1 119.4(2) . . ? C5 C6 C1 121.1(2) . . ? N1 C7 C2 117.2(2) . . ? N1 C7 C8 122.2(2) . . ? C2 C7 C8 120.5(2) . . ? N2 C9 C1 121.9(2) . . ? N2 C9 Pd1 127.16(18) . . ? C1 C9 Pd1 110.65(15) . . ? C16 C11 C12 121.1(2) . . ? C16 C11 N2 120.9(2) . . ? C12 C11 N2 117.8(2) . . ? C13 C12 C11 118.4(2) . . ? C13 C12 C18 120.7(2) . . ? C11 C12 C18 120.9(2) . . ? C14 C13 C12 121.3(2) . . ? C15 C14 C13 119.6(2) . . ? C14 C15 C16 121.4(2) . . ? C15 C16 C11 118.2(2) . . ? C15 C16 C17 119.4(2) . . ? C11 C16 C17 122.5(2) . . ? N3 C19 Pd1 179.0(2) . . ? C26 C21 N3 117.9(2) . . ? C26 C21 C22 124.8(2) . . ? N3 C21 C22 117.3(2) . . ? C23 C22 C21 116.0(3) . . ? C23 C22 C28 122.6(3) . . ? C21 C22 C28 121.4(2) . . ? C24 C23 C22 121.2(3) . . ? C23 C24 C25 120.9(3) . . ? C24 C25 C26 121.0(3) . . ? C21 C26 C25 116.0(3) . . ? C21 C26 C27 121.3(2) . . ? C25 C26 C27 122.7(3) . . ? C4 O2 C29 116.94(18) . . ? C5 O3 C30' 116.7(3) . . ? C5 O3 C30 114.7(2) . . ? C30' O3 C30 24.3(3) . . ? C6 O4 C31 112.90(18) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H01A Cl1 0.87(4) 2.25(4) 3.030(2) 149(4) . C8 H8A Cl1 0.98 2.82 3.681(3) 147.5 4_576 _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.171 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.094 # Attachment '- 9_aab112s.cif' data_aab112s _database_code_depnum_ccdc_archive 'CCDC 837026' #TrackingRef '- 9_aab112s.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 Cl8 N4 O2 Pd2' _chemical_formula_weight 1053.09 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' Cl Cl 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M ' P 2(1)/n' 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 16.9138(6) _cell_length_b 11.0175(4) _cell_length_c 22.5029(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.541(2) _cell_angle_gamma 90.00 _cell_volume 4193.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8505 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.66 _exptl_crystal_description plate _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 1.405 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8385 _exptl_absorpt_correction_T_max 0.9331 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47665 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.26 _reflns_number_total 9799 _reflns_number_gt 8119 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure contains two solvent residues: one dicholoromethane is disordered over two positions, ca (83:17%) and an ill-defined region of residual electron density was identified also as disorderd dicholoromethane, but the refinement was far from satisfactory. Only the hydrogen of the main part of one dicholoromethane was included in the refinement. OH free with DFIX, rigid methyls others riding ; _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^)+(0.0326P)^2^+6.3253P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9799 _refine_ls_number_parameters 527 _refine_ls_number_restraints 144 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.0935 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.121 _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 0.862240(14) 0.22946(2) 0.436273(11) 0.01609(7) Uani 1 1 d . . . Pd2 Pd 0.688080(15) 0.26874(2) 0.382089(11) 0.01668(7) Uani 1 1 d . . . N1 N 0.89140(16) 0.0614(3) 0.46790(13) 0.0188(6) Uani 1 1 d . . . O1 O 0.92199(16) -0.0203(2) 0.42676(12) 0.0262(6) Uani 1 1 d D . . H01 H 0.939(3) 0.027(4) 0.4005(18) 0.059(17) Uiso 1 1 d D . . N2 N 0.70421(16) 0.2352(2) 0.47091(13) 0.0174(6) Uani 1 1 d . . . N21 N 0.66987(17) 0.3165(3) 0.29599(13) 0.0216(6) Uani 1 1 d . . . O21 O 0.65758(18) 0.2209(2) 0.25641(12) 0.0298(6) Uani 1 1 d D . . H021 H 0.644(3) 0.166(4) 0.2795(19) 0.063(18) Uiso 1 1 d D . . N22 N 0.82542(16) 0.3987(3) 0.40891(12) 0.0165(6) Uani 1 1 d . . . Cl1 Cl 0.96671(5) 0.20708(8) 0.36358(4) 0.02501(19) Uani 1 1 d . . . Cl2 Cl 0.61828(6) 0.08002(8) 0.36486(4) 0.0278(2) Uani 1 1 d . . . C1 C 0.79435(19) 0.1912(3) 0.55368(15) 0.0199(7) Uani 1 1 d . . . C2 C 0.8423(2) 0.0899(3) 0.56553(15) 0.0205(7) Uani 1 1 d . . . C3 C 0.8611(2) 0.0597(4) 0.62456(17) 0.0284(9) Uani 1 1 d . . . H3 H 0.8919 -0.0105 0.6329 0.034 Uiso 1 1 calc R . . C4 C 0.8349(2) 0.1320(4) 0.67053(17) 0.0338(10) Uani 1 1 d . . . H4 H 0.8490 0.1125 0.7104 0.041 Uiso 1 1 calc R . . C5 C 0.7883(2) 0.2327(4) 0.65873(17) 0.0325(9) Uani 1 1 d . . . H5 H 0.7703 0.2818 0.6906 0.039 Uiso 1 1 calc R . . C6 C 0.7679(2) 0.2621(4) 0.60096(16) 0.0253(8) Uani 1 1 d . . . H6 H 0.7357 0.3311 0.5933 0.030 Uiso 1 1 calc R . . C7 C 0.8730(2) 0.0117(3) 0.51795(16) 0.0210(7) Uani 1 1 d . . . C8 C 0.8829(2) -0.1210(3) 0.52753(17) 0.0294(9) Uani 1 1 d . . . H8A H 0.9387 -0.1391 0.5357 0.044 Uiso 1 1 calc R . . H8B H 0.8655 -0.1649 0.4918 0.044 Uiso 1 1 calc R . . H8C H 0.8509 -0.1466 0.5614 0.044 Uiso 1 1 calc R . . C9 C 0.7746(2) 0.2218(3) 0.49126(15) 0.0180(7) Uani 1 1 d . . . C11 C 0.63525(19) 0.2120(3) 0.50728(15) 0.0184(7) Uani 1 1 d . . . C12 C 0.6173(2) 0.0931(3) 0.52425(15) 0.0200(7) Uani 1 1 d . . . C13 C 0.5500(2) 0.0756(4) 0.55847(16) 0.0254(8) Uani 1 1 d . . . H13 H 0.5360 -0.0042 0.5704 0.030 Uiso 1 1 calc R . . C14 C 0.5037(2) 0.1717(4) 0.57530(17) 0.0288(9) Uani 1 1 d . . . H14 H 0.4584 0.1578 0.5990 0.035 Uiso 1 1 calc R . . C15 C 0.5224(2) 0.2882(4) 0.55807(17) 0.0292(9) Uani 1 1 d . . . H15 H 0.4900 0.3539 0.5702 0.035 Uiso 1 1 calc R . . C16 C 0.5883(2) 0.3107(3) 0.52313(16) 0.0224(7) Uani 1 1 d . . . C17 C 0.6084(2) 0.4372(3) 0.50294(19) 0.0318(9) Uani 1 1 d . . . H17A H 0.5991 0.4440 0.4600 0.048 Uiso 1 1 calc R . . H17B H 0.6641 0.4542 0.5119 0.048 Uiso 1 1 calc R . . H17C H 0.5750 0.4959 0.5238 0.048 Uiso 1 1 calc R . . C18 C 0.6668(2) -0.0151(3) 0.50753(17) 0.0236(8) Uani 1 1 d . . . H18A H 0.6991 -0.0402 0.5418 0.035 Uiso 1 1 calc R . . H18B H 0.7014 0.0066 0.4745 0.035 Uiso 1 1 calc R . . H18C H 0.6321 -0.0822 0.4955 0.035 Uiso 1 1 calc R . . C21 C 0.72248(19) 0.5272(3) 0.36427(15) 0.0186(7) Uani 1 1 d . . . C22 C 0.6820(2) 0.5308(3) 0.30933(15) 0.0186(7) Uani 1 1 d . . . C23 C 0.6506(2) 0.6407(3) 0.28936(16) 0.0227(8) Uani 1 1 d . . . H23 H 0.6243 0.6443 0.2519 0.027 Uiso 1 1 calc R . . C24 C 0.6574(2) 0.7445(3) 0.32358(17) 0.0254(8) Uani 1 1 d . . . H24 H 0.6351 0.8184 0.3097 0.031 Uiso 1 1 calc R . . C25 C 0.6964(2) 0.7416(3) 0.37785(16) 0.0240(8) Uani 1 1 d . . . H25 H 0.7011 0.8133 0.4011 0.029 Uiso 1 1 calc R . . C26 C 0.7287(2) 0.6334(3) 0.39807(16) 0.0213(7) Uani 1 1 d . . . H26 H 0.7555 0.6314 0.4354 0.026 Uiso 1 1 calc R . . C27 C 0.6708(2) 0.4218(3) 0.27144(15) 0.0210(7) Uani 1 1 d . . . C28 C 0.6577(2) 0.4359(4) 0.20550(16) 0.0302(9) Uani 1 1 d . . . H28A H 0.6016 0.4523 0.1975 0.045 Uiso 1 1 calc R . . H28B H 0.6732 0.3611 0.1852 0.045 Uiso 1 1 calc R . . H28C H 0.6896 0.5037 0.1909 0.045 Uiso 1 1 calc R . . C29 C 0.75496(19) 0.4116(3) 0.38775(14) 0.0174(7) Uani 1 1 d . . . C31 C 0.8839(2) 0.4946(3) 0.40676(16) 0.0193(7) Uani 1 1 d . . . C32 C 0.9172(2) 0.5254(3) 0.35198(17) 0.0229(8) Uani 1 1 d . . . C33 C 0.9753(2) 0.6154(4) 0.35187(18) 0.0285(9) Uani 1 1 d . . . H33 H 0.9983 0.6392 0.3153 0.034 Uiso 1 1 calc R . . C34 C 0.9998(2) 0.6703(3) 0.4038(2) 0.0327(9) Uani 1 1 d . . . H34 H 1.0397 0.7309 0.4029 0.039 Uiso 1 1 calc R . . C35 C 0.9666(2) 0.6374(3) 0.45704(18) 0.0280(9) Uani 1 1 d . . . H35 H 0.9844 0.6756 0.4926 0.034 Uiso 1 1 calc R . . C36 C 0.9078(2) 0.5498(3) 0.46000(16) 0.0235(8) Uani 1 1 d . . . C37 C 0.8690(2) 0.5197(4) 0.51816(16) 0.0288(9) Uani 1 1 d . . . H37A H 0.8978 0.5594 0.5507 0.043 Uiso 1 1 calc R . . H37B H 0.8697 0.4316 0.5242 0.043 Uiso 1 1 calc R . . H37C H 0.8141 0.5485 0.5174 0.043 Uiso 1 1 calc R . . C38 C 0.8920(2) 0.4649(3) 0.29483(16) 0.0242(8) Uani 1 1 d . . . H38A H 0.8404 0.4968 0.2822 0.036 Uiso 1 1 calc R . . H38B H 0.8880 0.3771 0.3011 0.036 Uiso 1 1 calc R . . H38C H 0.9311 0.4814 0.2640 0.036 Uiso 1 1 calc R . . C92 C 0.3802(4) -0.1648(5) 0.2143(3) 0.0434(15) Uani 0.826(3) 1 d PDU A 1 H92 H 0.4268 -0.1657 0.1872 0.052 Uiso 0.826(3) 1 calc PR A 1 Cl6 Cl 0.32351(11) -0.29502(17) 0.20036(9) 0.0723(7) Uani 0.826(3) 1 d PD A 1 Cl7 Cl 0.41523(9) -0.16368(17) 0.28786(7) 0.0582(5) Uani 0.826(3) 1 d PD A 1 Cl8 Cl 0.32500(11) -0.03480(17) 0.19939(9) 0.0698(6) Uani 0.826(3) 1 d PD A 1 C92' C 0.3933(16) -0.1741(15) 0.2255(11) 0.061(9) Uiso 0.174(3) 1 d PDU A 2 Cl6' Cl 0.3837(7) -0.0414(10) 0.2662(5) 0.098(4) Uiso 0.174(3) 1 d PD A 2 Cl7' Cl 0.3083(7) -0.1916(11) 0.1823(5) 0.090(3) Uiso 0.174(3) 1 d PD A 2 Cl8' Cl 0.4098(7) -0.3005(11) 0.2696(6) 0.102(4) Uiso 0.174(3) 1 d PD A 2 C91 C 0.4686(6) 0.2787(8) 0.3398(4) 0.043(3) Uiso 0.482(5) 1 d PDU B 1 Cl3 Cl 0.4095(2) 0.1850(4) 0.29843(16) 0.0380(9) Uani 0.482(5) 1 d PDU B 1 Cl4 Cl 0.4699(3) 0.4235(7) 0.3108(4) 0.0637(19) Uani 0.482(5) 1 d PDU B 1 Cl5 Cl 0.4577(3) 0.2811(3) 0.41633(13) 0.0716(15) Uani 0.482(5) 1 d PDU B 1 C91' C 0.4463(5) 0.2785(7) 0.3559(4) 0.037(2) Uiso 0.518(5) 1 d PDU B 2 Cl3' Cl 0.3757(3) 0.2859(3) 0.41152(13) 0.0865(19) Uani 0.518(5) 1 d PDU B 2 Cl4' Cl 0.3911(6) 0.1951(7) 0.3078(4) 0.188(4) Uani 0.518(5) 1 d PDU B 2 Cl5' Cl 0.4669(5) 0.4259(7) 0.3310(4) 0.090(3) Uani 0.518(5) 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01516(13) 0.01871(14) 0.01439(13) 0.00115(10) -0.00072(10) 0.00083(10) Pd2 0.01812(13) 0.01687(13) 0.01503(13) -0.00101(10) -0.00144(10) -0.00050(10) N1 0.0185(14) 0.0203(15) 0.0174(15) -0.0001(12) -0.0030(12) 0.0031(11) O1 0.0319(15) 0.0261(15) 0.0207(14) -0.0017(11) 0.0021(12) 0.0072(11) N2 0.0199(14) 0.0146(14) 0.0177(14) -0.0028(11) 0.0004(11) -0.0011(11) N21 0.0258(16) 0.0236(16) 0.0154(15) -0.0052(12) -0.0028(12) -0.0004(12) O21 0.0467(17) 0.0239(15) 0.0188(14) -0.0041(12) -0.0033(12) -0.0031(13) N22 0.0169(14) 0.0179(15) 0.0146(14) -0.0006(11) 0.0012(11) -0.0010(11) Cl1 0.0210(4) 0.0306(5) 0.0235(4) 0.0066(4) 0.0052(3) 0.0054(3) Cl2 0.0390(5) 0.0227(5) 0.0215(4) -0.0017(4) -0.0040(4) -0.0104(4) C1 0.0154(16) 0.0258(19) 0.0184(17) 0.0007(14) -0.0007(13) -0.0049(14) C2 0.0175(17) 0.0267(19) 0.0171(17) 0.0018(14) -0.0017(14) -0.0054(14) C3 0.025(2) 0.036(2) 0.024(2) 0.0102(17) -0.0040(16) -0.0042(16) C4 0.038(2) 0.046(3) 0.0173(19) 0.0057(17) -0.0041(17) -0.0116(19) C5 0.035(2) 0.045(2) 0.0172(19) -0.0072(17) 0.0046(16) -0.0085(19) C6 0.0233(18) 0.030(2) 0.0225(19) -0.0045(15) 0.0012(15) -0.0011(15) C7 0.0173(17) 0.0246(19) 0.0211(18) 0.0027(14) -0.0074(14) -0.0005(14) C8 0.034(2) 0.027(2) 0.027(2) 0.0057(16) -0.0052(17) 0.0041(16) C9 0.0211(17) 0.0153(16) 0.0175(17) -0.0019(13) 0.0018(13) 0.0006(13) C11 0.0157(16) 0.0265(19) 0.0131(16) -0.0020(14) -0.0015(13) -0.0002(13) C12 0.0167(17) 0.0257(19) 0.0177(17) -0.0024(14) -0.0025(13) -0.0015(14) C13 0.0226(19) 0.034(2) 0.0199(19) 0.0009(15) -0.0015(15) -0.0048(16) C14 0.0187(18) 0.041(2) 0.027(2) 0.0016(17) 0.0066(15) -0.0002(16) C15 0.0230(19) 0.040(2) 0.024(2) -0.0039(17) 0.0041(15) 0.0103(16) C16 0.0225(18) 0.0239(18) 0.0208(18) -0.0011(15) 0.0008(14) 0.0024(14) C17 0.036(2) 0.025(2) 0.034(2) -0.0010(17) 0.0107(18) 0.0087(17) C18 0.0247(19) 0.0218(19) 0.0243(19) -0.0004(15) -0.0023(15) -0.0023(15) C21 0.0154(16) 0.0203(18) 0.0202(18) 0.0021(14) 0.0028(14) -0.0007(13) C22 0.0202(17) 0.0201(18) 0.0156(17) -0.0007(13) 0.0048(14) 0.0002(13) C23 0.0241(18) 0.027(2) 0.0172(18) 0.0039(15) 0.0001(14) 0.0046(15) C24 0.030(2) 0.0164(19) 0.029(2) 0.0054(15) 0.0040(16) 0.0059(14) C25 0.0269(19) 0.0200(19) 0.025(2) -0.0017(15) 0.0067(15) 0.0012(14) C26 0.0192(17) 0.0256(19) 0.0192(18) -0.0029(14) 0.0018(14) 0.0001(14) C27 0.0195(17) 0.0253(19) 0.0181(18) -0.0002(14) 0.0006(14) -0.0001(14) C28 0.041(2) 0.031(2) 0.0182(19) 0.0004(16) -0.0031(17) 0.0067(18) C29 0.0197(17) 0.0193(17) 0.0133(16) -0.0012(13) 0.0030(13) 0.0001(13) C31 0.0168(16) 0.0167(17) 0.0244(19) 0.0009(14) -0.0029(14) -0.0004(13) C32 0.0223(18) 0.0190(18) 0.027(2) 0.0029(15) -0.0004(15) 0.0018(14) C33 0.0251(19) 0.027(2) 0.033(2) 0.0109(16) 0.0033(17) -0.0005(16) C34 0.023(2) 0.022(2) 0.053(3) 0.0042(18) -0.0092(19) -0.0065(16) C35 0.026(2) 0.0221(19) 0.035(2) -0.0077(16) -0.0114(17) 0.0006(15) C36 0.0189(18) 0.026(2) 0.025(2) -0.0019(15) -0.0063(15) 0.0050(14) C37 0.030(2) 0.033(2) 0.023(2) -0.0067(16) -0.0067(16) 0.0026(16) C38 0.0269(19) 0.0240(19) 0.0218(19) 0.0046(15) 0.0054(15) 0.0022(15) C92 0.042(3) 0.050(4) 0.038(3) -0.012(3) 0.012(3) 0.004(3) Cl6 0.0785(12) 0.0668(12) 0.0724(12) -0.0429(10) 0.0414(10) -0.0279(9) Cl7 0.0448(9) 0.0820(13) 0.0480(9) 0.0019(8) 0.0043(7) -0.0036(8) Cl8 0.0771(13) 0.0628(12) 0.0693(12) -0.0110(9) -0.0092(10) 0.0207(9) Cl3 0.0418(15) 0.0444(18) 0.0275(14) -0.0217(13) -0.0069(12) 0.0157(13) Cl4 0.035(2) 0.065(3) 0.090(5) 0.016(3) -0.009(3) -0.0109(18) Cl5 0.132(4) 0.0417(17) 0.0406(16) -0.0112(12) -0.0065(18) 0.0190(18) Cl3' 0.168(5) 0.0494(18) 0.0429(16) -0.0049(13) 0.023(2) -0.032(2) Cl4' 0.236(8) 0.160(6) 0.164(7) 0.072(5) -0.143(6) -0.121(6) Cl5' 0.094(4) 0.060(3) 0.118(6) -0.013(3) 0.053(3) -0.024(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C9 1.942(3) . ? Pd1 N1 2.042(3) . ? Pd1 N22 2.058(3) . ? Pd1 Cl1 2.4318(9) . ? Pd1 Pd2 3.2068(4) . ? Pd2 C29 1.941(3) . ? Pd2 N21 2.028(3) . ? Pd2 N2 2.048(3) . ? Pd2 Cl2 2.4205(9) . ? N1 C7 1.293(4) . ? N1 O1 1.395(4) . ? N2 C9 1.279(4) . ? N2 C11 1.454(4) . ? N21 C27 1.285(5) . ? N21 O21 1.393(4) . ? N22 C29 1.287(4) . ? N22 C31 1.449(4) . ? C1 C6 1.397(5) . ? C1 C2 1.404(5) . ? C1 C9 1.480(5) . ? C2 C3 1.403(5) . ? C2 C7 1.472(5) . ? C3 C4 1.382(6) . ? C4 C5 1.386(6) . ? C5 C6 1.380(5) . ? C7 C8 1.488(5) . ? C11 C16 1.395(5) . ? C11 C12 1.399(5) . ? C12 C13 1.394(5) . ? C12 C18 1.506(5) . ? C13 C14 1.372(5) . ? C14 C15 1.378(6) . ? C15 C16 1.392(5) . ? C16 C17 1.506(5) . ? C21 C26 1.399(5) . ? C21 C22 1.408(5) . ? C21 C29 1.482(5) . ? C22 C23 1.395(5) . ? C22 C27 1.485(5) . ? C23 C24 1.382(5) . ? C24 C25 1.383(5) . ? C25 C26 1.386(5) . ? C27 C28 1.506(5) . ? C31 C36 1.400(5) . ? C31 C32 1.402(5) . ? C32 C33 1.396(5) . ? C32 C38 1.507(5) . ? C33 C34 1.376(6) . ? C34 C35 1.375(6) . ? C35 C36 1.389(5) . ? C36 C37 1.507(5) . ? C92 Cl8 1.741(6) . ? C92 Cl7 1.753(6) . ? C92 Cl6 1.753(6) . ? C92' Cl8' 1.731(15) . ? C92' Cl6' 1.734(15) . ? C92' Cl7' 1.739(15) . ? C91 Cl3 1.707(9) . ? C91 Cl4 1.723(9) . ? C91 Cl5 1.735(9) . ? C91' Cl4' 1.694(9) . ? C91' Cl3' 1.740(9) . ? C91' Cl5' 1.754(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 C9 Pd1 N1 85.52(13) . . ? C9 Pd1 N22 89.96(12) . . ? N1 Pd1 N22 175.48(11) . . ? C9 Pd1 Cl1 171.18(10) . . ? N1 Pd1 Cl1 88.16(8) . . ? N22 Pd1 Cl1 96.34(8) . . ? C9 Pd1 Pd2 62.87(10) . . ? N1 Pd1 Pd2 118.22(8) . . ? N22 Pd1 Pd2 59.32(8) . . ? Cl1 Pd1 Pd2 115.38(2) . . ? C29 Pd2 N21 86.31(13) . . ? C29 Pd2 N2 90.58(12) . . ? N21 Pd2 N2 175.21(11) . . ? C29 Pd2 Cl2 171.80(10) . . ? N21 Pd2 Cl2 90.01(9) . . ? N2 Pd2 Cl2 93.53(8) . . ? C29 Pd2 Pd1 63.38(10) . . ? N21 Pd2 Pd1 121.93(8) . . ? N2 Pd2 Pd1 59.42(8) . . ? Cl2 Pd2 Pd1 112.95(3) . . ? C7 N1 O1 113.5(3) . . ? C7 N1 Pd1 128.9(2) . . ? O1 N1 Pd1 116.4(2) . . ? C9 N2 C11 121.8(3) . . ? C9 N2 Pd2 119.0(2) . . ? C11 N2 Pd2 118.7(2) . . ? C27 N21 O21 114.2(3) . . ? C27 N21 Pd2 130.0(2) . . ? O21 N21 Pd2 115.8(2) . . ? C29 N22 C31 122.5(3) . . ? C29 N22 Pd1 119.1(2) . . ? C31 N22 Pd1 117.7(2) . . ? C6 C1 C2 119.3(3) . . ? C6 C1 C9 121.6(3) . . ? C2 C1 C9 119.1(3) . . ? C3 C2 C1 119.6(3) . . ? C3 C2 C7 118.1(3) . . ? C1 C2 C7 122.3(3) . . ? C4 C3 C2 120.1(4) . . ? C3 C4 C5 120.3(4) . . ? C6 C5 C4 120.3(4) . . ? C5 C6 C1 120.5(4) . . ? N1 C7 C2 118.4(3) . . ? N1 C7 C8 121.0(3) . . ? C2 C7 C8 120.6(3) . . ? N2 C9 C1 124.6(3) . . ? N2 C9 Pd1 118.7(3) . . ? C1 C9 Pd1 116.6(2) . . ? C16 C11 C12 122.3(3) . . ? C16 C11 N2 118.0(3) . . ? C12 C11 N2 119.7(3) . . ? C13 C12 C11 117.4(3) . . ? C13 C12 C18 119.1(3) . . ? C11 C12 C18 123.4(3) . . ? C14 C13 C12 121.1(4) . . ? C13 C14 C15 120.5(3) . . ? C14 C15 C16 120.8(3) . . ? C15 C16 C11 117.8(3) . . ? C15 C16 C17 121.3(3) . . ? C11 C16 C17 120.9(3) . . ? C26 C21 C22 119.1(3) . . ? C26 C21 C29 120.0(3) . . ? C22 C21 C29 120.9(3) . . ? C23 C22 C21 119.2(3) . . ? C23 C22 C27 118.1(3) . . ? C21 C22 C27 122.6(3) . . ? C24 C23 C22 120.6(3) . . ? C23 C24 C25 120.6(3) . . ? C24 C25 C26 119.5(3) . . ? C25 C26 C21 120.9(3) . . ? N21 C27 C22 119.1(3) . . ? N21 C27 C28 121.0(3) . . ? C22 C27 C28 119.9(3) . . ? N22 C29 C21 124.4(3) . . ? N22 C29 Pd2 118.2(3) . . ? C21 C29 Pd2 117.3(2) . . ? C36 C31 C32 122.2(3) . . ? C36 C31 N22 118.7(3) . . ? C32 C31 N22 119.1(3) . . ? C33 C32 C31 117.5(3) . . ? C33 C32 C38 120.4(3) . . ? C31 C32 C38 122.1(3) . . ? C34 C33 C32 121.1(4) . . ? C35 C34 C33 120.1(4) . . ? C34 C35 C36 121.5(4) . . ? C35 C36 C31 117.5(3) . . ? C35 C36 C37 120.9(3) . . ? C31 C36 C37 121.6(3) . . ? Cl8 C92 Cl7 110.6(3) . . ? Cl8 C92 Cl6 110.3(4) . . ? Cl7 C92 Cl6 110.7(4) . . ? Cl8' C92' Cl6' 113.0(14) . . ? Cl8' C92' Cl7' 111.1(13) . . ? Cl6' C92' Cl7' 108.0(13) . . ? Cl3 C91 Cl4 111.3(6) . . ? Cl3 C91 Cl5 118.9(6) . . ? Cl4 C91 Cl5 111.3(6) . . ? Cl4' C91' Cl3' 96.2(6) . . ? Cl4' C91' Cl5' 114.1(6) . . ? Cl3' C91' Cl5' 109.0(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H01 Cl1 0.840(19) 2.20(3) 2.982(3) 154(5) . O21 H021 Cl2 0.828(19) 2.19(3) 2.973(3) 157(5) . _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.831 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.105 # Attachment '- 3_aab501s.cif' data_aab501s _database_code_depnum_ccdc_archive 'CCDC 837027' #TrackingRef '- 3_aab501s.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H37 Cl2 N3 O3 P2 Pd' _chemical_formula_weight 895.01 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M 'P 2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.5577(7) _cell_length_b 13.2121(9) _cell_length_c 14.6686(11) _cell_angle_alpha 90.00 _cell_angle_beta 105.436(2) _cell_angle_gamma 90.00 _cell_volume 1972.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8415 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 28.45 _exptl_crystal_description lath _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.732 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7603 _exptl_absorpt_correction_T_max 0.9643 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method '\w- & \f-scan' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31495 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 28.65 _reflns_number_total 9375 _reflns_number_gt 9201 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. OH free with DFIX, methyls riding, others rigid ; _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^)+(0.0367P)^2^+0.3646P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(14) _refine_ls_number_reflns 9375 _refine_ls_number_parameters 501 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0690 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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 0.194954(16) 0.200875(13) 0.602410(11) 0.01466(5) Uani 1 1 d . . . Cl1 Cl 0.27739(6) 0.36150(5) 0.60107(5) 0.02108(13) Uani 1 1 d . . . Cl2 Cl 0.05328(7) 0.23486(5) 0.70568(5) 0.02677(15) Uani 1 1 d . . . N1 N 0.1311(2) 0.05761(17) 0.59000(15) 0.0180(4) Uani 1 1 d . . . O1 O 0.0343(2) 0.02160(15) 0.62858(14) 0.0255(4) Uani 1 1 d D . . H01 H 0.021(3) 0.0765(17) 0.651(2) 0.029(9) Uiso 1 1 d D . . C1 C 0.3050(2) 0.1459(2) 0.52375(16) 0.0170(5) Uani 1 1 d . . . C2 C 0.2810(3) 0.0409(2) 0.50360(18) 0.0180(5) Uani 1 1 d . . . C3 C 0.3512(3) -0.0130(2) 0.45141(18) 0.0214(5) Uani 1 1 d . . . H3 H 0.3356 -0.0833 0.4405 0.026 Uiso 1 1 calc R . . C4 C 0.4435(3) 0.0358(2) 0.41542(18) 0.0232(6) Uani 1 1 d . . . H4 H 0.4917 0.0004 0.3792 0.028 Uiso 1 1 calc R . . N2 N 0.5572(2) 0.1924(2) 0.39333(16) 0.0286(5) Uani 1 1 d . . . O2 O 0.5812(3) 0.2813(2) 0.4148(2) 0.0705(11) Uani 1 1 d . . . O3 O 0.6041(2) 0.14870(18) 0.33791(17) 0.0399(6) Uani 1 1 d . . . C5 C 0.4630(3) 0.1384(2) 0.43433(18) 0.0208(5) Uani 1 1 d . . . C6 C 0.3962(2) 0.1929(3) 0.48917(16) 0.0199(5) Uani 1 1 d . . . H6 H 0.4150 0.2625 0.5020 0.024 Uiso 1 1 calc R . . C7 C 0.1783(3) -0.0061(2) 0.54009(18) 0.0197(5) Uani 1 1 d . . . C8 C 0.1335(3) -0.1132(2) 0.5249(2) 0.0247(6) Uani 1 1 d . . . H8A H 0.1922 -0.1566 0.5719 0.037 Uiso 1 1 calc R . . H8B H 0.1350 -0.1348 0.4613 0.037 Uiso 1 1 calc R . . H8C H 0.0438 -0.1188 0.5315 0.037 Uiso 1 1 calc R . . N3 N 0.0733(2) 0.79833(16) 0.91644(15) 0.0154(4) Uani 1 1 d . . . P1 P -0.05394(6) 0.76346(5) 0.83717(4) 0.01289(12) Uani 1 1 d . . . P2 P 0.22294(6) 0.76436(5) 0.94294(4) 0.01255(13) Uani 1 1 d . . . C21 C -0.1642(2) 0.6974(2) 0.89189(16) 0.0164(4) Uani 1 1 d . . . C22 C -0.1389(2) 0.6928(2) 0.98987(17) 0.0194(5) Uani 1 1 d . . . H22 H -0.0636 0.7258 1.0284 0.023 Uiso 1 1 calc R . . C23 C -0.2225(3) 0.6405(2) 1.0317(2) 0.0256(6) Uani 1 1 d . . . H23 H -0.2060 0.6389 1.0986 0.031 Uiso 1 1 calc R . . C24 C -0.3304(3) 0.5904(2) 0.9750(2) 0.0247(6) Uani 1 1 d . . . H24 H -0.3865 0.5530 1.0035 0.030 Uiso 1 1 calc R . . C25 C -0.3576(3) 0.5942(2) 0.8771(2) 0.0246(6) Uani 1 1 d . . . H25 H -0.4322 0.5601 0.8390 0.029 Uiso 1 1 calc R . . C26 C -0.2753(3) 0.6480(2) 0.8350(2) 0.0211(5) Uani 1 1 d . . . H26 H -0.2939 0.6515 0.7681 0.025 Uiso 1 1 calc R . . C31 C -0.0236(2) 0.68054(17) 0.74851(16) 0.0147(5) Uani 1 1 d . . . C32 C 0.0234(3) 0.72260(18) 0.67601(18) 0.0192(5) Uani 1 1 d . . . H32 H 0.0277 0.7940 0.6696 0.023 Uiso 1 1 calc R . . C33 C 0.0635(3) 0.6593(2) 0.61402(19) 0.0217(5) Uani 1 1 d . . . H33 H 0.0938 0.6874 0.5640 0.026 Uiso 1 1 calc R . . C34 C 0.0599(3) 0.5553(2) 0.62416(19) 0.0218(6) Uani 1 1 d . . . H34 H 0.0905 0.5125 0.5825 0.026 Uiso 1 1 calc R . . C35 C 0.0121(3) 0.5134(2) 0.69480(19) 0.0207(5) Uani 1 1 d . . . H35 H 0.0083 0.4420 0.7008 0.025 Uiso 1 1 calc R . . C36 C -0.0304(2) 0.57572(19) 0.75682(18) 0.0182(5) Uani 1 1 d . . . H36 H -0.0640 0.5470 0.8049 0.022 Uiso 1 1 calc R . . C41 C -0.1352(2) 0.87465(19) 0.77814(17) 0.0152(5) Uani 1 1 d . . . C42 C -0.2276(3) 0.8668(2) 0.69030(19) 0.0220(5) Uani 1 1 d . . . H42 H -0.2485 0.8023 0.6616 0.026 Uiso 1 1 calc R . . C43 C -0.2886(3) 0.9523(2) 0.6452(2) 0.0268(6) Uani 1 1 d . . . H43 H -0.3505 0.9467 0.5851 0.032 Uiso 1 1 calc R . . C44 C -0.2600(3) 1.0466(2) 0.6872(2) 0.0268(6) Uani 1 1 d . . . H44 H -0.3029 1.1052 0.6563 0.032 Uiso 1 1 calc R . . C45 C -0.1683(3) 1.0553(2) 0.7748(2) 0.0241(6) Uani 1 1 d . . . H45 H -0.1482 1.1199 0.8033 0.029 Uiso 1 1 calc R . . C46 C -0.1062(3) 0.96945(19) 0.82039(18) 0.0179(5) Uani 1 1 d . . . H46 H -0.0440 0.9753 0.8803 0.021 Uiso 1 1 calc R . . C51 C 0.2509(2) 0.6329(2) 0.92094(17) 0.0140(5) Uani 1 1 d . . . C52 C 0.2972(2) 0.6012(2) 0.84552(18) 0.0171(5) Uani 1 1 d . . . H52 H 0.3237 0.6496 0.8063 0.020 Uiso 1 1 calc R . . C53 C 0.3048(3) 0.4986(2) 0.8277(2) 0.0217(6) Uani 1 1 d . . . H53 H 0.3368 0.4769 0.7762 0.026 Uiso 1 1 calc R . . C54 C 0.2663(3) 0.4277(2) 0.8839(2) 0.0261(6) Uani 1 1 d . . . H54 H 0.2717 0.3576 0.8711 0.031 Uiso 1 1 calc R . . C55 C 0.2196(3) 0.4593(2) 0.9590(2) 0.0297(7) Uani 1 1 d . . . H55 H 0.1930 0.4105 0.9978 0.036 Uiso 1 1 calc R . . C56 C 0.2113(3) 0.5613(2) 0.97787(19) 0.0243(6) Uani 1 1 d . . . H56 H 0.1788 0.5826 1.0293 0.029 Uiso 1 1 calc R . . C61 C 0.3183(2) 0.84057(19) 0.88342(18) 0.0155(5) Uani 1 1 d . . . C62 C 0.4501(3) 0.8210(2) 0.8913(2) 0.0253(6) Uani 1 1 d . . . H62 H 0.4913 0.7644 0.9270 0.030 Uiso 1 1 calc R . . C63 C 0.5221(3) 0.8829(2) 0.8478(2) 0.0320(7) Uani 1 1 d . . . H63 H 0.6115 0.8677 0.8521 0.038 Uiso 1 1 calc R . . C64 C 0.4626(3) 0.9678(2) 0.7974(2) 0.0265(6) Uani 1 1 d . . . H64 H 0.5119 1.0110 0.7680 0.032 Uiso 1 1 calc R . . C65 C 0.3328(3) 0.9891(2) 0.79033(19) 0.0239(6) Uani 1 1 d . . . H65 H 0.2932 1.0476 0.7569 0.029 Uiso 1 1 calc R . . C66 C 0.2590(3) 0.9252(2) 0.83210(18) 0.0173(5) Uani 1 1 d . . . H66 H 0.1688 0.9391 0.8257 0.021 Uiso 1 1 calc R . . C71 C 0.2877(3) 0.78188(18) 1.06833(17) 0.0163(5) Uani 1 1 d . . . C72 C 0.4115(3) 0.7431(2) 1.1139(2) 0.0259(6) Uani 1 1 d . . . H72 H 0.4608 0.7073 1.0787 0.031 Uiso 1 1 calc R . . C73 C 0.4624(3) 0.7568(2) 1.2105(2) 0.0282(6) Uani 1 1 d . . . H73 H 0.5476 0.7321 1.2412 0.034 Uiso 1 1 calc R . . C74 C 0.3889(3) 0.8066(2) 1.26201(19) 0.0262(6) Uani 1 1 d . . . H74 H 0.4236 0.8151 1.3283 0.031 Uiso 1 1 calc R . . C75 C 0.2655(3) 0.8441(2) 1.21784(19) 0.0268(6) Uani 1 1 d . . . H75 H 0.2153 0.8775 1.2538 0.032 Uiso 1 1 calc R . . C76 C 0.2151(3) 0.8326(2) 1.12020(17) 0.0189(5) Uani 1 1 d . . . H76 H 0.1312 0.8596 1.0894 0.023 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 0.01498(8) 0.01534(8) 0.01412(8) -0.00094(8) 0.00469(6) 0.00148(8) Cl1 0.0216(3) 0.0167(3) 0.0263(3) -0.0036(2) 0.0088(3) -0.0005(2) Cl2 0.0336(4) 0.0217(3) 0.0326(3) -0.0021(3) 0.0221(3) 0.0013(3) N1 0.0186(11) 0.0210(11) 0.0150(10) 0.0016(8) 0.0056(8) -0.0005(9) O1 0.0303(11) 0.0222(10) 0.0287(10) 0.0004(8) 0.0161(9) -0.0036(8) C1 0.0166(12) 0.0229(13) 0.0094(10) -0.0013(9) -0.0001(9) 0.0096(10) C2 0.0205(13) 0.0188(12) 0.0146(11) 0.0041(10) 0.0046(10) 0.0015(10) C3 0.0286(15) 0.0170(12) 0.0185(12) -0.0004(10) 0.0062(11) 0.0052(11) C4 0.0254(14) 0.0270(14) 0.0172(12) -0.0025(11) 0.0060(11) 0.0090(11) N2 0.0208(10) 0.0396(14) 0.0285(11) -0.0091(13) 0.0122(9) -0.0085(13) O2 0.078(2) 0.0604(18) 0.100(2) -0.0452(18) 0.071(2) -0.0478(16) O3 0.0461(14) 0.0438(14) 0.0424(13) -0.0042(11) 0.0336(12) 0.0029(11) C5 0.0172(13) 0.0290(14) 0.0163(12) -0.0011(10) 0.0047(10) -0.0008(10) C6 0.0179(11) 0.0207(12) 0.0172(10) -0.0042(12) -0.0023(9) 0.0013(12) C7 0.0222(13) 0.0207(12) 0.0146(11) 0.0020(10) 0.0019(10) 0.0000(10) C8 0.0336(16) 0.0187(13) 0.0222(13) 0.0011(10) 0.0081(12) 0.0009(11) N3 0.0129(10) 0.0159(10) 0.0179(10) -0.0022(8) 0.0051(8) -0.0006(8) P1 0.0113(3) 0.0129(3) 0.0146(3) -0.0009(2) 0.0036(2) 0.0003(2) P2 0.0115(3) 0.0133(3) 0.0130(3) -0.0013(2) 0.0034(2) -0.0005(2) C21 0.0137(10) 0.0121(9) 0.0248(11) 0.0018(12) 0.0077(8) 0.0022(12) C22 0.0210(11) 0.0143(11) 0.0233(11) -0.0009(12) 0.0063(9) 0.0015(12) C23 0.0313(16) 0.0243(14) 0.0237(13) 0.0042(11) 0.0119(12) 0.0001(11) C24 0.0197(14) 0.0187(13) 0.0408(16) 0.0084(12) 0.0170(12) 0.0017(10) C25 0.0125(12) 0.0250(14) 0.0372(16) 0.0010(12) 0.0083(11) -0.0004(10) C26 0.0138(12) 0.0231(14) 0.0257(13) 0.0028(11) 0.0040(10) 0.0040(10) C31 0.0105(10) 0.0152(14) 0.0169(10) -0.0031(9) 0.0010(8) 0.0003(8) C32 0.0180(12) 0.0163(14) 0.0229(12) -0.0036(9) 0.0046(10) -0.0006(9) C33 0.0211(13) 0.0253(12) 0.0202(12) -0.0028(11) 0.0078(11) -0.0023(11) C34 0.0172(13) 0.0248(14) 0.0210(13) -0.0097(11) 0.0008(10) 0.0031(10) C35 0.0179(13) 0.0148(12) 0.0252(13) -0.0043(10) -0.0015(11) 0.0010(10) C36 0.0148(12) 0.0171(12) 0.0208(12) -0.0005(10) 0.0014(10) -0.0025(10) C41 0.0121(12) 0.0174(12) 0.0171(11) 0.0021(9) 0.0056(9) 0.0035(9) C42 0.0197(14) 0.0228(13) 0.0218(13) 0.0000(11) 0.0025(11) 0.0018(11) C43 0.0244(15) 0.0313(15) 0.0220(14) 0.0034(12) 0.0013(11) 0.0068(12) C44 0.0288(15) 0.0242(14) 0.0319(15) 0.0091(12) 0.0160(12) 0.0116(12) C45 0.0314(16) 0.0163(13) 0.0295(14) -0.0003(11) 0.0165(12) 0.0012(11) C46 0.0175(13) 0.0196(12) 0.0190(12) -0.0013(10) 0.0089(10) 0.0011(10) C51 0.0122(12) 0.0167(11) 0.0134(11) -0.0022(9) 0.0038(9) 0.0018(9) C52 0.0097(12) 0.0234(13) 0.0175(12) -0.0025(10) 0.0025(9) -0.0022(10) C53 0.0116(12) 0.0257(14) 0.0269(14) -0.0072(11) 0.0035(11) 0.0002(10) C54 0.0258(15) 0.0173(13) 0.0312(15) -0.0067(11) 0.0009(12) 0.0014(11) C55 0.0441(19) 0.0161(13) 0.0302(15) 0.0052(12) 0.0121(14) 0.0006(12) C56 0.0321(16) 0.0233(14) 0.0196(13) 0.0007(11) 0.0106(12) 0.0028(12) C61 0.0140(12) 0.0156(12) 0.0175(12) -0.0039(9) 0.0049(10) -0.0025(9) C62 0.0177(14) 0.0200(13) 0.0394(16) 0.0022(12) 0.0097(12) 0.0031(10) C63 0.0190(14) 0.0309(16) 0.0515(19) -0.0025(14) 0.0187(14) -0.0012(12) C64 0.0253(15) 0.0280(15) 0.0310(15) -0.0036(12) 0.0160(12) -0.0105(12) C65 0.0278(15) 0.0227(13) 0.0215(13) 0.0023(11) 0.0072(11) -0.0050(11) C66 0.0149(13) 0.0209(13) 0.0159(12) 0.0012(10) 0.0034(10) -0.0006(10) C71 0.0190(12) 0.0142(11) 0.0150(11) -0.0017(9) 0.0031(10) -0.0014(9) C72 0.0193(13) 0.0330(15) 0.0227(13) -0.0074(11) 0.0013(11) 0.0079(11) C73 0.0239(14) 0.0326(16) 0.0218(13) -0.0045(12) -0.0049(11) 0.0036(12) C74 0.0355(17) 0.0235(14) 0.0155(12) -0.0042(11) -0.0003(12) 0.0005(12) C75 0.0344(17) 0.0262(15) 0.0189(13) -0.0075(11) 0.0054(12) 0.0026(12) C76 0.0188(13) 0.0214(12) 0.0149(11) -0.0009(10) 0.0020(10) 0.0026(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.981(2) . ? Pd1 N1 2.001(2) . ? Pd1 Cl1 2.2958(7) . ? Pd1 Cl2 2.4371(7) . ? N1 C7 1.299(3) . ? N1 O1 1.378(3) . ? C1 C6 1.353(4) . ? C1 C2 1.426(4) . ? C2 C3 1.395(4) . ? C2 C7 1.469(4) . ? C3 C4 1.385(4) . ? C4 C5 1.387(4) . ? N2 O3 1.206(3) . ? N2 O2 1.224(4) . ? N2 C5 1.476(4) . ? C5 C6 1.402(4) . ? C7 C8 1.490(4) . ? N3 P2 1.588(2) . ? N3 P1 1.593(2) . ? P1 C31 1.793(2) . ? P1 C41 1.803(2) . ? P1 C21 1.806(3) . ? P2 C71 1.799(3) . ? P2 C61 1.805(3) . ? P2 C51 1.805(3) . ? C21 C22 1.392(3) . ? C21 C26 1.405(4) . ? C22 C23 1.386(4) . ? C23 C24 1.387(4) . ? C24 C25 1.389(4) . ? C25 C26 1.388(4) . ? C31 C36 1.394(3) . ? C31 C32 1.403(4) . ? C32 C33 1.382(4) . ? C33 C34 1.383(4) . ? C34 C35 1.384(4) . ? C35 C36 1.387(4) . ? C41 C46 1.395(4) . ? C41 C42 1.398(4) . ? C42 C43 1.380(4) . ? C43 C44 1.386(4) . ? C44 C45 1.392(4) . ? C45 C46 1.389(4) . ? C51 C52 1.388(3) . ? C51 C56 1.398(4) . ? C52 C53 1.388(4) . ? C53 C54 1.378(4) . ? C54 C55 1.386(4) . ? C55 C56 1.384(4) . ? C61 C62 1.390(4) . ? C61 C66 1.399(4) . ? C62 C63 1.382(4) . ? C63 C64 1.398(4) . ? C64 C65 1.375(4) . ? C65 C66 1.396(4) . ? C71 C76 1.388(4) . ? C71 C72 1.398(4) . ? C72 C73 1.386(4) . ? C73 C74 1.386(4) . ? C74 C75 1.383(4) . ? C75 C76 1.397(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 C1 Pd1 N1 80.54(10) . . ? C1 Pd1 Cl1 92.97(8) . . ? N1 Pd1 Cl1 173.13(6) . . ? C1 Pd1 Cl2 169.08(8) . . ? N1 Pd1 Cl2 89.03(6) . . ? Cl1 Pd1 Cl2 97.58(2) . . ? C7 N1 O1 116.4(2) . . ? C7 N1 Pd1 119.59(19) . . ? O1 N1 Pd1 123.92(16) . . ? C6 C1 C2 118.2(2) . . ? C6 C1 Pd1 129.5(2) . . ? C2 C1 Pd1 112.2(2) . . ? C3 C2 C1 121.3(2) . . ? C3 C2 C7 122.4(2) . . ? C1 C2 C7 116.3(2) . . ? C4 C3 C2 120.2(2) . . ? C3 C4 C5 117.4(2) . . ? O3 N2 O2 122.6(3) . . ? O3 N2 C5 119.0(3) . . ? O2 N2 C5 118.4(2) . . ? C4 C5 C6 123.1(3) . . ? C4 C5 N2 118.1(3) . . ? C6 C5 N2 118.8(3) . . ? C1 C6 C5 119.8(3) . . ? N1 C7 C2 111.2(2) . . ? N1 C7 C8 123.1(3) . . ? C2 C7 C8 125.7(3) . . ? P2 N3 P1 133.45(14) . . ? N3 P1 C31 115.30(11) . . ? N3 P1 C41 108.43(12) . . ? C31 P1 C41 107.68(11) . . ? N3 P1 C21 109.49(11) . . ? C31 P1 C21 106.72(12) . . ? C41 P1 C21 109.07(12) . . ? N3 P2 C71 107.24(12) . . ? N3 P2 C61 111.75(12) . . ? C71 P2 C61 108.29(12) . . ? N3 P2 C51 115.32(12) . . ? C71 P2 C51 105.72(12) . . ? C61 P2 C51 108.15(12) . . ? C22 C21 C26 119.6(2) . . ? C22 C21 P1 120.72(19) . . ? C26 C21 P1 119.69(18) . . ? C23 C22 C21 120.6(2) . . ? C22 C23 C24 119.4(3) . . ? C23 C24 C25 120.9(3) . . ? C26 C25 C24 119.8(3) . . ? C25 C26 C21 119.7(3) . . ? C36 C31 C32 119.8(2) . . ? C36 C31 P1 121.4(2) . . ? C32 C31 P1 118.39(17) . . ? C33 C32 C31 119.4(2) . . ? C32 C33 C34 120.5(3) . . ? C33 C34 C35 120.3(3) . . ? C34 C35 C36 120.0(2) . . ? C35 C36 C31 120.0(3) . . ? C46 C41 C42 119.6(2) . . ? C46 C41 P1 119.88(19) . . ? C42 C41 P1 120.5(2) . . ? C43 C42 C41 120.2(3) . . ? C42 C43 C44 120.3(3) . . ? C43 C44 C45 120.0(3) . . ? C46 C45 C44 120.0(3) . . ? C45 C46 C41 119.9(2) . . ? C52 C51 C56 119.8(2) . . ? C52 C51 P2 122.8(2) . . ? C56 C51 P2 117.07(19) . . ? C53 C52 C51 119.7(3) . . ? C54 C53 C52 120.7(3) . . ? C53 C54 C55 119.7(3) . . ? C56 C55 C54 120.4(3) . . ? C55 C56 C51 119.7(3) . . ? C62 C61 C66 119.2(2) . . ? C62 C61 P2 122.1(2) . . ? C66 C61 P2 118.62(19) . . ? C63 C62 C61 120.9(3) . . ? C62 C63 C64 119.6(3) . . ? C65 C64 C63 120.2(3) . . ? C64 C65 C66 120.2(3) . . ? C65 C66 C61 119.9(3) . . ? C76 C71 C72 119.8(2) . . ? C76 C71 P2 120.52(19) . . ? C72 C71 P2 119.6(2) . . ? C73 C72 C71 120.0(3) . . ? C74 C73 C72 119.9(3) . . ? C75 C74 C73 120.6(3) . . ? C74 C75 C76 119.8(3) . . ? C71 C76 C75 119.9(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H01 Cl2 0.825(18) 2.23(2) 3.023(2) 160(3) . C34 H34 Cl1 0.95 2.77 3.515(3) 136.1 . C35 H35 Cl2 0.95 2.78 3.704(3) 166.2 . _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.765 _refine_diff_density_min -0.670 _refine_diff_density_rms 0.077 # Attachment '- 3_aab241s.cif' data_aab241s _database_code_depnum_ccdc_archive 'CCDC 837028' #TrackingRef '- 3_aab241s.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H38 Cl2 N2 O P2 Pd' _chemical_formula_weight 850.00 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M 'P 2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.4042(4) _cell_length_b 13.5259(6) _cell_length_c 13.7681(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.603(2) _cell_angle_gamma 90.00 _cell_volume 1897.94(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8491 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 28.10 _exptl_crystal_description tablet _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 0.752 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8522 _exptl_absorpt_correction_T_max 0.9705 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22172 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 28.27 _reflns_number_total 8427 _reflns_number_gt 8112 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. OH free, rigid methyls, others riding ; _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^)+(0.0329P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.026(15) _refine_ls_number_reflns 8427 _refine_ls_number_parameters 474 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0673 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 0.769992(18) 0.487897(14) 0.906066(14) 0.01424(5) Uani 1 1 d . . . Cl1 Cl 0.70239(7) 0.64839(5) 0.89541(5) 0.02094(16) Uani 1 1 d . . . Cl2 Cl 0.92662(8) 0.50699(5) 0.79750(6) 0.02676(18) Uani 1 1 d . . . N1 N 0.8127(2) 0.34477(18) 0.92211(18) 0.0169(5) Uani 1 1 d . . . O1 O 0.9048(2) 0.29731(17) 0.87802(17) 0.0220(5) Uani 1 1 d . . . H01 H 0.929(3) 0.344(3) 0.853(3) 0.021(10) Uiso 1 1 d . . . C1 C 0.6465(3) 0.4491(2) 0.9913(2) 0.0145(6) Uani 1 1 d . . . C2 C 0.6521(3) 0.3465(2) 1.0137(2) 0.0157(6) Uani 1 1 d . . . C3 C 0.5660(3) 0.3042(2) 1.0682(2) 0.0186(6) Uani 1 1 d . . . H3 H 0.5699 0.2354 1.0820 0.022 Uiso 1 1 calc R . . C4 C 0.4751(3) 0.3633(2) 1.1020(2) 0.0193(6) Uani 1 1 d . . . H4 H 0.4150 0.3348 1.1376 0.023 Uiso 1 1 calc R . . C5 C 0.4725(3) 0.4641(2) 1.0836(2) 0.0212(7) Uani 1 1 d . . . H5 H 0.4125 0.5049 1.1088 0.025 Uiso 1 1 calc R . . C6 C 0.5572(3) 0.5062(2) 1.0285(2) 0.0171(6) Uani 1 1 d . . . H6 H 0.5534 0.5753 1.0163 0.020 Uiso 1 1 calc R . . C7 C 0.7500(3) 0.2896(2) 0.9742(2) 0.0171(6) Uani 1 1 d . . . C8 C 0.7754(3) 0.1819(2) 0.9862(2) 0.0238(7) Uani 1 1 d . . . H8A H 0.8674 0.1710 1.0178 0.036 Uiso 1 1 calc R . . H8B H 0.7570 0.1499 0.9211 0.036 Uiso 1 1 calc R . . H8C H 0.7185 0.1537 1.0278 0.036 Uiso 1 1 calc R . . P1 P -0.03483(7) 0.53970(5) 0.32364(5) 0.01256(14) Uani 1 1 d . . . N2 N 0.0857(2) 0.56929(18) 0.40848(18) 0.0160(5) Uani 1 1 d . . . P2 P 0.23343(7) 0.53319(6) 0.43942(5) 0.01347(15) Uani 1 1 d . . . C11 C -0.1509(2) 0.4699(2) 0.3778(2) 0.0150(6) Uani 1 1 d . . . C12 C -0.1359(3) 0.46570(19) 0.4811(2) 0.0168(6) Uani 1 1 d . . . H12 H -0.0675 0.5017 0.5222 0.020 Uiso 1 1 calc R . . C13 C -0.2217(3) 0.4084(2) 0.5234(2) 0.0221(7) Uani 1 1 d . . . H13 H -0.2128 0.4062 0.5934 0.026 Uiso 1 1 calc R . . C14 C -0.3197(3) 0.3549(2) 0.4631(2) 0.0231(7) Uani 1 1 d . . . H14 H -0.3762 0.3142 0.4921 0.028 Uiso 1 1 calc R . . C15 C -0.3360(3) 0.3602(2) 0.3617(2) 0.0218(7) Uani 1 1 d . . . H15 H -0.4048 0.3240 0.3213 0.026 Uiso 1 1 calc R . . C16 C -0.2532(3) 0.4178(2) 0.3176(2) 0.0181(6) Uani 1 1 d . . . H16 H -0.2658 0.4218 0.2475 0.022 Uiso 1 1 calc R . . C21 C -0.1101(3) 0.6525(2) 0.2698(2) 0.0137(6) Uani 1 1 d . . . C22 C -0.0749(3) 0.7424(2) 0.3177(2) 0.0163(6) Uani 1 1 d . . . H22 H -0.0135 0.7438 0.3789 0.020 Uiso 1 1 calc R . . C23 C -0.1294(3) 0.8290(2) 0.2762(2) 0.0211(6) Uani 1 1 d . . . H23 H -0.1062 0.8901 0.3092 0.025 Uiso 1 1 calc R . . C24 C -0.2181(3) 0.8276(2) 0.1860(2) 0.0236(7) Uani 1 1 d . . . H24 H -0.2545 0.8876 0.1569 0.028 Uiso 1 1 calc R . . C25 C -0.2533(3) 0.7386(2) 0.1389(2) 0.0229(7) Uani 1 1 d . . . H25 H -0.3149 0.7376 0.0777 0.027 Uiso 1 1 calc R . . C26 C -0.1995(3) 0.6511(2) 0.1800(2) 0.0184(6) Uani 1 1 d . . . H26 H -0.2235 0.5902 0.1470 0.022 Uiso 1 1 calc R . . C31 C 0.0037(3) 0.46532(19) 0.22521(19) 0.0142(6) Uani 1 1 d . . . C32 C 0.0037(3) 0.3618(2) 0.2319(2) 0.0165(6) Uani 1 1 d . . . H32 H -0.0274 0.3305 0.2844 0.020 Uiso 1 1 calc R . . C33 C 0.0492(3) 0.3054(2) 0.1622(2) 0.0185(6) Uani 1 1 d . . . H33 H 0.0517 0.2354 0.1680 0.022 Uiso 1 1 calc R . . C34 C 0.0909(3) 0.3508(2) 0.0837(2) 0.0189(6) Uani 1 1 d . . . H34 H 0.1211 0.3117 0.0355 0.023 Uiso 1 1 calc R . . C35 C 0.0888(3) 0.4532(2) 0.0754(2) 0.0222(7) Uani 1 1 d . . . H35 H 0.1169 0.4839 0.0212 0.027 Uiso 1 1 calc R . . C36 C 0.0458(3) 0.5109(2) 0.1459(2) 0.0179(7) Uani 1 1 d . . . H36 H 0.0450 0.5809 0.1403 0.022 Uiso 1 1 calc R . . C41 C 0.3409(3) 0.6071(2) 0.3816(2) 0.0163(6) Uani 1 1 d . . . C42 C 0.4752(3) 0.5879(2) 0.3959(3) 0.0262(7) Uani 1 1 d . . . H42 H 0.5113 0.5320 0.4336 0.031 Uiso 1 1 calc R . . C43 C 0.5554(3) 0.6498(3) 0.3553(3) 0.0320(8) Uani 1 1 d . . . H43 H 0.6464 0.6354 0.3638 0.038 Uiso 1 1 calc R . . C44 C 0.5048(3) 0.7327(3) 0.3024(2) 0.0283(7) Uani 1 1 d . . . H44 H 0.5613 0.7759 0.2762 0.034 Uiso 1 1 calc R . . C45 C 0.3716(3) 0.7526(3) 0.2877(2) 0.0248(7) Uani 1 1 d . . . H45 H 0.3364 0.8094 0.2513 0.030 Uiso 1 1 calc R . . C46 C 0.2899(3) 0.6890(2) 0.3264(2) 0.0177(6) Uani 1 1 d . . . H46 H 0.1983 0.7018 0.3150 0.021 Uiso 1 1 calc R . . C51 C 0.2575(3) 0.4039(2) 0.4171(2) 0.0151(6) Uani 1 1 d . . . C52 C 0.1937(3) 0.3372(2) 0.4696(2) 0.0223(7) Uani 1 1 d . . . H52 H 0.1479 0.3608 0.5181 0.027 Uiso 1 1 calc R . . C53 C 0.1975(3) 0.2373(2) 0.4507(2) 0.0266(7) Uani 1 1 d . . . H53 H 0.1541 0.1922 0.4862 0.032 Uiso 1 1 calc R . . C54 C 0.2644(3) 0.2020(2) 0.3801(2) 0.0235(7) Uani 1 1 d . . . H54 H 0.2657 0.1332 0.3666 0.028 Uiso 1 1 calc R . . C55 C 0.3290(3) 0.2674(2) 0.3297(2) 0.0188(7) Uani 1 1 d . . . H55 H 0.3776 0.2432 0.2832 0.023 Uiso 1 1 calc R . . C56 C 0.3234(3) 0.3688(2) 0.3465(2) 0.0166(6) Uani 1 1 d . . . H56 H 0.3649 0.4136 0.3095 0.020 Uiso 1 1 calc R . . C61 C 0.2840(3) 0.5483(2) 0.5715(2) 0.0172(6) Uani 1 1 d . . . C62 C 0.2067(3) 0.6008(2) 0.6246(2) 0.0211(6) Uani 1 1 d . . . H62 H 0.1270 0.6303 0.5914 0.025 Uiso 1 1 calc R . . C63 C 0.2464(4) 0.6101(3) 0.7266(2) 0.0283(8) Uani 1 1 d . . . H63 H 0.1927 0.6443 0.7637 0.034 Uiso 1 1 calc R . . C64 C 0.3643(4) 0.5695(2) 0.7740(2) 0.0289(8) Uani 1 1 d . . . H64 H 0.3924 0.5777 0.8436 0.035 Uiso 1 1 calc R . . C65 C 0.4411(3) 0.5175(2) 0.7220(2) 0.0307(8) Uani 1 1 d . . . H65 H 0.5215 0.4893 0.7555 0.037 Uiso 1 1 calc R . . C66 C 0.4014(3) 0.5063(3) 0.6210(2) 0.0282(8) Uani 1 1 d . . . H66 H 0.4542 0.4699 0.5849 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01498(10) 0.01327(10) 0.01481(10) 0.00126(9) 0.00381(7) -0.00061(9) Cl1 0.0261(4) 0.0144(3) 0.0247(4) 0.0042(3) 0.0106(3) 0.0003(3) Cl2 0.0305(4) 0.0237(5) 0.0316(4) 0.0061(3) 0.0193(3) 0.0041(3) N1 0.0160(12) 0.0164(13) 0.0181(12) -0.0024(10) 0.0031(10) 0.0025(10) O1 0.0262(12) 0.0174(12) 0.0247(12) 0.0017(9) 0.0108(10) 0.0025(9) C1 0.0119(13) 0.0174(13) 0.0128(13) 0.0019(11) -0.0009(11) -0.0035(10) C2 0.0173(15) 0.0150(14) 0.0130(14) -0.0008(11) -0.0013(11) -0.0016(11) C3 0.0221(16) 0.0152(14) 0.0179(15) 0.0020(11) 0.0026(12) -0.0032(12) C4 0.0201(15) 0.0194(15) 0.0192(15) 0.0034(12) 0.0057(12) -0.0047(12) C5 0.0159(14) 0.028(2) 0.0207(14) -0.0016(12) 0.0051(12) 0.0010(12) C6 0.0174(13) 0.0134(17) 0.0185(13) 0.0012(11) -0.0009(11) -0.0006(11) C7 0.0173(15) 0.0177(15) 0.0147(14) -0.0013(11) -0.0005(12) -0.0004(11) C8 0.0320(18) 0.0161(15) 0.0246(16) -0.0006(12) 0.0086(14) 0.0020(13) P1 0.0117(3) 0.0133(3) 0.0129(3) -0.0015(3) 0.0031(3) -0.0005(3) N2 0.0152(13) 0.0175(12) 0.0164(12) -0.0019(10) 0.0053(10) -0.0018(9) P2 0.0114(4) 0.0155(3) 0.0133(4) -0.0020(3) 0.0019(3) -0.0010(3) C11 0.0126(12) 0.0134(16) 0.0200(13) 0.0017(10) 0.0053(10) 0.0013(10) C12 0.0164(14) 0.0147(17) 0.0197(14) 0.0008(11) 0.0044(11) 0.0014(10) C13 0.0202(16) 0.0243(16) 0.0235(16) 0.0053(13) 0.0087(13) 0.0029(13) C14 0.0180(16) 0.0214(16) 0.0324(18) 0.0067(13) 0.0107(14) 0.0015(12) C15 0.0149(15) 0.0152(15) 0.0355(19) 0.0007(13) 0.0053(13) -0.0017(12) C16 0.0142(14) 0.0208(15) 0.0198(15) 0.0000(12) 0.0047(12) 0.0007(12) C21 0.0114(13) 0.0137(13) 0.0177(14) 0.0004(11) 0.0072(11) -0.0013(11) C22 0.0163(14) 0.0183(15) 0.0161(14) -0.0027(11) 0.0077(12) -0.0024(11) C23 0.0266(17) 0.0160(15) 0.0259(16) -0.0026(12) 0.0174(13) -0.0019(12) C24 0.0277(17) 0.0221(16) 0.0251(16) 0.0080(13) 0.0151(14) 0.0095(13) C25 0.0218(16) 0.0301(17) 0.0175(15) 0.0026(13) 0.0056(13) 0.0067(13) C26 0.0179(15) 0.0176(15) 0.0195(15) -0.0009(12) 0.0032(12) 0.0004(12) C31 0.0092(12) 0.0196(17) 0.0130(13) -0.0041(10) 0.0007(10) -0.0001(10) C32 0.0117(14) 0.0212(15) 0.0155(14) -0.0012(11) 0.0001(11) -0.0004(11) C33 0.0158(14) 0.0144(14) 0.0235(16) -0.0075(12) -0.0002(12) 0.0000(11) C34 0.0146(14) 0.0225(16) 0.0186(15) -0.0053(12) 0.0006(12) 0.0027(12) C35 0.0201(15) 0.0271(17) 0.0205(15) -0.0019(12) 0.0070(13) 0.0001(12) C36 0.0154(14) 0.0175(18) 0.0207(14) -0.0023(11) 0.0031(11) -0.0005(11) C41 0.0144(15) 0.0180(15) 0.0157(15) -0.0066(12) 0.0010(12) -0.0031(12) C42 0.0196(16) 0.0198(16) 0.039(2) 0.0020(14) 0.0060(15) 0.0024(13) C43 0.0154(16) 0.0288(18) 0.055(2) -0.0063(17) 0.0153(16) -0.0032(14) C44 0.0296(18) 0.0302(18) 0.0290(18) -0.0042(15) 0.0157(15) -0.0121(15) C45 0.0278(18) 0.0285(18) 0.0182(16) 0.0041(13) 0.0045(14) -0.0048(14) C46 0.0103(14) 0.0286(17) 0.0144(15) 0.0010(12) 0.0030(12) -0.0030(12) C51 0.0131(14) 0.0149(15) 0.0156(14) -0.0008(11) -0.0011(11) 0.0027(11) C52 0.0269(17) 0.0221(16) 0.0197(15) -0.0004(13) 0.0089(13) 0.0023(13) C53 0.0345(19) 0.0198(16) 0.0275(17) 0.0049(14) 0.0109(15) -0.0014(14) C54 0.0269(17) 0.0184(16) 0.0244(16) -0.0004(12) 0.0034(14) 0.0019(13) C55 0.0155(16) 0.0225(17) 0.0176(16) -0.0065(12) 0.0011(12) 0.0021(12) C56 0.0115(14) 0.0233(16) 0.0145(15) 0.0002(12) 0.0020(12) -0.0018(12) C61 0.0187(15) 0.0174(16) 0.0143(14) -0.0034(11) 0.0005(12) -0.0052(12) C62 0.0236(16) 0.0187(16) 0.0208(15) -0.0018(12) 0.0042(13) -0.0012(13) C63 0.042(2) 0.0264(17) 0.0173(16) -0.0062(13) 0.0073(15) -0.0008(15) C64 0.045(2) 0.0218(16) 0.0148(15) -0.0012(13) -0.0060(15) -0.0055(14) C65 0.0354(19) 0.0248(19) 0.0249(17) -0.0036(13) -0.0104(14) 0.0022(14) C66 0.0262(17) 0.032(2) 0.0237(15) -0.0064(13) -0.0021(13) 0.0062(14) _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 C1 1.977(3) . ? Pd1 N1 1.989(2) . ? Pd1 Cl1 2.2775(7) . ? Pd1 Cl2 2.4364(7) . ? N1 C7 1.298(4) . ? N1 O1 1.391(3) . ? C1 C6 1.384(4) . ? C1 C2 1.420(4) . ? C2 C3 1.401(4) . ? C2 C7 1.466(4) . ? C3 C4 1.388(4) . ? C4 C5 1.385(4) . ? C5 C6 1.395(4) . ? C7 C8 1.484(4) . ? P1 N2 1.584(3) . ? P1 C31 1.797(3) . ? P1 C21 1.805(3) . ? P1 C11 1.807(3) . ? N2 P2 1.587(3) . ? P2 C61 1.800(3) . ? P2 C41 1.800(3) . ? P2 C51 1.801(3) . ? C11 C16 1.400(4) . ? C11 C12 1.401(4) . ? C12 C13 1.395(4) . ? C13 C14 1.383(4) . ? C14 C15 1.374(4) . ? C15 C16 1.388(4) . ? C21 C26 1.390(4) . ? C21 C22 1.397(4) . ? C22 C23 1.375(4) . ? C23 C24 1.390(5) . ? C24 C25 1.381(5) . ? C25 C26 1.381(4) . ? C31 C36 1.399(4) . ? C31 C32 1.403(4) . ? C32 C33 1.382(4) . ? C33 C34 1.386(4) . ? C34 C35 1.391(4) . ? C35 C36 1.387(4) . ? C41 C46 1.387(4) . ? C41 C42 1.396(4) . ? C42 C43 1.377(5) . ? C43 C44 1.382(5) . ? C44 C45 1.386(5) . ? C45 C46 1.388(4) . ? C51 C56 1.382(4) . ? C51 C52 1.404(4) . ? C52 C53 1.378(5) . ? C53 C54 1.389(4) . ? C54 C55 1.379(4) . ? C55 C56 1.394(4) . ? C61 C62 1.388(4) . ? C61 C66 1.394(4) . ? C62 C63 1.387(4) . ? C63 C64 1.382(5) . ? C64 C65 1.369(5) . ? C65 C66 1.378(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 C1 Pd1 N1 80.37(11) . . ? C1 Pd1 Cl1 93.57(9) . . ? N1 Pd1 Cl1 173.86(7) . . ? C1 Pd1 Cl2 170.68(9) . . ? N1 Pd1 Cl2 90.53(7) . . ? Cl1 Pd1 Cl2 95.48(3) . . ? C7 N1 O1 116.3(2) . . ? C7 N1 Pd1 119.7(2) . . ? O1 N1 Pd1 124.00(18) . . ? C6 C1 C2 117.8(3) . . ? C6 C1 Pd1 129.5(2) . . ? C2 C1 Pd1 112.7(2) . . ? C3 C2 C1 120.8(3) . . ? C3 C2 C7 123.5(3) . . ? C1 C2 C7 115.7(3) . . ? C4 C3 C2 119.8(3) . . ? C5 C4 C3 119.7(3) . . ? C4 C5 C6 120.7(3) . . ? C1 C6 C5 121.2(3) . . ? N1 C7 C2 111.5(3) . . ? N1 C7 C8 121.9(3) . . ? C2 C7 C8 126.5(3) . . ? N2 P1 C31 115.74(13) . . ? N2 P1 C21 107.65(13) . . ? C31 P1 C21 107.92(13) . . ? N2 P1 C11 108.88(13) . . ? C31 P1 C11 106.72(12) . . ? C21 P1 C11 109.87(12) . . ? P1 N2 P2 134.48(16) . . ? N2 P2 C61 107.88(13) . . ? N2 P2 C41 111.38(14) . . ? C61 P2 C41 107.59(14) . . ? N2 P2 C51 114.41(13) . . ? C61 P2 C51 105.07(13) . . ? C41 P2 C51 110.09(14) . . ? C16 C11 C12 119.7(2) . . ? C16 C11 P1 120.7(2) . . ? C12 C11 P1 119.5(2) . . ? C13 C12 C11 119.8(3) . . ? C14 C13 C12 119.8(3) . . ? C15 C14 C13 120.5(3) . . ? C14 C15 C16 120.9(3) . . ? C15 C16 C11 119.2(3) . . ? C26 C21 C22 119.8(3) . . ? C26 C21 P1 120.8(2) . . ? C22 C21 P1 119.4(2) . . ? C23 C22 C21 119.9(3) . . ? C22 C23 C24 120.2(3) . . ? C25 C24 C23 119.9(3) . . ? C26 C25 C24 120.4(3) . . ? C25 C26 C21 119.8(3) . . ? C36 C31 C32 119.6(2) . . ? C36 C31 P1 119.7(2) . . ? C32 C31 P1 120.4(2) . . ? C33 C32 C31 120.1(3) . . ? C32 C33 C34 120.1(3) . . ? C33 C34 C35 120.2(3) . . ? C36 C35 C34 120.3(3) . . ? C35 C36 C31 119.6(3) . . ? C46 C41 C42 119.2(3) . . ? C46 C41 P2 118.9(2) . . ? C42 C41 P2 121.8(2) . . ? C43 C42 C41 120.1(3) . . ? C42 C43 C44 120.6(3) . . ? C43 C44 C45 119.9(3) . . ? C44 C45 C46 119.7(3) . . ? C41 C46 C45 120.6(3) . . ? C56 C51 C52 119.6(3) . . ? C56 C51 P2 124.0(2) . . ? C52 C51 P2 116.1(2) . . ? C53 C52 C51 119.9(3) . . ? C52 C53 C54 120.4(3) . . ? C55 C54 C53 119.7(3) . . ? C54 C55 C56 120.4(3) . . ? C51 C56 C55 119.9(3) . . ? C62 C61 C66 119.6(3) . . ? C62 C61 P2 120.5(2) . . ? C66 C61 P2 119.8(2) . . ? C63 C62 C61 119.6(3) . . ? C64 C63 C62 119.9(3) . . ? C65 C64 C63 120.9(3) . . ? C64 C65 C66 119.7(3) . . ? C65 C66 C61 120.3(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H01 Cl2 0.78(4) 2.33(4) 3.070(2) 157(3) . _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.715 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.076 # Attachment '- 6b_aab731s.cif' data_aab731s _database_code_depnum_ccdc_archive 'CCDC 837029' #TrackingRef '- 6b_aab731s.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H22 N4 O3 Pd' _chemical_formula_weight 400.76 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 monoclinic _symmetry_space_group_name_H-M 'P 2(1)/n' 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 8.4822(8) _cell_length_b 11.5612(11) _cell_length_c 15.6484(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.517(2) _cell_angle_gamma 90.00 _cell_volume 1534.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5408 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.72 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 1.228 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8100 _exptl_absorpt_correction_T_max 0.9190 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18671 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0187 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.72 _reflns_number_total 3762 _reflns_number_gt 3587 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0189P)^2^+1.7854P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3762 _refine_ls_number_parameters 204 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0248 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0526 _refine_ls_wR_factor_gt 0.0518 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _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 0.043687(15) 0.546728(11) 0.796365(8) 0.01030(5) Uani 1 1 d . . . N1 N -0.05323(18) 0.69015(14) 0.84761(10) 0.0129(3) Uani 1 1 d . . . N2 N -0.08509(19) 0.55128(13) 0.67522(10) 0.0132(3) Uani 1 1 d . . . O1 O -0.15263(16) 0.75495(12) 0.80566(9) 0.0164(3) Uani 1 1 d . . . N3 N 0.16715(18) 0.40900(14) 0.73548(10) 0.0134(3) Uani 1 1 d . . . C1 C 0.1490(2) 0.54319(16) 0.91176(12) 0.0124(3) Uani 1 1 d . . . C2 C 0.1082(2) 0.64039(16) 0.96261(11) 0.0126(3) Uani 1 1 d . . . C3 C 0.1685(2) 0.65362(17) 1.04565(12) 0.0150(4) Uani 1 1 d . . . H3 H 0.1417 0.7204 1.0778 0.018 Uiso 1 1 calc R . . C4 C 0.2666(2) 0.57062(17) 1.08158(12) 0.0153(4) Uani 1 1 d . . . H4 H 0.3084 0.5794 1.1377 0.018 Uiso 1 1 calc R . . C5 C 0.3014(2) 0.47478(16) 1.03272(12) 0.0133(4) Uani 1 1 d . . . N4 N 0.40032(19) 0.38382(14) 1.07005(10) 0.0151(3) Uani 1 1 d . . . O2 O 0.45846(17) 0.39948(13) 1.14123(9) 0.0207(3) Uani 1 1 d . . . O3 O 0.42188(18) 0.29445(12) 1.02847(9) 0.0213(3) Uani 1 1 d . . . C6 C 0.2442(2) 0.45999(16) 0.94956(12) 0.0137(4) Uani 1 1 d . . . H6 H 0.2707 0.3922 0.9186 0.016 Uiso 1 1 calc R . . C7 C -0.0015(2) 0.72150(16) 0.92397(12) 0.0133(3) Uani 1 1 d . . . C8 C -0.0587(2) 0.82981(17) 0.96544(13) 0.0183(4) Uani 1 1 d . . . H8A H -0.0723 0.8902 0.9221 0.027 Uiso 1 1 calc R . . H8B H 0.0185 0.8554 1.0084 0.027 Uiso 1 1 calc R . . H8C H -0.1599 0.8149 0.9931 0.027 Uiso 1 1 calc R . . C9 C 0.1259(2) 0.41445(17) 0.64232(12) 0.0160(4) Uani 1 1 d . . . H9A H 0.1501 0.3394 0.6150 0.019 Uiso 1 1 calc R . . H9B H 0.1900 0.4749 0.6143 0.019 Uiso 1 1 calc R . . C10 C -0.0468(2) 0.44168(16) 0.63062(12) 0.0150(4) Uani 1 1 d . . . H10A H -0.0720 0.4492 0.5690 0.018 Uiso 1 1 calc R . . H10B H -0.1112 0.3779 0.6541 0.018 Uiso 1 1 calc R . . C11 C 0.3412(2) 0.42347(18) 0.74250(13) 0.0182(4) Uani 1 1 d . . . H11A H 0.3739 0.4165 0.8025 0.027 Uiso 1 1 calc R . . H11B H 0.3709 0.4999 0.7209 0.027 Uiso 1 1 calc R . . H11C H 0.3935 0.3635 0.7087 0.027 Uiso 1 1 calc R . . C12 C 0.1224(2) 0.29343(17) 0.76876(13) 0.0189(4) Uani 1 1 d . . . H12A H 0.1853 0.2338 0.7405 0.028 Uiso 1 1 calc R . . H12B H 0.0102 0.2796 0.7573 0.028 Uiso 1 1 calc R . . H12C H 0.1423 0.2906 0.8305 0.028 Uiso 1 1 calc R . . C13 C -0.0309(2) 0.65266(17) 0.62565(13) 0.0180(4) Uani 1 1 d . . . H13A H 0.0832 0.6474 0.6171 0.027 Uiso 1 1 calc R . . H13B H -0.0552 0.7237 0.6570 0.027 Uiso 1 1 calc R . . H13C H -0.0848 0.6540 0.5700 0.027 Uiso 1 1 calc R . . C14 C -0.2581(2) 0.55969(17) 0.68494(12) 0.0163(4) Uani 1 1 d . . . H14A H -0.2836 0.6280 0.7192 0.024 Uiso 1 1 calc R . . H14B H -0.2972 0.4901 0.7136 0.024 Uiso 1 1 calc R . . H14C H -0.3080 0.5665 0.6284 0.024 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 0.01088(7) 0.00931(7) 0.01069(7) -0.00064(5) -0.00088(5) 0.00006(5) N1 0.0113(7) 0.0117(7) 0.0157(7) 0.0010(6) 0.0004(6) -0.0003(6) N2 0.0133(7) 0.0113(7) 0.0150(7) 0.0005(6) -0.0003(6) -0.0008(6) O1 0.0158(6) 0.0139(6) 0.0194(7) 0.0002(5) -0.0038(5) 0.0036(5) N3 0.0137(7) 0.0127(7) 0.0139(7) -0.0016(6) -0.0021(6) 0.0008(6) C1 0.0122(8) 0.0123(8) 0.0126(8) 0.0001(7) -0.0005(6) -0.0037(7) C2 0.0114(8) 0.0119(8) 0.0144(8) 0.0008(7) 0.0018(6) -0.0031(7) C3 0.0155(9) 0.0140(9) 0.0157(9) -0.0031(7) 0.0019(7) -0.0017(7) C4 0.0165(9) 0.0161(9) 0.0134(9) -0.0012(7) -0.0010(7) -0.0039(7) C5 0.0115(8) 0.0142(9) 0.0142(9) 0.0037(7) -0.0001(7) -0.0015(7) N4 0.0137(7) 0.0162(8) 0.0153(8) 0.0042(6) 0.0003(6) -0.0011(6) O2 0.0224(7) 0.0229(7) 0.0166(7) 0.0034(6) -0.0062(6) 0.0006(6) O3 0.0275(8) 0.0162(7) 0.0202(7) -0.0009(6) -0.0017(6) 0.0064(6) C6 0.0146(9) 0.0115(8) 0.0150(9) -0.0017(7) 0.0007(7) -0.0009(7) C7 0.0125(8) 0.0120(8) 0.0155(8) -0.0008(7) 0.0011(7) -0.0015(7) C8 0.0210(10) 0.0159(9) 0.0179(9) -0.0029(7) -0.0022(7) 0.0038(8) C9 0.0178(9) 0.0171(9) 0.0131(9) -0.0029(7) -0.0012(7) 0.0012(7) C10 0.0184(9) 0.0138(9) 0.0128(8) -0.0015(7) -0.0020(7) 0.0004(7) C11 0.0135(9) 0.0230(10) 0.0179(9) -0.0044(8) -0.0009(7) 0.0020(8) C12 0.0254(10) 0.0127(9) 0.0186(9) -0.0002(7) -0.0031(8) -0.0008(8) C13 0.0208(9) 0.0157(9) 0.0176(9) 0.0033(7) -0.0006(7) -0.0031(8) C14 0.0127(8) 0.0191(9) 0.0169(9) -0.0009(7) -0.0013(7) 0.0007(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.0078(18) . ? Pd1 N1 2.0199(16) . ? Pd1 N3 2.1349(16) . ? Pd1 N2 2.1800(16) . ? N1 O1 1.301(2) . ? N1 C7 1.320(2) . ? N2 C14 1.480(2) . ? N2 C13 1.481(2) . ? N2 C10 1.484(2) . ? N3 C12 1.485(2) . ? N3 C11 1.489(2) . ? N3 C9 1.498(2) . ? C1 C6 1.385(3) . ? C1 C2 1.421(3) . ? C2 C3 1.400(3) . ? C2 C7 1.449(3) . ? C3 C4 1.386(3) . ? C4 C5 1.380(3) . ? C5 C6 1.395(3) . ? C5 N4 1.464(2) . ? N4 O2 1.227(2) . ? N4 O3 1.235(2) . ? C7 C8 1.493(3) . ? C9 C10 1.508(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 C1 Pd1 N1 80.74(7) . . ? C1 Pd1 N3 99.79(7) . . ? N1 Pd1 N3 172.95(6) . . ? C1 Pd1 N2 176.34(7) . . ? N1 Pd1 N2 97.06(6) . . ? N3 Pd1 N2 82.76(6) . . ? O1 N1 C7 120.48(16) . . ? O1 N1 Pd1 122.44(12) . . ? C7 N1 Pd1 116.85(13) . . ? C14 N2 C13 108.34(15) . . ? C14 N2 C10 109.00(15) . . ? C13 N2 C10 111.06(15) . . ? C14 N2 Pd1 113.69(12) . . ? C13 N2 Pd1 108.61(11) . . ? C10 N2 Pd1 106.17(11) . . ? C12 N3 C11 109.37(15) . . ? C12 N3 C9 108.73(15) . . ? C11 N3 C9 106.86(14) . . ? C12 N3 Pd1 112.75(12) . . ? C11 N3 Pd1 111.92(12) . . ? C9 N3 Pd1 106.96(11) . . ? C6 C1 C2 116.99(17) . . ? C6 C1 Pd1 130.63(14) . . ? C2 C1 Pd1 112.26(13) . . ? C3 C2 C1 121.14(17) . . ? C3 C2 C7 122.95(17) . . ? C1 C2 C7 115.88(16) . . ? C4 C3 C2 120.90(17) . . ? C5 C4 C3 117.51(17) . . ? C4 C5 C6 122.74(18) . . ? C4 C5 N4 118.73(17) . . ? C6 C5 N4 118.53(17) . . ? O2 N4 O3 122.76(16) . . ? O2 N4 C5 118.70(16) . . ? O3 N4 C5 118.54(16) . . ? C1 C6 C5 120.66(17) . . ? N1 C7 C2 114.01(16) . . ? N1 C7 C8 121.12(17) . . ? C2 C7 C8 124.83(17) . . ? N3 C9 C10 110.20(15) . . ? N2 C10 C9 109.72(15) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C10 H10B O1 0.99 2.54 3.493(2) 161.3 2_446 C14 H14B O1 0.98 2.77 3.607(2) 144.0 2_446 C11 H11C O1 0.98 2.54 3.373(2) 142.4 2_546 C11 H11C N1 0.98 2.58 3.542(3) 167.3 2_546 _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.513 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.078