# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Ming-Hua Xie' 'Xiu-Li Yang' 'Chuan-De Wu' _publ_contact_author_name 'Wu, Chuan-De' _publ_contact_author_email cdwu@zju.edu.cn data_New1 _database_code_depnum_ccdc_archive 'CCDC 715005' #TrackingRef 'New1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H41.50 Cd1.25 N6 O11 Pd' _chemical_formula_weight 1197.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/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 7.29530(10) _cell_length_b 25.5761(7) _cell_length_c 30.7597(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.361(2) _cell_angle_gamma 90.00 _cell_volume 5704.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15512 _cell_measurement_theta_min 3.46 _cell_measurement_theta_max 58.91 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2406 _exptl_absorpt_coefficient_mu 6.756 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.290 _exptl_absorpt_correction_T_max 0.713 _exptl_absorpt_process_details CrysAlisPro _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15512 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 58.91 _reflns_number_total 4054 _reflns_number_gt 3395 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'CrystalStructure and PLATON (Spek, 2001)' _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.111 0.250 0.000 364 56 ' ' 2 0.048 0.750 0.000 364 56 ' ' 3 -0.017 0.579 0.250 242 36 ' ' 4 -0.017 0.079 0.250 242 36 ' ' 5 -0.085 0.750 0.500 363 56 ' ' 6 0.090 0.250 0.501 363 56 ' ' 7 -0.016 0.422 0.750 242 36 ' ' 8 -0.018 0.922 0.750 242 36 ' ' _platon_squeeze_details ; ; _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^)+(0.0867P)^2^+21.1888P] 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 4054 _refine_ls_number_parameters 284 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0776 _refine_ls_wR_factor_ref 0.1904 _refine_ls_wR_factor_gt 0.1837 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.5000 0.34476(3) 0.2500 0.0995(3) Uani 1 2 d S . . Cd2 Cd 1.0000 0.2909(2) 0.2500 0.1441(16) Uani 0.25 2 d SPD . . Pd1 Pd 1.5000 0.5000 0.0000 0.0954(3) Uani 1 2 d S . . O1 O 0.7851(8) 0.3686(3) 0.22808(18) 0.1140(17) Uani 1 1 d . . . O2 O 0.5485(9) 0.4081(3) 0.1943(2) 0.142(3) Uani 1 1 d . . . O3 O 0.913(4) 0.2360(7) -0.2022(6) 0.357(18) Uani 1 1 d D . . O4 O 1.197(4) 0.2027(5) -0.1961(4) 0.366(17) Uani 1 1 d D . . O5 O 0.991(5) 0.2418(15) 0.3074(9) 0.303(15) Uani 0.25 1 d PD . . N1 N 1.4447(9) 0.5295(3) 0.05850(19) 0.0964(17) Uani 1 1 d . . . N2 N 1.2867(9) 0.4502(3) -0.0003(2) 0.0998(17) Uani 1 1 d . . . C1 C 1.5364(13) 0.5692(4) 0.0816(3) 0.101(2) Uani 1 1 d . . . C2 C 1.4591(16) 0.5756(5) 0.1223(3) 0.127(3) Uani 1 1 d . . . H2A H 1.4974 0.5994 0.1443 0.153 Uiso 1 1 calc R . . C3 C 1.3246(14) 0.5417(5) 0.1224(3) 0.123(3) Uani 1 1 d . . . H3A H 1.2499 0.5379 0.1448 0.147 Uiso 1 1 calc R . . C4 C 1.3093(12) 0.5114(4) 0.0832(3) 0.107(2) Uani 1 1 d . . . C5 C 1.1839(11) 0.4725(4) 0.0713(3) 0.103(2) Uani 1 1 d . . . C6 C 1.1709(12) 0.4447(4) 0.0320(3) 0.106(2) Uani 1 1 d . . . C7 C 1.0463(18) 0.4047(5) 0.0203(4) 0.149(4) Uani 1 1 d . . . H7A H 0.9528 0.3936 0.0364 0.179 Uiso 1 1 calc R . . C8 C 1.0835(18) 0.3845(5) -0.0182(4) 0.146(4) Uani 1 1 d . . . H8A H 1.0233 0.3568 -0.0333 0.175 Uiso 1 1 calc R . . C9 C 1.2316(14) 0.4137(4) -0.0309(3) 0.113(3) Uani 1 1 d . . . C10 C 1.3174(14) 0.4033(4) -0.0695(3) 0.110(2) Uani 1 1 d . . . C11 C 1.0624(11) 0.4553(4) 0.1050(3) 0.107(2) Uani 1 1 d . . . C12 C 1.1363(12) 0.4282(4) 0.1417(3) 0.121(3) Uani 1 1 d . . . H12A H 1.2621 0.4213 0.1458 0.145 Uiso 1 1 calc R . . C13 C 1.0252(12) 0.4116(4) 0.1719(3) 0.118(3) Uani 1 1 d . . . H13A H 1.0773 0.3939 0.1966 0.142 Uiso 1 1 calc R . . C14 C 0.8373(11) 0.4204(4) 0.1664(2) 0.102(2) Uani 1 1 d . . . C15 C 0.7642(12) 0.4481(4) 0.1305(3) 0.111(3) Uani 1 1 d . . . H15A H 0.6387 0.4556 0.1267 0.133 Uiso 1 1 calc R . . C16 C 0.8749(12) 0.4646(4) 0.1002(3) 0.116(3) Uani 1 1 d . . . H16A H 0.8225 0.4826 0.0756 0.139 Uiso 1 1 calc R . . C17 C 0.7153(12) 0.3975(4) 0.1987(3) 0.104(2) Uani 1 1 d . . . C18 C 1.2470(14) 0.3592(3) -0.0981(2) 0.137(4) Uani 1 1 d G . . C19 C 1.0731(13) 0.3619(3) -0.1216(3) 0.160(4) Uani 1 1 d G . . H19A H 0.9972 0.3905 -0.1181 0.191 Uiso 1 1 calc R . . C20 C 1.0126(14) 0.3218(5) -0.1502(3) 0.188(6) Uani 1 1 d G . . H20A H 0.8962 0.3236 -0.1659 0.225 Uiso 1 1 calc R . . C21 C 1.126(2) 0.2791(4) -0.1554(3) 0.236(11) Uani 1 1 d GD . . C22 C 1.300(2) 0.2765(3) -0.1319(4) 0.273(14) Uani 1 1 d G . . H22A H 1.3758 0.2479 -0.1354 0.328 Uiso 1 1 calc R . . C23 C 1.3604(15) 0.3165(4) -0.1033(3) 0.204(8) Uani 1 1 d G . . H23A H 1.4767 0.3147 -0.0876 0.245 Uiso 1 1 calc R . . C24 C 1.072(4) 0.2363(8) -0.1888(6) 0.244(13) Uani 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 Cd1 0.1069(6) 0.1207(6) 0.0743(5) 0.000 0.0249(4) 0.000 Cd2 0.142(3) 0.148(3) 0.154(4) 0.000 0.070(3) 0.000 Pd1 0.0987(6) 0.1158(7) 0.0744(5) 0.0031(4) 0.0222(4) 0.0111(4) O1 0.101(3) 0.158(5) 0.083(3) 0.019(3) 0.009(3) -0.010(3) O2 0.102(4) 0.206(7) 0.125(5) 0.051(5) 0.044(4) 0.026(4) O3 0.67(5) 0.211(16) 0.176(13) -0.030(11) -0.02(2) -0.20(2) O4 0.81(5) 0.149(9) 0.115(8) -0.027(7) -0.047(15) 0.047(18) O5 0.15(3) 0.30(4) 0.43(4) -0.04(3) -0.09(2) -0.03(2) N1 0.097(4) 0.120(5) 0.075(3) 0.005(3) 0.021(3) 0.016(3) N2 0.107(4) 0.125(5) 0.070(3) 0.002(3) 0.021(3) 0.005(4) C1 0.115(6) 0.116(6) 0.074(5) -0.017(4) 0.015(4) 0.011(5) C2 0.127(7) 0.164(9) 0.094(6) -0.026(6) 0.026(5) 0.007(7) C3 0.112(6) 0.177(9) 0.084(5) -0.017(6) 0.031(5) 0.014(7) C4 0.098(5) 0.152(7) 0.074(5) 0.004(5) 0.027(4) 0.016(5) C5 0.085(5) 0.149(7) 0.078(5) 0.010(5) 0.017(4) 0.007(5) C6 0.101(5) 0.136(7) 0.082(5) 0.004(5) 0.022(4) -0.010(5) C7 0.161(9) 0.197(11) 0.098(7) -0.002(7) 0.046(6) -0.049(9) C8 0.174(10) 0.164(9) 0.104(7) -0.010(6) 0.034(7) -0.045(8) C9 0.132(7) 0.121(6) 0.089(5) 0.003(5) 0.030(5) -0.017(5) C10 0.128(7) 0.121(6) 0.082(5) -0.007(5) 0.016(5) 0.000(5) C11 0.090(5) 0.156(7) 0.077(5) 0.013(5) 0.020(4) 0.010(5) C12 0.090(5) 0.185(9) 0.092(6) 0.021(6) 0.024(4) 0.021(5) C13 0.095(5) 0.179(9) 0.081(5) 0.025(5) 0.009(4) 0.014(5) C14 0.090(5) 0.146(7) 0.074(4) 0.007(4) 0.023(4) 0.013(4) C15 0.089(5) 0.147(7) 0.100(6) 0.020(5) 0.024(4) 0.021(5) C16 0.099(6) 0.162(8) 0.088(5) 0.027(5) 0.017(4) 0.021(5) C17 0.100(6) 0.137(7) 0.076(5) 0.002(5) 0.016(4) 0.005(5) C18 0.200(11) 0.129(8) 0.085(6) -0.003(5) 0.028(7) -0.011(8) C19 0.204(13) 0.151(10) 0.124(8) -0.014(8) 0.017(8) -0.043(9) C20 0.278(19) 0.156(11) 0.126(10) -0.015(9) 0.009(11) -0.064(12) C21 0.48(4) 0.124(10) 0.099(9) -0.014(8) 0.006(14) -0.059(16) C22 0.52(4) 0.178(15) 0.106(10) -0.047(10) -0.036(16) 0.11(2) C23 0.33(2) 0.148(11) 0.120(9) -0.025(8) -0.011(11) 0.057(13) C24 0.44(4) 0.19(2) 0.116(13) -0.008(12) 0.064(19) 0.06(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.337(5) . ? Cd1 O1 2.337(5) 2_655 ? Cd1 O4 2.402(16) 8_456 ? Cd1 O4 2.402(16) 7_655 ? Cd1 O2 2.414(7) 2_655 ? Cd1 O2 2.414(7) . ? Cd1 O3 2.65(2) 8_456 ? Cd1 O3 2.652(19) 7_655 ? Cd1 C17 2.708(9) . ? Cd1 C17 2.708(9) 2_655 ? Cd2 O5 2.174(10) . ? Cd2 O5 2.174(10) 2_755 ? Cd2 O1 2.574(8) . ? Cd2 O1 2.574(8) 2_755 ? Pd1 N2 2.011(7) 5_865 ? Pd1 N2 2.011(7) . ? Pd1 N1 2.032(6) . ? Pd1 N1 2.033(6) 5_865 ? O1 C17 1.235(10) . ? O2 C17 1.239(10) . ? O3 C24 1.188(10) . ? O3 Cd1 2.652(19) 7_655 ? O4 C24 1.292(10) . ? O4 Cd1 2.402(16) 7_655 ? N1 C1 1.370(11) . ? N1 C4 1.390(10) . ? N2 C9 1.354(11) . ? N2 C6 1.381(10) . ? C1 C10 1.364(13) 5_865 ? C1 C2 1.439(12) . ? C2 C3 1.310(14) . ? C3 C4 1.429(13) . ? C4 C5 1.374(13) . ? C5 C6 1.394(12) . ? C5 C11 1.503(11) . ? C6 C7 1.389(14) . ? C7 C8 1.346(15) . ? C8 C9 1.404(14) . ? C9 C10 1.426(12) . ? C10 C1 1.364(13) 5_865 ? C10 C18 1.487(11) . ? C11 C12 1.381(12) . ? C11 C16 1.380(11) . ? C12 C13 1.367(12) . ? C13 C14 1.381(11) . ? C14 C15 1.371(11) . ? C14 C17 1.521(12) . ? C15 C16 1.366(12) . ? C18 C19 1.3900 . ? C18 C23 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C21 C24 1.523(10) . ? C22 C23 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O1 149.8(4) . 2_655 ? O1 Cd1 O4 81.2(7) . 8_456 ? O1 Cd1 O4 114.6(6) 2_655 8_456 ? O1 Cd1 O4 114.6(6) . 7_655 ? O1 Cd1 O4 81.2(7) 2_655 7_655 ? O4 Cd1 O4 119.3(7) 8_456 7_655 ? O1 Cd1 O2 103.6(2) . 2_655 ? O1 Cd1 O2 54.2(2) 2_655 2_655 ? O4 Cd1 O2 88.4(4) 8_456 2_655 ? O4 Cd1 O2 134.9(6) 7_655 2_655 ? O1 Cd1 O2 54.2(2) . . ? O1 Cd1 O2 103.6(2) 2_655 . ? O4 Cd1 O2 134.9(6) 8_456 . ? O4 Cd1 O2 88.4(4) 7_655 . ? O2 Cd1 O2 95.6(4) 2_655 . ? O1 Cd1 O3 129.6(5) . 8_456 ? O1 Cd1 O3 76.6(5) 2_655 8_456 ? O4 Cd1 O3 52.1(4) 8_456 8_456 ? O4 Cd1 O3 80.1(6) 7_655 8_456 ? O2 Cd1 O3 93.8(5) 2_655 8_456 ? O2 Cd1 O3 168.4(5) . 8_456 ? O1 Cd1 O3 76.6(5) . 7_655 ? O1 Cd1 O3 129.6(5) 2_655 7_655 ? O4 Cd1 O3 80.1(6) 8_456 7_655 ? O4 Cd1 O3 52.1(4) 7_655 7_655 ? O2 Cd1 O3 168.4(5) 2_655 7_655 ? O2 Cd1 O3 93.8(5) . 7_655 ? O3 Cd1 O3 77.7(9) 8_456 7_655 ? O1 Cd1 C17 27.1(2) . . ? O1 Cd1 C17 129.1(3) 2_655 . ? O4 Cd1 C17 108.2(7) 8_456 . ? O4 Cd1 C17 101.0(5) 7_655 . ? O2 Cd1 C17 102.7(3) 2_655 . ? O2 Cd1 C17 27.2(2) . . ? O3 Cd1 C17 154.3(5) 8_456 . ? O3 Cd1 C17 82.8(5) 7_655 . ? O1 Cd1 C17 129.1(3) . 2_655 ? O1 Cd1 C17 27.1(2) 2_655 2_655 ? O4 Cd1 C17 101.0(5) 8_456 2_655 ? O4 Cd1 C17 108.2(7) 7_655 2_655 ? O2 Cd1 C17 27.2(2) 2_655 2_655 ? O2 Cd1 C17 102.7(3) . 2_655 ? O3 Cd1 C17 82.8(5) 8_456 2_655 ? O3 Cd1 C17 154.3(5) 7_655 2_655 ? C17 Cd1 C17 120.2(4) . 2_655 ? O5 Cd2 O5 109(2) . 2_755 ? O5 Cd2 O1 125.9(12) . . ? O5 Cd2 O1 107.7(10) 2_755 . ? O5 Cd2 O1 107.7(10) . 2_755 ? O5 Cd2 O1 125.9(12) 2_755 2_755 ? O1 Cd2 O1 79.0(3) . 2_755 ? N2 Pd1 N2 179.999(1) 5_865 . ? N2 Pd1 N1 89.4(3) 5_865 . ? N2 Pd1 N1 90.6(3) . . ? N2 Pd1 N1 90.6(3) 5_865 5_865 ? N2 Pd1 N1 89.4(3) . 5_865 ? N1 Pd1 N1 180.00(14) . 5_865 ? C17 O1 Cd1 93.4(5) . . ? C17 O1 Cd2 147.7(6) . . ? Cd1 O1 Cd2 105.0(2) . . ? C17 O2 Cd1 89.7(5) . . ? C24 O3 Cd1 85.0(12) . 7_655 ? C24 O4 Cd1 94.3(10) . 7_655 ? C1 N1 C4 107.5(7) . . ? C1 N1 Pd1 126.9(5) . . ? C4 N1 Pd1 125.6(6) . . ? C9 N2 C6 105.9(7) . . ? C9 N2 Pd1 127.5(5) . . ? C6 N2 Pd1 126.5(6) . . ? C10 C1 N1 126.4(7) 5_865 . ? C10 C1 C2 124.9(9) 5_865 . ? N1 C1 C2 108.7(9) . . ? C3 C2 C1 107.0(9) . . ? C2 C3 C4 110.2(8) . . ? C5 C4 N1 126.0(8) . . ? C5 C4 C3 127.3(8) . . ? N1 C4 C3 106.6(9) . . ? C4 C5 C6 125.4(7) . . ? C4 C5 C11 116.9(8) . . ? C6 C5 C11 117.4(8) . . ? N2 C6 C7 108.8(8) . . ? N2 C6 C5 125.7(8) . . ? C7 C6 C5 125.4(8) . . ? C8 C7 C6 108.7(9) . . ? C7 C8 C9 106.2(10) . . ? N2 C9 C8 110.5(8) . . ? N2 C9 C10 125.7(8) . . ? C8 C9 C10 123.7(9) . . ? C1 C10 C9 124.0(8) 5_865 . ? C1 C10 C18 117.3(8) 5_865 . ? C9 C10 C18 118.7(9) . . ? C12 C11 C16 117.8(7) . . ? C12 C11 C5 120.2(7) . . ? C16 C11 C5 121.9(7) . . ? C13 C12 C11 120.3(8) . . ? C12 C13 C14 121.5(8) . . ? C15 C14 C13 118.3(7) . . ? C15 C14 C17 121.4(7) . . ? C13 C14 C17 120.2(8) . . ? C16 C15 C14 120.3(8) . . ? C15 C16 C11 121.8(8) . . ? O1 C17 O2 122.1(8) . . ? O1 C17 C14 119.0(8) . . ? O2 C17 C14 118.9(8) . . ? O1 C17 Cd1 59.5(4) . . ? O2 C17 Cd1 63.1(5) . . ? C14 C17 Cd1 172.4(6) . . ? C19 C18 C23 120.0 . . ? C19 C18 C10 120.4(8) . . ? C23 C18 C10 119.5(8) . . ? C18 C19 C20 120.0 . . ? C21 C20 C19 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 C24 122.0(13) . . ? C22 C21 C24 117.8(13) . . ? C23 C22 C21 120.0 . . ? C22 C23 C18 120.0 . . ? O3 C24 O4 128.1(16) . . ? O3 C24 C21 114.1(16) . . ? O4 C24 C21 117.5(15) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 58.91 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.065 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.121 # Attachment 'New1a.cif' data_New1a _database_code_depnum_ccdc_archive 'CCDC 777026' #TrackingRef 'New1a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H25.50 Cd1.25 N4 O8 Pd' _chemical_formula_weight 1033.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/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 7.2172(15) _cell_length_b 25.613(5) _cell_length_c 30.660(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.392(13) _cell_angle_gamma 90.00 _cell_volume 5632.5(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7339 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 58.91 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.218 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2046 _exptl_absorpt_coefficient_mu 6.713 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.597 _exptl_absorpt_correction_T_max 0.668 _exptl_absorpt_process_details CrysAlisPro _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7339 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.1568 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 58.91 _reflns_number_total 3942 _reflns_number_gt 1498 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'CrystalStructure and PLATON (Spek, 2001)' _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^)+(0.0253P)^2^+0.3520P] 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 3942 _refine_ls_number_parameters 275 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1648 _refine_ls_R_factor_gt 0.0886 _refine_ls_wR_factor_ref 0.2164 _refine_ls_wR_factor_gt 0.1752 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.008 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 Cd1 Cd 1.0000 0.40505(6) 0.2500 0.1428(7) Uani 1 2 d S . . Cd2 Cd 0.5000 0.4560(2) 0.2500 0.146(2) Uani 0.25 2 d SP . . Pd1 Pd -0.2500 0.2500 0.0000 0.1339(7) Uani 1 2 d S . . O1 O 0.6892(15) 0.3831(5) 0.2275(3) 0.164(4) Uani 1 1 d . . . O2 O 0.895(2) 0.3433(5) 0.1945(3) 0.182(4) Uani 1 1 d . . . O3 O 0.142(5) 0.5126(13) -0.2012(11) 0.40(2) Uani 1 1 d DU . . O4 O -0.151(5) 0.5451(7) -0.1953(5) 0.324(13) Uani 1 1 d DU . . N1 N -0.138(2) 0.2202(5) 0.0592(3) 0.150(4) Uani 1 1 d . . . N2 N -0.0456(17) 0.2985(5) -0.0007(3) 0.144(4) Uani 1 1 d . . . C1 C -0.204(2) 0.1807(7) 0.0810(5) 0.134(4) Uani 1 1 d . . . C2 C -0.084(3) 0.1764(9) 0.1239(5) 0.166(6) Uani 1 1 d . . . H2A H -0.1011 0.1536 0.1468 0.199 Uiso 1 1 calc R . . C3 C 0.046(3) 0.2101(9) 0.1230(5) 0.166(6) Uani 1 1 d . . . H3A H 0.1441 0.2136 0.1452 0.200 Uiso 1 1 calc R . . C4 C 0.024(3) 0.2435(9) 0.0827(5) 0.150(5) Uani 1 1 d . . . C5 C 0.140(3) 0.2806(8) 0.0709(4) 0.151(5) Uani 1 1 d . . . C6 C 0.110(3) 0.3048(7) 0.0318(5) 0.154(5) Uani 1 1 d . . . C7 C 0.226(3) 0.3449(9) 0.0200(6) 0.197(7) Uani 1 1 d . . . H7A H 0.3366 0.3553 0.0361 0.236 Uiso 1 1 calc R . . C8 C 0.149(3) 0.3671(8) -0.0202(5) 0.188(7) Uani 1 1 d . . . H8A H 0.1942 0.3949 -0.0354 0.226 Uiso 1 1 calc R . . C9 C -0.015(3) 0.3365(7) -0.0320(5) 0.157(5) Uani 1 1 d . . . C10 C -0.137(3) 0.3455(7) -0.0709(4) 0.154(5) Uani 1 1 d . . . C11 C 0.291(3) 0.2988(7) 0.1034(5) 0.148(5) Uani 1 1 d . . . C12 C 0.255(3) 0.3275(9) 0.1409(6) 0.189(7) Uani 1 1 d . . . H12A H 0.1338 0.3376 0.1441 0.227 Uiso 1 1 calc R . . C13 C 0.392(3) 0.3404(9) 0.1714(5) 0.184(7) Uani 1 1 d . . . H13A H 0.3633 0.3562 0.1972 0.221 Uiso 1 1 calc R . . C14 C 0.574(3) 0.3308(7) 0.1659(4) 0.155(5) Uani 1 1 d . . . C15 C 0.620(2) 0.3030(7) 0.1299(5) 0.162(5) Uani 1 1 d . . . H15A H 0.7430 0.2954 0.1260 0.195 Uiso 1 1 calc R . . C16 C 0.473(3) 0.2871(7) 0.1000(4) 0.164(6) Uani 1 1 d . . . H16A H 0.5003 0.2672 0.0761 0.196 Uiso 1 1 calc R . . C17 C 0.731(3) 0.3547(8) 0.1982(5) 0.148(5) Uani 1 1 d . . . C18 C -0.097(3) 0.3888(6) -0.0997(4) 0.182(7) Uani 1 1 d G . . C19 C 0.056(2) 0.3881(6) -0.1235(6) 0.219(9) Uani 1 1 d G . . H19A H 0.1392 0.3602 -0.1207 0.263 Uiso 1 1 calc R . . C20 C 0.085(2) 0.4292(9) -0.1516(5) 0.244(12) Uani 1 1 d G . . H20A H 0.1877 0.4287 -0.1676 0.293 Uiso 1 1 calc R . . C21 C -0.038(3) 0.4709(6) -0.1559(5) 0.32(2) Uani 1 1 d GD . . C22 C -0.191(3) 0.4716(6) -0.1320(6) 0.276(16) Uani 1 1 d G . . H22A H -0.2741 0.4995 -0.1348 0.331 Uiso 1 1 calc R . . C23 C -0.220(2) 0.4305(8) -0.1039(5) 0.226(9) Uani 1 1 d G . . H23A H -0.3226 0.4310 -0.0880 0.271 Uiso 1 1 calc R . . C24 C -0.010(4) 0.5130(11) -0.1893(9) 0.27(2) Uani 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 Cd1 0.1552(13) 0.1677(13) 0.1000(8) 0.000 -0.0102(7) 0.000 Cd2 0.158(5) 0.131(4) 0.133(3) 0.000 -0.056(3) 0.000 Pd1 0.1491(13) 0.1546(13) 0.0927(8) -0.0035(7) -0.0094(7) 0.0026(10) O1 0.172(9) 0.216(10) 0.101(5) -0.029(6) 0.009(5) -0.001(7) O2 0.160(10) 0.246(12) 0.134(6) -0.060(7) -0.015(7) 0.011(9) O3 0.60(5) 0.33(3) 0.28(2) 0.09(2) 0.07(3) -0.15(3) O4 0.61(4) 0.214(16) 0.145(10) 0.019(10) 0.034(17) 0.02(2) N1 0.200(13) 0.141(9) 0.104(6) 0.003(7) 0.000(8) 0.028(9) N2 0.158(10) 0.181(10) 0.091(6) 0.008(7) 0.005(6) 0.032(9) C1 0.119(10) 0.151(12) 0.128(9) 0.037(9) -0.010(8) -0.002(9) C2 0.128(13) 0.24(2) 0.124(10) 0.038(11) -0.004(9) 0.028(13) C3 0.130(13) 0.26(2) 0.109(9) 0.030(11) 0.009(9) -0.004(13) C4 0.131(12) 0.206(16) 0.105(9) -0.030(11) -0.019(9) 0.015(12) C5 0.148(13) 0.213(17) 0.085(8) -0.009(9) -0.020(8) -0.017(12) C6 0.169(14) 0.147(12) 0.139(12) -0.004(10) -0.016(11) -0.046(11) C7 0.22(2) 0.209(19) 0.150(13) 0.001(13) -0.044(12) -0.046(16) C8 0.238(19) 0.184(14) 0.128(10) 0.012(10) -0.041(11) -0.054(14) C9 0.185(15) 0.168(13) 0.110(9) -0.029(10) -0.012(9) -0.014(11) C10 0.185(16) 0.176(14) 0.099(8) 0.003(9) 0.001(9) -0.031(12) C11 0.117(12) 0.203(14) 0.124(10) -0.022(10) 0.012(9) -0.003(10) C12 0.139(13) 0.29(2) 0.139(11) -0.041(14) 0.005(10) -0.003(14) C13 0.160(16) 0.28(2) 0.110(9) -0.044(11) -0.014(11) -0.008(15) C14 0.157(15) 0.199(14) 0.101(8) -0.025(9) -0.022(9) -0.028(12) C15 0.144(13) 0.208(15) 0.130(10) -0.014(11) -0.011(9) 0.006(11) C16 0.145(14) 0.234(18) 0.108(8) -0.043(9) 0.001(9) -0.005(12) C17 0.139(14) 0.193(15) 0.112(9) -0.004(10) 0.012(10) -0.011(12) C18 0.24(2) 0.176(18) 0.120(11) -0.008(13) -0.021(12) 0.030(17) C19 0.31(3) 0.161(17) 0.190(18) 0.009(15) 0.038(18) -0.018(18) C20 0.38(4) 0.20(2) 0.146(14) 0.051(15) 0.015(17) -0.05(2) C21 0.63(7) 0.19(3) 0.120(14) 0.044(17) 0.00(2) -0.03(3) C22 0.54(5) 0.149(17) 0.140(14) 0.027(14) 0.03(2) 0.02(2) C23 0.31(3) 0.194(19) 0.180(16) 0.045(15) 0.060(16) 0.05(2) C24 0.31(4) 0.28(4) 0.20(3) -0.02(3) -0.07(3) 0.09(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.341(10) . ? Cd1 O1 2.341(10) 2_755 ? Cd1 O2 2.383(10) . ? Cd1 O2 2.383(10) 2_755 ? Cd1 O4 2.46(2) 6_666 ? Cd1 O4 2.46(2) 5_665 ? Cd1 C17 2.693(17) . ? Cd1 C17 2.694(17) 2_755 ? Cd2 O1 2.457(13) . ? Cd2 O1 2.457(13) 2_655 ? Pd1 N2 1.930(14) . ? Pd1 N2 1.930(14) 7_455 ? Pd1 N1 2.050(11) . ? Pd1 N1 2.050(11) 7_455 ? O1 C17 1.220(18) . ? O2 C17 1.235(17) . ? O3 C24 1.200(10) . ? O4 C24 1.302(10) . ? O4 Cd1 2.46(2) 5_665 ? N1 C1 1.333(17) . ? N1 C4 1.43(2) . ? N2 C9 1.40(2) . ? N2 C6 1.424(18) . ? C1 C10 1.34(2) 7_455 ? C1 C2 1.49(2) . ? C2 C3 1.28(2) . ? C3 C4 1.50(2) . ? C4 C5 1.34(2) . ? C5 C6 1.35(2) . ? C5 C11 1.47(2) . ? C6 C7 1.40(2) . ? C7 C8 1.41(2) . ? C8 C9 1.43(2) . ? C9 C10 1.42(2) . ? C10 C1 1.34(2) 7_455 ? C10 C18 1.47(2) . ? C11 C16 1.36(2) . ? C11 C12 1.41(2) . ? C12 C13 1.32(2) . ? C13 C14 1.37(2) . ? C14 C15 1.39(2) . ? C14 C17 1.55(2) . ? C15 C16 1.38(2) . ? C18 C19 1.3900 . ? C18 C23 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C21 C24 1.517(10) . ? C22 C23 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O1 152.2(6) . 2_755 ? O1 Cd1 O2 54.0(4) . . ? O1 Cd1 O2 105.5(4) 2_755 . ? O1 Cd1 O2 105.5(4) . 2_755 ? O1 Cd1 O2 54.0(4) 2_755 2_755 ? O2 Cd1 O2 96.8(6) . 2_755 ? O1 Cd1 O4 81.0(8) . 6_666 ? O1 Cd1 O4 114.0(8) 2_755 6_666 ? O2 Cd1 O4 134.6(9) . 6_666 ? O2 Cd1 O4 89.3(6) 2_755 6_666 ? O1 Cd1 O4 114.0(8) . 5_665 ? O1 Cd1 O4 81.0(8) 2_755 5_665 ? O2 Cd1 O4 89.3(6) . 5_665 ? O2 Cd1 O4 134.6(9) 2_755 5_665 ? O4 Cd1 O4 117.4(10) 6_666 5_665 ? O1 Cd1 C17 26.9(4) . . ? O1 Cd1 C17 131.4(6) 2_755 . ? O2 Cd1 C17 27.3(4) . . ? O2 Cd1 C17 104.7(5) 2_755 . ? O4 Cd1 C17 107.8(9) 6_666 . ? O4 Cd1 C17 101.0(7) 5_665 . ? O1 Cd1 C17 131.4(6) . 2_755 ? O1 Cd1 C17 26.9(4) 2_755 2_755 ? O2 Cd1 C17 104.7(5) . 2_755 ? O2 Cd1 C17 27.3(4) 2_755 2_755 ? O4 Cd1 C17 101.0(7) 6_666 2_755 ? O4 Cd1 C17 107.9(9) 5_665 2_755 ? C17 Cd1 C17 122.8(9) . 2_755 ? O1 Cd2 O1 81.0(5) . 2_655 ? N2 Pd1 N2 179.998(2) . 7_455 ? N2 Pd1 N1 91.2(6) . . ? N2 Pd1 N1 88.8(6) 7_455 . ? N2 Pd1 N1 88.8(6) . 7_455 ? N2 Pd1 N1 91.2(6) 7_455 7_455 ? N1 Pd1 N1 179.998(1) . 7_455 ? C17 O1 Cd1 92.9(11) . . ? C17 O1 Cd2 148.3(11) . . ? Cd1 O1 Cd2 106.2(4) . . ? C17 O2 Cd1 90.5(10) . . ? C24 O4 Cd1 91.6(13) . 5_665 ? C1 N1 C4 112.5(13) . . ? C1 N1 Pd1 126.8(12) . . ? C4 N1 Pd1 120.7(12) . . ? C9 N2 C6 103.2(14) . . ? C9 N2 Pd1 129.2(11) . . ? C6 N2 Pd1 127.6(11) . . ? N1 C1 C10 127.8(14) . 7_455 ? N1 C1 C2 107.0(16) . . ? C10 C1 C2 124.5(17) 7_455 . ? C3 C2 C1 106.6(17) . . ? C2 C3 C4 113.1(17) . . ? C5 C4 N1 131.1(15) . . ? C5 C4 C3 127.9(16) . . ? N1 C4 C3 100.6(18) . . ? C4 C5 C6 121.5(15) . . ? C4 C5 C11 118.6(14) . . ? C6 C5 C11 119.6(19) . . ? C5 C6 C7 121.7(17) . . ? C5 C6 N2 127.3(17) . . ? C7 C6 N2 110.6(15) . . ? C6 C7 C8 109.4(17) . . ? C7 C8 C9 103.5(17) . . ? N2 C9 C10 124.1(17) . . ? N2 C9 C8 113.3(14) . . ? C10 C9 C8 122.6(18) . . ? C1 C10 C9 123.3(16) 7_455 . ? C1 C10 C18 117.5(15) 7_455 . ? C9 C10 C18 119.0(17) . . ? C16 C11 C12 116.3(14) . . ? C16 C11 C5 121.8(14) . . ? C12 C11 C5 121.9(16) . . ? C13 C12 C11 121.1(18) . . ? C12 C13 C14 121.2(16) . . ? C13 C14 C15 120.7(14) . . ? C13 C14 C17 119.8(18) . . ? C15 C14 C17 119(2) . . ? C16 C15 C14 116.5(16) . . ? C11 C16 C15 123.9(15) . . ? O1 C17 O2 121.9(16) . . ? O1 C17 C14 119(2) . . ? O2 C17 C14 119.4(18) . . ? O1 C17 Cd1 60.2(9) . . ? O2 C17 Cd1 62.2(9) . . ? C14 C17 Cd1 174.4(12) . . ? C19 C18 C23 120.0 . . ? C19 C18 C10 122.0(17) . . ? C23 C18 C10 118.0(17) . . ? C20 C19 C18 120.0 . . ? C21 C20 C19 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 C24 119(2) . . ? C22 C21 C24 121(2) . . ? C23 C22 C21 120.0 . . ? C22 C23 C18 120.0 . . ? O3 C24 O4 134(2) . . ? O3 C24 C21 113(2) . . ? O4 C24 C21 113(2) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 58.91 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.481 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.065 # Attachment 'New1b.cif' data_New1b _database_code_depnum_ccdc_archive 'CCDC 777027' #TrackingRef 'New1b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H47.50 Cd1.25 N4 O19 Pd' _chemical_formula_weight 1231.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/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 7.1564(9) _cell_length_b 25.080(4) _cell_length_c 31.192(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.287(11) _cell_angle_gamma 90.00 _cell_volume 5564.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8511 _cell_measurement_theta_min 6.71 _cell_measurement_theta_max 58.91 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2486 _exptl_absorpt_coefficient_mu 7.036 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.581 _exptl_absorpt_correction_T_max 0.656 _exptl_absorpt_process_details CrysAlisPro _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8511 _diffrn_reflns_av_R_equivalents 0.0783 _diffrn_reflns_av_sigmaI/netI 0.1362 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 6.71 _diffrn_reflns_theta_max 58.91 _reflns_number_total 3941 _reflns_number_gt 1638 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'CrystalStructure and PLATON (Spek, 2001)' _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.020 0.000 0.000 289 17 ' ' 2 -0.045 0.500 0.000 289 17 ' ' 3 -0.003 0.674 0.250 219 10 ' ' 4 -0.021 0.174 0.250 219 10 ' ' 5 -0.007 1.000 0.500 289 17 ' ' 6 0.092 0.500 0.500 289 17 ' ' 7 -0.004 0.326 0.750 219 10 ' ' 8 -0.027 0.826 0.750 219 10 ' ' _platon_squeeze_details ; ; _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^)+(0.0796P)^2^+35.3560P] 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 3941 _refine_ls_number_parameters 284 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1608 _refine_ls_R_factor_gt 0.0938 _refine_ls_wR_factor_ref 0.2562 _refine_ls_wR_factor_gt 0.2092 _refine_ls_goodness_of_fit_ref 0.788 _refine_ls_restrained_S_all 0.788 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 1.0000 0.40132(7) 0.2500 0.1368(7) Uani 1 2 d S . . Cd2 Cd 0.5000 0.4567(3) 0.2500 0.156(2) Uani 0.25 2 d SPD . . Pd1 Pd -0.2500 0.2500 0.0000 0.1317(7) Uani 1 2 d S . . O1 O 0.6867(13) 0.3792(5) 0.2275(3) 0.144(3) Uani 1 1 d . . . O2 O 0.8932(15) 0.3349(5) 0.1955(3) 0.165(4) Uani 1 1 d . . . O3 O 0.148(4) 0.5136(11) -0.2009(8) 0.311(11) Uani 1 1 d DU . . O4 O -0.137(4) 0.5534(11) -0.1993(9) 0.343(12) Uani 1 1 d DU . . O5 O 0.545(7) 0.514(4) 0.199(4) 0.44(7) Uani 0.25 1 d PDU . . N1 N -0.1358(17) 0.2186(5) 0.0576(3) 0.128(3) Uani 1 1 d . . . N2 N -0.0435(17) 0.3008(6) 0.0010(4) 0.147(4) Uani 1 1 d . . . C1 C -0.206(2) 0.1782(7) 0.0794(5) 0.142(5) Uani 1 1 d . . . C2 C -0.087(3) 0.1701(8) 0.1189(5) 0.157(6) Uani 1 1 d . . . H2A H -0.0989 0.1439 0.1395 0.189 Uiso 1 1 calc R . . C3 C 0.043(3) 0.2079(10) 0.1197(5) 0.170(7) Uani 1 1 d . . . H3A H 0.1381 0.2129 0.1422 0.204 Uiso 1 1 calc R . . C4 C 0.019(2) 0.2393(7) 0.0822(4) 0.132(5) Uani 1 1 d . . . C5 C 0.1315(19) 0.2801(8) 0.0705(5) 0.139(5) Uani 1 1 d D . . C6 C 0.108(3) 0.3085(9) 0.0331(5) 0.158(6) Uani 1 1 d . . . C7 C 0.221(3) 0.3505(11) 0.0215(7) 0.215(10) Uani 1 1 d . . . H7A H 0.3295 0.3623 0.0380 0.257 Uiso 1 1 calc R . . C8 C 0.151(4) 0.3718(11) -0.0176(6) 0.226(11) Uani 1 1 d . . . H8A H 0.1993 0.4001 -0.0323 0.272 Uiso 1 1 calc R . . C9 C -0.015(3) 0.3400(8) -0.0308(6) 0.164(6) Uani 1 1 d . . . C10 C -0.133(3) 0.3499(7) -0.0671(5) 0.160(6) Uani 1 1 d . . . C11 C 0.2929(19) 0.2971(7) 0.1035(4) 0.136(5) Uani 1 1 d D . . C12 C 0.252(2) 0.3248(8) 0.1401(5) 0.170(7) Uani 1 1 d . . . H12A H 0.1274 0.3317 0.1441 0.204 Uiso 1 1 calc R . . C13 C 0.393(2) 0.3421(8) 0.1702(4) 0.159(6) Uani 1 1 d . . . H13A H 0.3624 0.3625 0.1934 0.190 Uiso 1 1 calc R . . C14 C 0.572(2) 0.3305(7) 0.1669(4) 0.138(5) Uani 1 1 d . . . C15 C 0.619(2) 0.2992(8) 0.1314(6) 0.163(6) Uani 1 1 d . . . H15A H 0.7420 0.2890 0.1289 0.195 Uiso 1 1 calc R . . C16 C 0.471(2) 0.2846(9) 0.1007(5) 0.162(6) Uani 1 1 d . . . H16A H 0.4992 0.2651 0.0769 0.194 Uiso 1 1 calc R . . C17 C 0.727(2) 0.3485(7) 0.1986(4) 0.124(4) Uani 1 1 d . . . C18 C -0.093(3) 0.3964(6) -0.0968(4) 0.178(7) Uani 1 1 d G . . C19 C 0.057(3) 0.3915(6) -0.1212(6) 0.200(8) Uani 1 1 d G . . H19A H 0.1344 0.3617 -0.1180 0.240 Uiso 1 1 calc R . . C20 C 0.091(3) 0.4311(9) -0.1505(6) 0.244(12) Uani 1 1 d G . . H20A H 0.1920 0.4278 -0.1668 0.293 Uiso 1 1 calc R . . C21 C -0.024(4) 0.4757(7) -0.1553(5) 0.32(2) Uani 1 1 d GD . . C22 C -0.175(4) 0.4806(6) -0.1309(6) 0.36(3) Uani 1 1 d G . . H22A H -0.2523 0.5104 -0.1342 0.431 Uiso 1 1 calc R . . C23 C -0.209(3) 0.4410(9) -0.1017(5) 0.298(18) Uani 1 1 d G . . H23A H -0.3098 0.4443 -0.0853 0.358 Uiso 1 1 calc R . . C24 C -0.002(3) 0.5202(8) -0.1885(6) 0.220(11) Uani 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 Cd1 0.1345(12) 0.1600(13) 0.1089(9) 0.000 -0.0183(7) 0.000 Cd2 0.120(4) 0.180(6) 0.158(5) 0.000 -0.032(4) 0.000 Pd1 0.1263(12) 0.1573(14) 0.1057(10) 0.0005(8) -0.0140(8) 0.0046(9) O1 0.140(7) 0.177(9) 0.113(6) -0.020(6) 0.003(5) -0.006(6) O2 0.109(7) 0.223(11) 0.156(8) -0.036(8) -0.025(6) 0.022(7) O3 0.338(14) 0.296(13) 0.300(13) 0.026(9) 0.045(9) -0.037(9) O4 0.372(15) 0.330(14) 0.323(14) -0.016(10) 0.025(10) 0.009(10) O5 0.45(7) 0.44(7) 0.44(7) 0.000(10) 0.046(13) 0.001(10) N1 0.128(8) 0.146(9) 0.105(7) 0.009(7) -0.016(7) 0.021(7) N2 0.147(10) 0.181(11) 0.105(7) -0.014(8) -0.016(7) 0.014(8) C1 0.151(13) 0.159(13) 0.111(10) 0.023(10) -0.014(9) -0.011(11) C2 0.150(14) 0.202(17) 0.116(11) 0.018(11) -0.007(10) -0.002(13) C3 0.139(14) 0.23(2) 0.126(12) 0.007(13) -0.032(10) -0.001(14) C4 0.093(9) 0.199(15) 0.099(9) 0.028(9) -0.012(7) 0.014(9) C5 0.107(10) 0.200(15) 0.107(10) -0.007(10) -0.005(8) 0.003(10) C6 0.154(14) 0.212(18) 0.103(10) 0.014(11) -0.014(10) -0.039(13) C7 0.201(19) 0.28(3) 0.149(16) 0.013(17) -0.037(14) -0.08(2) C8 0.26(2) 0.28(3) 0.132(13) 0.034(15) -0.034(15) -0.11(2) C9 0.165(14) 0.197(16) 0.121(11) 0.006(12) -0.020(10) -0.036(13) C10 0.186(15) 0.171(14) 0.110(10) 0.022(10) -0.039(10) -0.033(12) C11 0.102(10) 0.196(14) 0.106(9) -0.024(9) -0.009(7) 0.001(9) C12 0.119(11) 0.27(2) 0.123(11) -0.019(13) -0.001(9) 0.041(12) C13 0.108(10) 0.249(19) 0.112(9) -0.046(10) -0.022(8) 0.028(11) C14 0.109(10) 0.202(15) 0.096(8) -0.012(9) -0.019(7) 0.011(10) C15 0.113(10) 0.219(17) 0.149(13) -0.038(13) -0.014(9) 0.024(11) C16 0.113(12) 0.26(2) 0.114(10) -0.035(11) -0.003(9) 0.008(12) C17 0.113(11) 0.164(13) 0.093(8) -0.002(8) 0.002(8) 0.014(9) C18 0.23(2) 0.177(19) 0.118(12) 0.018(13) -0.042(13) -0.012(16) C19 0.23(2) 0.167(18) 0.20(2) 0.021(17) 0.015(17) -0.030(16) C20 0.34(3) 0.19(2) 0.20(2) 0.06(2) 0.02(2) -0.06(2) C21 0.68(7) 0.18(2) 0.100(14) 0.024(16) 0.04(2) -0.10(3) C22 0.73(8) 0.24(3) 0.114(16) 0.067(18) 0.04(3) 0.11(4) C23 0.51(5) 0.24(3) 0.142(17) 0.059(18) 0.03(2) 0.12(3) C24 0.177(18) 0.32(3) 0.152(15) -0.043(18) -0.014(14) 0.09(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 Cd1 O4 2.26(3) 5_665 ? Cd1 O4 2.26(3) 6_666 ? Cd1 O1 2.341(9) 2_755 ? Cd1 O1 2.341(9) . ? Cd1 O2 2.443(10) . ? Cd1 O2 2.443(10) 2_755 ? Cd1 C17 2.729(15) 2_755 ? Cd1 C17 2.730(15) . ? Cd1 C24 2.749(15) 5_665 ? Cd1 C24 2.749(15) 6_666 ? Cd2 O5 2.195(10) . ? Cd2 O5 2.195(10) 2_655 ? Cd2 O1 2.503(13) 2_655 ? Cd2 O1 2.503(13) . ? Pd1 N2 1.948(14) 7_455 ? Pd1 N2 1.948(14) . ? Pd1 N1 2.047(10) . ? Pd1 N1 2.048(10) 7_455 ? O1 C17 1.241(16) . ? O2 C17 1.251(15) . ? O3 C24 1.192(10) . ? O4 C24 1.289(10) . ? O4 Cd1 2.26(3) 5_665 ? N1 C1 1.348(18) . ? N1 C4 1.376(18) . ? N2 C6 1.404(18) . ? N2 C9 1.43(2) . ? C1 C10 1.37(2) 7_455 ? C1 C2 1.43(2) . ? C2 C3 1.33(2) . ? C3 C4 1.41(2) . ? C4 C5 1.38(2) . ? C5 C6 1.36(2) . ? C5 C11 1.521(9) . ? C6 C7 1.40(2) . ? C7 C8 1.38(3) . ? C8 C9 1.46(2) . ? C9 C10 1.36(2) . ? C10 C1 1.37(2) 7_455 ? C10 C18 1.54(2) . ? C11 C16 1.325(19) . ? C11 C12 1.39(2) . ? C12 C13 1.37(2) . ? C13 C14 1.332(18) . ? C14 C15 1.43(2) . ? C14 C17 1.473(19) . ? C15 C16 1.40(2) . ? C18 C19 1.3900 . ? C18 C23 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C21 C24 1.542(10) . ? C22 C23 1.3900 . ? C24 Cd1 2.749(15) 5_665 ? 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 O4 Cd1 O4 119.6(13) 5_665 6_666 ? O4 Cd1 O1 81.6(7) 5_665 2_755 ? O4 Cd1 O1 112.6(7) 6_666 2_755 ? O4 Cd1 O1 112.6(7) 5_665 . ? O4 Cd1 O1 81.6(7) 6_666 . ? O1 Cd1 O1 152.6(6) 2_755 . ? O4 Cd1 O2 89.0(8) 5_665 . ? O4 Cd1 O2 134.8(7) 6_666 . ? O1 Cd1 O2 105.3(4) 2_755 . ? O1 Cd1 O2 54.1(4) . . ? O4 Cd1 O2 134.8(7) 5_665 2_755 ? O4 Cd1 O2 89.0(8) 6_666 2_755 ? O1 Cd1 O2 54.1(4) 2_755 2_755 ? O1 Cd1 O2 105.3(4) . 2_755 ? O2 Cd1 O2 93.9(6) . 2_755 ? O4 Cd1 C17 108.5(7) 5_665 2_755 ? O4 Cd1 C17 99.8(8) 6_666 2_755 ? O1 Cd1 C17 27.0(4) 2_755 2_755 ? O1 Cd1 C17 131.4(5) . 2_755 ? O2 Cd1 C17 103.1(4) . 2_755 ? O2 Cd1 C17 27.3(4) 2_755 2_755 ? O4 Cd1 C17 99.8(8) 5_665 . ? O4 Cd1 C17 108.5(7) 6_666 . ? O1 Cd1 C17 131.4(5) 2_755 . ? O1 Cd1 C17 27.0(4) . . ? O2 Cd1 C17 27.3(4) . . ? O2 Cd1 C17 103.1(4) 2_755 . ? C17 Cd1 C17 122.0(7) 2_755 . ? O4 Cd1 C24 27.7(3) 5_665 5_665 ? O4 Cd1 C24 99.5(9) 6_666 5_665 ? O1 Cd1 C24 107.5(6) 2_755 5_665 ? O1 Cd1 C24 92.2(5) . 5_665 ? O2 Cd1 C24 91.6(5) . 5_665 ? O2 Cd1 C24 161.5(6) 2_755 5_665 ? C17 Cd1 C24 134.3(6) 2_755 5_665 ? C17 Cd1 C24 89.8(6) . 5_665 ? O4 Cd1 C24 99.5(9) 5_665 6_666 ? O4 Cd1 C24 27.7(3) 6_666 6_666 ? O1 Cd1 C24 92.2(6) 2_755 6_666 ? O1 Cd1 C24 107.5(6) . 6_666 ? O2 Cd1 C24 161.5(6) . 6_666 ? O2 Cd1 C24 91.6(5) 2_755 6_666 ? C17 Cd1 C24 89.8(6) 2_755 6_666 ? C17 Cd1 C24 134.3(6) . 6_666 ? C24 Cd1 C24 88.6(9) 5_665 6_666 ? O5 Cd2 O5 98(8) . 2_655 ? O5 Cd2 O1 147(3) . 2_655 ? O5 Cd2 O1 100(3) 2_655 2_655 ? O5 Cd2 O1 100(3) . . ? O5 Cd2 O1 147(3) 2_655 . ? O1 Cd2 O1 78.1(5) 2_655 . ? N2 Pd1 N2 180.0(6) 7_455 . ? N2 Pd1 N1 89.6(5) 7_455 . ? N2 Pd1 N1 90.4(5) . . ? N2 Pd1 N1 90.4(5) 7_455 7_455 ? N2 Pd1 N1 89.6(5) . 7_455 ? N1 Pd1 N1 179.998(2) . 7_455 ? C17 O1 Cd1 94.2(9) . . ? C17 O1 Cd2 149.1(9) . . ? Cd1 O1 Cd2 104.8(4) . . ? C17 O2 Cd1 89.2(9) . . ? C24 O4 Cd1 97.9(17) . 5_665 ? C1 N1 C4 108.8(12) . . ? C1 N1 Pd1 126.7(10) . . ? C4 N1 Pd1 124.3(11) . . ? C6 N2 C9 104.1(14) . . ? C6 N2 Pd1 128.8(13) . . ? C9 N2 Pd1 127.1(10) . . ? N1 C1 C10 126.4(14) . 7_455 ? N1 C1 C2 108.8(15) . . ? C10 C1 C2 124.8(17) 7_455 . ? C3 C2 C1 105.3(17) . . ? C2 C3 C4 111.1(15) . . ? N1 C4 C5 126.2(12) . . ? N1 C4 C3 105.8(16) . . ? C5 C4 C3 127.8(15) . . ? C6 C5 C4 126.4(12) . . ? C6 C5 C11 116.7(16) . . ? C4 C5 C11 116.9(14) . . ? C5 C6 N2 123.6(17) . . ? C5 C6 C7 126.3(16) . . ? N2 C6 C7 110.1(15) . . ? C8 C7 C6 110.9(17) . . ? C7 C8 C9 104.1(19) . . ? C10 C9 N2 125.9(16) . . ? C10 C9 C8 123.2(19) . . ? N2 C9 C8 110.8(14) . . ? C9 C10 C1 124.4(17) . 7_455 ? C9 C10 C18 120.4(16) . . ? C1 C10 C18 115.1(13) 7_455 . ? C16 C11 C12 117.6(12) . . ? C16 C11 C5 123.6(14) . . ? C12 C11 C5 118.8(14) . . ? C13 C12 C11 121.0(14) . . ? C14 C13 C12 121.3(15) . . ? C13 C14 C15 119.3(13) . . ? C13 C14 C17 122.8(15) . . ? C15 C14 C17 117.9(14) . . ? C16 C15 C14 117.0(14) . . ? C11 C16 C15 123.6(15) . . ? O1 C17 O2 121.6(14) . . ? O1 C17 C14 117.4(15) . . ? O2 C17 C14 121.0(15) . . ? O1 C17 Cd1 58.8(7) . . ? O2 C17 Cd1 63.5(8) . . ? C14 C17 Cd1 168.6(11) . . ? C19 C18 C23 120.0 . . ? C19 C18 C10 117.8(17) . . ? C23 C18 C10 122.0(17) . . ? C18 C19 C20 120.0 . . ? C21 C20 C19 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 C24 123.5(19) . . ? C22 C21 C24 116.5(19) . . ? C21 C22 C23 120.0 . . ? C22 C23 C18 120.0 . . ? O3 C24 O4 133(2) . . ? O3 C24 C21 106.2(19) . . ? O4 C24 C21 121(2) . . ? O3 C24 Cd1 78.3(15) . 5_665 ? O4 C24 Cd1 54.4(15) . 5_665 ? C21 C24 Cd1 174.4(17) . 5_665 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 58.91 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.524 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.081 # Attachment 'New1c.cif' data_New1c _database_code_depnum_ccdc_archive 'CCDC 806276' #TrackingRef 'New1c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H41 Cd1.25 N4 O8.50 Pd' _chemical_formula_weight 1248.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/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 7.2751(3) _cell_length_b 25.5905(15) _cell_length_c 30.7749(11) _cell_angle_alpha 90.00 _cell_angle_beta 96.478(4) _cell_angle_gamma 90.00 _cell_volume 5692.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9346 _cell_measurement_theta_min 3.45 _cell_measurement_theta_max 58.93 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2508 _exptl_absorpt_coefficient_mu 6.754 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.401 _exptl_absorpt_correction_T_max 0.583 _exptl_absorpt_process_details CrysAlisPro _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9346 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 58.93 _reflns_number_total 4037 _reflns_number_gt 2852 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'CrystalStructure and PLATON (Spek, 2001)' _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.109 0.250 0.000 357 67 ' ' 2 0.047 0.750 0.000 357 67 ' ' 3 -0.013 0.573 0.250 230 47 ' ' 4 -0.022 0.073 0.250 230 47 ' ' 5 -0.088 0.750 0.500 357 67 ' ' 6 0.104 0.250 0.500 357 67 ' ' 7 -0.013 0.427 0.750 230 47 ' ' 8 -0.022 0.927 0.750 230 47 ' ' _platon_squeeze_details ; ; _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^)+(0.0796P)^2^+28.3160P] 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 4037 _refine_ls_number_parameters 280 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1136 _refine_ls_R_factor_gt 0.0969 _refine_ls_wR_factor_ref 0.2323 _refine_ls_wR_factor_gt 0.2234 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.5000 0.34427(5) 0.2500 0.1149(5) Uani 1 2 d S . . Cd2 Cd 1.0000 0.2891(3) 0.2500 0.1442(19) Uani 0.25 2 d SPD . . Pd1 Pd 1.5000 0.5000 0.0000 0.1079(5) Uani 1 2 d S . . O1 O 0.7872(10) 0.3669(3) 0.2278(2) 0.119(2) Uani 1 1 d . . . O2 O 0.5501(12) 0.4079(5) 0.1941(3) 0.154(3) Uani 1 1 d . . . O3 O 0.889(3) 0.2409(9) -0.2027(8) 0.285(9) Uani 1 1 d DU . . O5 O 1.0000 0.1993(5) 0.2500 0.42(4) Uani 0.25 2 d SPDU . . N1 N 1.4468(12) 0.5284(4) 0.0588(3) 0.106(2) Uani 1 1 d . . . N2 N 1.2905(13) 0.4504(4) -0.0001(3) 0.115(3) Uani 1 1 d . . . C1 C 1.5381(17) 0.5675(5) 0.0816(4) 0.112(3) Uani 1 1 d . . . C2 C 1.464(2) 0.5748(6) 0.1225(4) 0.130(4) Uani 1 1 d . . . H2A H 1.5037 0.5988 0.1443 0.157 Uiso 1 1 calc R . . C3 C 1.332(2) 0.5410(6) 0.1229(4) 0.128(4) Uani 1 1 d . . . H3A H 1.2589 0.5373 0.1456 0.154 Uiso 1 1 calc R . . C4 C 1.3117(16) 0.5094(6) 0.0833(3) 0.115(4) Uani 1 1 d . . . C5 C 1.1862(15) 0.4705(6) 0.0714(3) 0.114(3) Uani 1 1 d . . . C6 C 1.1728(17) 0.4445(5) 0.0332(4) 0.115(3) Uani 1 1 d . . . C7 C 1.048(3) 0.4034(8) 0.0216(5) 0.175(6) Uani 1 1 d . . . H7A H 0.9575 0.3912 0.0382 0.210 Uiso 1 1 calc R . . C8 C 1.084(3) 0.3838(7) -0.0196(5) 0.172(6) Uani 1 1 d . . . H8A H 1.0197 0.3575 -0.0357 0.207 Uiso 1 1 calc R . . C9 C 1.2351(19) 0.4121(5) -0.0312(4) 0.123(4) Uani 1 1 d . . . C10 C 1.3165(19) 0.4032(5) -0.0688(4) 0.122(3) Uani 1 1 d . . . C11 C 1.0628(15) 0.4553(6) 0.1054(4) 0.120(4) Uani 1 1 d . . . C12 C 1.1394(17) 0.4259(6) 0.1412(4) 0.137(5) Uani 1 1 d . . . H12A H 1.2649 0.4178 0.1444 0.165 Uiso 1 1 calc R . . C13 C 1.0276(16) 0.4090(6) 0.1716(4) 0.131(4) Uani 1 1 d . . . H13A H 1.0788 0.3900 0.1958 0.157 Uiso 1 1 calc R . . C14 C 0.8383(15) 0.4200(5) 0.1666(3) 0.105(3) Uani 1 1 d . . . C15 C 0.7662(16) 0.4493(6) 0.1313(4) 0.128(4) Uani 1 1 d . . . H15A H 0.6414 0.4581 0.1285 0.154 Uiso 1 1 calc R . . C16 C 0.8739(15) 0.4660(6) 0.1003(4) 0.126(4) Uani 1 1 d . . . H16A H 0.8211 0.4844 0.0760 0.151 Uiso 1 1 calc R . . C17 C 0.7195(16) 0.3967(5) 0.1987(4) 0.111(3) Uani 1 1 d . . . C18 C 1.242(2) 0.3594(4) -0.0992(3) 0.149(5) Uani 1 1 d G . . C19 C 1.0676(19) 0.3635(5) -0.1227(4) 0.175(6) Uani 1 1 d G . . H19A H 0.9955 0.3930 -0.1196 0.210 Uiso 1 1 calc R . . C20 C 1.001(2) 0.3235(7) -0.1507(4) 0.228(11) Uani 1 1 d G . . H20A H 0.8847 0.3262 -0.1664 0.274 Uiso 1 1 calc R . . C21 C 1.109(3) 0.2794(5) -0.1553(4) 0.28(2) Uani 1 1 d GD . . C22 C 1.283(3) 0.2753(5) -0.1318(5) 0.30(2) Uani 1 1 d G . . H22A H 1.3555 0.2459 -0.1349 0.365 Uiso 1 1 calc R . . C23 C 1.350(2) 0.3154(6) -0.1038(4) 0.226(11) Uani 1 1 d G . . H23A H 1.4663 0.3126 -0.0881 0.271 Uiso 1 1 calc R . . C24 C 1.049(3) 0.2366(7) -0.1891(5) 0.215(10) Uani 1 1 d D . . O4 O 1.183(3) 0.2050(9) -0.1934(7) 0.310(9) Uani 1 1 d DU . . 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 Cd1 0.1186(8) 0.1421(10) 0.0869(7) 0.000 0.0238(5) 0.000 Cd2 0.129(4) 0.166(5) 0.146(4) 0.000 0.050(3) 0.000 Pd1 0.1060(8) 0.1338(10) 0.0859(7) 0.0026(6) 0.0205(5) 0.0123(6) O1 0.111(5) 0.146(6) 0.097(5) 0.021(5) 0.001(4) -0.007(5) O2 0.115(6) 0.213(9) 0.141(7) 0.051(7) 0.046(5) 0.025(6) O3 0.317(13) 0.262(12) 0.272(12) -0.013(9) 0.014(9) -0.045(9) O5 0.50(5) 0.35(5) 0.42(5) 0.02(3) 0.11(3) 0.00(3) N1 0.101(5) 0.132(7) 0.084(5) 0.005(5) 0.015(4) 0.017(5) N2 0.126(6) 0.139(7) 0.082(5) -0.004(5) 0.019(5) 0.019(6) C1 0.118(8) 0.128(9) 0.092(7) -0.016(7) 0.015(6) 0.015(7) C2 0.126(9) 0.160(11) 0.108(8) -0.021(8) 0.023(7) -0.002(9) C3 0.123(9) 0.169(12) 0.095(7) -0.011(8) 0.030(6) 0.024(9) C4 0.103(7) 0.162(10) 0.083(6) 0.000(7) 0.027(6) 0.027(8) C5 0.095(7) 0.163(10) 0.084(7) 0.001(7) 0.012(5) -0.003(7) C6 0.121(8) 0.131(9) 0.095(7) -0.001(7) 0.019(6) -0.021(7) C7 0.191(15) 0.225(18) 0.113(10) -0.006(11) 0.040(9) -0.058(14) C8 0.206(16) 0.195(15) 0.120(10) -0.029(10) 0.035(10) -0.069(13) C9 0.141(9) 0.135(9) 0.097(7) 0.004(7) 0.035(7) -0.017(8) C10 0.137(9) 0.125(9) 0.104(8) -0.002(7) 0.013(7) -0.001(8) C11 0.099(7) 0.176(11) 0.086(6) 0.016(7) 0.019(5) -0.001(7) C12 0.099(7) 0.216(14) 0.100(8) 0.019(9) 0.023(6) 0.022(8) C13 0.104(8) 0.195(13) 0.093(7) 0.039(8) 0.009(6) 0.017(8) C14 0.102(7) 0.133(8) 0.083(6) 0.009(6) 0.017(5) 0.012(6) C15 0.094(7) 0.175(11) 0.116(8) 0.029(8) 0.016(6) 0.028(7) C16 0.092(7) 0.180(12) 0.107(7) 0.037(8) 0.018(6) 0.013(7) C17 0.098(7) 0.142(9) 0.093(7) -0.003(7) 0.014(6) 0.003(7) C18 0.212(16) 0.134(11) 0.105(9) 0.002(8) 0.040(10) 0.002(11) C19 0.191(16) 0.177(15) 0.153(13) -0.010(12) 0.008(12) -0.037(13) C20 0.34(3) 0.199(19) 0.138(14) -0.031(15) 0.008(16) -0.11(2) C21 0.58(6) 0.158(17) 0.100(12) -0.031(13) 0.00(2) -0.10(3) C22 0.55(6) 0.21(2) 0.129(15) -0.072(16) -0.06(2) 0.12(3) C23 0.34(3) 0.181(16) 0.139(14) -0.035(13) -0.038(16) 0.08(2) C24 0.25(2) 0.26(2) 0.147(15) 0.039(17) 0.061(16) 0.08(2) O4 0.352(13) 0.293(12) 0.282(12) -0.015(9) 0.026(9) 0.000(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 Cd1 O1 2.343(7) . ? Cd1 O1 2.343(7) 2_655 ? Cd1 O4 2.42(2) 7_655 ? Cd1 O4 2.42(2) 8_456 ? Cd1 O2 2.426(9) . ? Cd1 O2 2.426(9) 2_655 ? Cd1 C17 2.723(12) . ? Cd1 C17 2.723(12) 2_655 ? Cd2 O5 2.299(10) . ? Cd2 O1 2.566(10) 2_755 ? Cd2 O1 2.566(10) . ? Pd1 N2 1.982(10) 5_865 ? Pd1 N2 1.982(10) . ? Pd1 N1 2.028(8) 5_865 ? Pd1 N1 2.028(8) . ? O1 C17 1.236(13) . ? O2 C17 1.257(13) . ? O3 C24 1.193(10) . ? N1 C1 1.353(15) . ? N1 C4 1.392(14) . ? N2 C9 1.398(15) . ? N2 C6 1.417(14) . ? C1 C10 1.389(17) 5_865 ? C1 C2 1.436(16) . ? C2 C3 1.296(17) . ? C3 C4 1.455(17) . ? C4 C5 1.374(17) . ? C5 C6 1.342(16) . ? C5 C11 1.505(15) . ? C6 C7 1.41(2) . ? C7 C8 1.41(2) . ? C8 C9 1.397(19) . ? C9 C10 1.377(16) . ? C10 C1 1.389(17) 5_865 ? C10 C18 1.520(15) . ? C11 C16 1.393(15) . ? C11 C12 1.397(17) . ? C12 C13 1.378(16) . ? C13 C14 1.397(15) . ? C14 C15 1.374(15) . ? C14 C17 1.507(15) . ? C15 C16 1.369(16) . ? C18 C19 1.3900 . ? C18 C23 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C21 C24 1.540(10) . ? C22 C23 1.3900 . ? C24 O4 1.288(10) . ? O4 Cd1 2.42(2) 7_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O1 151.4(4) . 2_655 ? O1 Cd1 O4 110.8(6) . 7_655 ? O1 Cd1 O4 84.4(6) 2_655 7_655 ? O1 Cd1 O4 84.4(6) . 8_456 ? O1 Cd1 O4 110.8(6) 2_655 8_456 ? O4 Cd1 O4 117.3(11) 7_655 8_456 ? O1 Cd1 O2 54.3(3) . . ? O1 Cd1 O2 104.6(3) 2_655 . ? O4 Cd1 O2 87.4(6) 7_655 . ? O4 Cd1 O2 138.1(6) 8_456 . ? O1 Cd1 O2 104.6(3) . 2_655 ? O1 Cd1 O2 54.3(3) 2_655 2_655 ? O4 Cd1 O2 138.1(6) 7_655 2_655 ? O4 Cd1 O2 87.4(6) 8_456 2_655 ? O2 Cd1 O2 95.7(5) . 2_655 ? O1 Cd1 C17 26.9(3) . . ? O1 Cd1 C17 130.4(4) 2_655 . ? O4 Cd1 C17 98.7(6) 7_655 . ? O4 Cd1 C17 111.2(6) 8_456 . ? O2 Cd1 C17 27.5(3) . . ? O2 Cd1 C17 103.1(4) 2_655 . ? O1 Cd1 C17 130.4(4) . 2_655 ? O1 Cd1 C17 26.9(3) 2_655 2_655 ? O4 Cd1 C17 111.2(6) 7_655 2_655 ? O4 Cd1 C17 98.7(6) 8_456 2_655 ? O2 Cd1 C17 103.1(4) . 2_655 ? O2 Cd1 C17 27.5(3) 2_655 2_655 ? C17 Cd1 C17 120.9(5) . 2_655 ? O5 Cd2 O1 140.8(2) . 2_755 ? O5 Cd2 O1 140.8(2) . . ? O1 Cd2 O1 78.3(4) 2_755 . ? N2 Pd1 N2 180.0(5) 5_865 . ? N2 Pd1 N1 90.4(4) 5_865 5_865 ? N2 Pd1 N1 89.6(4) . 5_865 ? N2 Pd1 N1 89.6(4) 5_865 . ? N2 Pd1 N1 90.4(4) . . ? N1 Pd1 N1 180.0(6) 5_865 . ? C17 O1 Cd1 93.9(7) . . ? C17 O1 Cd2 148.3(7) . . ? Cd1 O1 Cd2 105.2(3) . . ? C17 O2 Cd1 89.5(7) . . ? C1 N1 C4 108.2(10) . . ? C1 N1 Pd1 126.6(7) . . ? C4 N1 Pd1 125.2(8) . . ? C9 N2 C6 105.7(10) . . ? C9 N2 Pd1 127.8(7) . . ? C6 N2 Pd1 126.4(8) . . ? N1 C1 C10 126.7(10) . 5_865 ? N1 C1 C2 109.9(12) . . ? C10 C1 C2 123.4(12) 5_865 . ? C3 C2 C1 105.8(12) . . ? C2 C3 C4 111.7(11) . . ? C5 C4 N1 126.6(10) . . ? C5 C4 C3 128.9(11) . . ? N1 C4 C3 104.4(12) . . ? C6 C5 C4 125.0(10) . . ? C6 C5 C11 119.4(12) . . ? C4 C5 C11 115.5(10) . . ? C5 C6 C7 124.8(12) . . ? C5 C6 N2 126.2(11) . . ? C7 C6 N2 108.7(11) . . ? C6 C7 C8 108.2(13) . . ? C9 C8 C7 106.1(14) . . ? C10 C9 C8 123.8(13) . . ? C10 C9 N2 125.0(12) . . ? C8 C9 N2 111.2(11) . . ? C9 C10 C1 124.2(12) . 5_865 ? C9 C10 C18 118.8(12) . . ? C1 C10 C18 117.0(11) 5_865 . ? C16 C11 C12 119.7(10) . . ? C16 C11 C5 122.0(10) . . ? C12 C11 C5 118.1(10) . . ? C13 C12 C11 119.5(11) . . ? C12 C13 C14 120.7(11) . . ? C15 C14 C13 118.8(10) . . ? C15 C14 C17 122.5(10) . . ? C13 C14 C17 118.6(10) . . ? C16 C15 C14 121.6(10) . . ? C15 C16 C11 119.7(11) . . ? O1 C17 O2 121.8(11) . . ? O1 C17 C14 120.5(10) . . ? O2 C17 C14 117.6(11) . . ? O1 C17 Cd1 59.1(6) . . ? O2 C17 Cd1 63.0(6) . . ? C14 C17 Cd1 172.9(8) . . ? C19 C18 C23 120.0 . . ? C19 C18 C10 120.4(11) . . ? C23 C18 C10 119.6(11) . . ? C18 C19 C20 120.0 . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C22 C21 C24 118.2(16) . . ? C20 C21 C24 121.6(16) . . ? C21 C22 C23 120.0 . . ? C22 C23 C18 120.0 . . ? O3 C24 O4 138(2) . . ? O3 C24 C21 111.4(19) . . ? O4 C24 C21 110.6(19) . . ? C24 O4 Cd1 92.2(13) . 7_655 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 58.93 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.877 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.113