#------------------------------------------------------------------------------ #$Date: 2019-02-09 03:59:04 +0200 (Sat, 09 Feb 2019) $ #$Revision: 213572 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/81/7058162.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7058162 loop_ _publ_author_name 'Inci, Duygu' 'Ayd\?in, Rahmiye' 'Vatan, \"Ozg\"ur' '\,SAH\.IN, Onur' '\,Cink\?il\?i\,c, Nil\"ufer' _publ_section_title ; Water soluble binary and ternary palladium(II) complexes containing amino acids and intercalating ligands: Synthesis, characterization, biomolecular interactions and cytotoxicities ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/C8NJ05934A _journal_year 2019 _chemical_formula_moiety 'C21 H18 N3 O3 Pd, N O3, H2 O' _chemical_formula_sum 'C21 H20 N4 O7 Pd' _chemical_formula_weight 546.81 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2013 _audit_update_record ; 2017-12-13 deposited with the CCDC. 2019-02-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.171(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.6375(19) _cell_length_b 22.698(5) _cell_length_c 10.034(2) _cell_measurement_reflns_used 9787 _cell_measurement_temperature 296 _cell_measurement_theta_max 26.38 _cell_measurement_theta_min 3.15 _cell_volume 2108.1(8) _computing_cell_refinement 'SAINT(Bruker, 2013)' _computing_data_collection 'APEX2 (Bruker, 2013)' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 296 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0675 _diffrn_reflns_av_unetI/netI 0.0349 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 49452 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.467 _diffrn_reflns_theta_min 2.840 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.934 _exptl_absorpt_correction_T_max 0.7166 _exptl_absorpt_correction_T_min 0.6372 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details Bruker _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.723 _exptl_crystal_description block _exptl_crystal_F_000 1104 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _refine_diff_density_max 1.181 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.110 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.217 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 310 _refine_ls_number_reflns 4286 _refine_ls_number_restraints 9 _refine_ls_restrained_S_all 1.254 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0635 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+13.2398P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1233 _refine_ls_wR_factor_ref 0.1282 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3732 _reflns_number_total 4286 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8nj05934a2.cif _cod_data_source_block shelx_CCDC1 _cod_original_cell_volume 2108.0(7) _cod_database_code 7058162 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelxl_version_number 2013-4 _shelx_res_file ; TITL rahmiye12_6_0m_a.res in P2(1)/n CELL 0.71073 9.6375 22.6976 10.0338 90.000 106.171 90.000 ZERR 4.00 0.0019 0.0049 0.0020 0.000 0.006 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O PD UNIT 84 80 16 28 4 MERG 2 OMIT -4.00 180.00 DFIX 1.300 0.020 H4A H4B DFIX 0.830 0.020 H4A O4 DFIX 0.830 0.020 O4 H4B EQIV $1 x+1/2, -y+1/2, z+1/2 HTAB C1 O2_$1 EQIV $2 x-1/2, -y+1/2, z-1/2 HTAB C1 O6_$2 EQIV $3 x-1/2, -y+1/2, z-3/2 HTAB C9 O6_$3 HTAB C20 O5 HTAB O3 O5 HTAB N3 O2_$1 HTAB N3 O5_$2 HTAB N3 O6_$2 EQIV $4 x, y, z-1 HTAB O4 O7_$4 DFIX 2.100 0.020 H3A H14B DFIX 2.100 0.020 H3B H14A DFIX 2.100 0.020 H14B H15A EADP C14A C14B DFIX 2.100 0.020 H3B H14A DFIX 2.100 0.020 H14A H15B DFIX 2.100 0.020 H14B H4A FMAP 2 PLAN 5 ACTA BOND BOND $H CONF L.S. 10 WGHT 0.000100 13.239799 FVAR 0.35850 0.74640 C1 1 0.616860 0.393825 0.317110 11.00000 0.04316 0.03551 = 0.03465 0.00287 0.00424 0.00268 AFIX 43 H1 2 0.568306 0.367011 0.358023 11.00000 -1.20000 AFIX 0 C2 1 0.729722 0.426743 0.401347 11.00000 0.05267 0.05588 = 0.03223 -0.00664 -0.00077 0.00255 AFIX 43 H2 2 0.754354 0.422225 0.497212 11.00000 -1.20000 AFIX 0 C3 1 0.804495 0.465787 0.343031 11.00000 0.04637 0.05319 = 0.04844 -0.01512 -0.00145 -0.00697 AFIX 43 H3 2 0.880435 0.487414 0.399260 11.00000 -1.20000 AFIX 0 C4 1 0.766328 0.473071 0.198509 11.00000 0.03623 0.03763 = 0.05253 -0.00292 0.00595 0.00293 C5 1 0.835980 0.511409 0.124176 11.00000 0.04743 0.05420 = 0.07030 -0.00209 0.00962 -0.01752 AFIX 43 H5 2 0.913364 0.534229 0.173688 11.00000 -1.20000 AFIX 0 C6 1 0.793368 0.515557 -0.014731 11.00000 0.05171 0.04775 = 0.07452 0.00790 0.02232 -0.01580 AFIX 43 H6 2 0.840314 0.541775 -0.058723 11.00000 -1.20000 AFIX 0 C7 1 0.677450 0.480568 -0.096478 11.00000 0.04163 0.03741 = 0.05464 0.01096 0.01914 0.00159 C8 1 0.628560 0.480177 -0.242015 11.00000 0.05861 0.04702 = 0.05488 0.01739 0.02604 0.00383 AFIX 43 H8 2 0.671500 0.504795 -0.293142 11.00000 -1.20000 AFIX 0 C9 1 0.518788 0.443987 -0.308458 11.00000 0.05266 0.05445 = 0.04129 0.01246 0.01579 0.00069 AFIX 43 H9 2 0.487153 0.443702 -0.404890 11.00000 -1.20000 AFIX 0 C10 1 0.453277 0.407134 -0.231901 11.00000 0.03962 0.04629 = 0.03619 0.00388 0.00729 0.00087 AFIX 43 H10 2 0.378258 0.382501 -0.278358 11.00000 -1.20000 AFIX 0 C11 1 0.606950 0.442300 -0.025917 11.00000 0.03150 0.02882 = 0.03899 0.00293 0.00967 0.00347 C12 1 0.650123 0.438637 0.121139 11.00000 0.03430 0.02948 = 0.04098 -0.00011 0.00955 0.00517 C13 1 0.200956 0.273811 -0.069609 11.00000 0.03838 0.03844 = 0.03561 -0.00218 0.00680 -0.00302 C15 1 0.167785 0.217434 0.138615 11.00000 0.08550 0.07576 = 0.04685 0.01506 0.00238 -0.03653 AFIX 23 H15A 2 0.189761 0.182247 0.093512 11.00000 -1.20000 H15B 2 0.063411 0.221135 0.112880 11.00000 -1.20000 AFIX 0 C16 1 0.218114 0.207012 0.292873 11.00000 0.04984 0.03871 = 0.04043 0.00638 0.01245 -0.01419 C17 1 0.162966 0.237745 0.384966 11.00000 0.05810 0.04716 = 0.08704 0.00874 0.03716 -0.00089 AFIX 43 H17 2 0.091440 0.265796 0.351321 11.00000 -1.20000 AFIX 0 C18 1 0.211885 0.227765 0.527297 11.00000 0.12311 0.07018 = 0.07457 -0.02556 0.07301 -0.03997 AFIX 43 H18 2 0.176178 0.249888 0.588465 11.00000 -1.20000 AFIX 0 C19 1 0.313715 0.184741 0.576095 11.00000 0.07858 0.09015 = 0.04344 0.00947 0.00685 -0.05595 C20 1 0.368214 0.154485 0.488392 11.00000 0.05065 0.06962 = 0.06513 0.03381 0.00007 -0.01791 AFIX 43 H20 2 0.438219 0.125843 0.522027 11.00000 -1.20000 AFIX 0 C21 1 0.320646 0.165689 0.347345 11.00000 0.06357 0.04168 = 0.06319 0.00840 0.03333 -0.00702 AFIX 43 H21 2 0.360065 0.144260 0.287757 11.00000 -1.20000 AFIX 0 N1 3 0.577086 0.399697 0.180885 11.00000 0.03312 0.02914 = 0.03362 0.00071 0.00537 0.00282 N2 3 0.496198 0.406694 -0.094353 11.00000 0.03068 0.03231 = 0.03275 0.00170 0.00766 0.00142 N4 3 0.708275 0.102645 0.876127 11.00000 0.06628 0.05256 = 0.04783 0.01915 0.02251 0.02237 O1 4 0.269602 0.315943 -0.109949 11.00000 0.04345 0.04544 = 0.02717 0.00353 0.00014 -0.01010 O2 4 0.108554 0.244688 -0.149609 11.00000 0.05461 0.05647 = 0.03812 -0.00762 0.00039 -0.02081 O3 4 0.358323 0.176970 0.717351 11.00000 0.13227 0.19683 = 0.03677 0.01594 0.00263 -0.10555 AFIX 83 H3C 2 0.421127 0.151516 0.736716 11.00000 -1.50000 AFIX 0 O5 4 0.644539 0.109758 0.753701 11.00000 0.12294 0.09573 = 0.05463 0.00854 0.00187 0.01766 O6 4 0.830412 0.123072 0.915430 11.00000 0.07668 0.14267 = 0.11734 0.04597 -0.00076 -0.00893 O7 4 0.661213 0.076587 0.957370 11.00000 0.15114 0.15914 = 0.12382 0.06555 0.06690 -0.01264 PD1 5 0.422371 0.355530 0.037792 11.00000 0.03134 0.03251 = 0.02703 0.00164 0.00483 -0.00152 MOLE 3 N3 3 0.347469 0.300971 0.163194 11.00000 0.03465 0.04199 = 0.02277 0.00522 0.00441 -0.00107 H3A 2 10.417809 10.277740 10.216201 11.00000 0.05351 H3B 2 10.320797 10.321548 10.222873 11.00000 0.04899 MOLE 4 O4 4 0.532096 0.132999 0.144820 11.00000 0.10579 0.19202 = 0.09716 -0.03949 0.04190 -0.02550 H4A 2 0.568321 0.166196 0.168739 11.00000 -1.50000 H4B 2 0.570495 0.123842 0.082342 11.00000 -1.50000 MOLE 14 PART 1 C14A 1 0.223449 0.267028 0.080457 21.00000 0.09373 0.08441 = 0.02533 0.00490 -0.00014 -0.06322 AFIX 13 H14A 2 0.148938 0.295132 0.088331 21.00000 -1.20000 AFIX 0 MOLE 15 PART 2 C14B 1 0.303946 0.241031 0.077470 -21.00000 0.09373 0.08441 = 0.02533 0.00490 -0.00014 -0.06322 AFIX 13 H14B 2 0.379885 0.213322 0.071271 -21.00000 -1.20000 AFIX 0 HKLF 4 REM rahmiye12_6_0m_a.res in P2(1)/n REM R1 = 0.0635 for 3732 Fo > 4sig(Fo) and 0.0745 for all 4286 data REM 310 parameters refined using 9 restraints END WGHT 0.0000 13.2399 REM Highest difference peak 1.181, deepest hole -0.621, 1-sigma level 0.110 Q1 1 0.2822 0.2516 0.0968 11.00000 0.05 1.18 Q2 1 0.5772 0.0656 0.9584 11.00000 0.05 0.88 Q3 1 0.3732 0.1617 0.7001 11.00000 0.05 0.54 Q4 1 0.5848 0.0762 0.7790 11.00000 0.05 0.48 Q5 1 0.2258 0.2802 0.1114 11.00000 0.05 0.48 ; _shelx_res_checksum 99332 loop_ _space_group_symop_operation_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' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6169(7) 0.3938(3) 0.3171(6) 0.0391(14) Uani 1 1 d . . . . . H1 H 0.5683 0.3670 0.3580 0.047 Uiso 1 1 calc R U . . . C2 C 0.7297(8) 0.4267(3) 0.4013(7) 0.0495(17) Uani 1 1 d . . . . . H2 H 0.7544 0.4222 0.4972 0.059 Uiso 1 1 calc R U . . . C3 C 0.8045(8) 0.4658(3) 0.3430(7) 0.0523(18) Uani 1 1 d . . . . . H3 H 0.8804 0.4874 0.3993 0.063 Uiso 1 1 calc R U . . . C4 C 0.7663(7) 0.4731(3) 0.1985(7) 0.0434(15) Uani 1 1 d . . . . . C5 C 0.8360(8) 0.5114(3) 0.1242(9) 0.0587(19) Uani 1 1 d . . . . . H5 H 0.9134 0.5342 0.1737 0.070 Uiso 1 1 calc R U . . . C6 C 0.7934(8) 0.5156(3) -0.0147(9) 0.0570(19) Uani 1 1 d . . . . . H6 H 0.8403 0.5418 -0.0587 0.068 Uiso 1 1 calc R U . . . C7 C 0.6775(7) 0.4806(3) -0.0965(7) 0.0434(15) Uani 1 1 d . . . . . C8 C 0.6286(8) 0.4802(3) -0.2420(7) 0.0514(17) Uani 1 1 d . . . . . H8 H 0.6715 0.5048 -0.2931 0.062 Uiso 1 1 calc R U . . . C9 C 0.5188(8) 0.4440(3) -0.3085(7) 0.0489(16) Uani 1 1 d . . . . . H9 H 0.4872 0.4437 -0.4049 0.059 Uiso 1 1 calc R U . . . C10 C 0.4533(7) 0.4071(3) -0.2319(6) 0.0414(14) Uani 1 1 d . . . . . H10 H 0.3783 0.3825 -0.2784 0.050 Uiso 1 1 calc R U . . . C11 C 0.6070(6) 0.4423(2) -0.0259(6) 0.0331(12) Uani 1 1 d . . . . . C12 C 0.6501(6) 0.4386(3) 0.1211(6) 0.0351(13) Uani 1 1 d . . . . . C13 C 0.2010(7) 0.2738(3) -0.0696(6) 0.0382(13) Uani 1 1 d . . . . . C15 C 0.1678(10) 0.2174(4) 0.1386(8) 0.073(3) Uani 1 1 d . . . . . H15A H 0.1898 0.1822 0.0935 0.087 Uiso 1 1 calc DR U . A 1 H15B H 0.0634 0.2211 0.1129 0.087 Uiso 1 1 calc DR U . A 1 C16 C 0.2181(7) 0.2070(3) 0.2929(7) 0.0430(15) Uani 1 1 d . . . . . C17 C 0.1630(8) 0.2377(3) 0.3850(9) 0.061(2) Uani 1 1 d . . . . . H17 H 0.0914 0.2658 0.3513 0.073 Uiso 1 1 calc R U . . . C18 C 0.2119(12) 0.2278(4) 0.5273(10) 0.080(3) Uani 1 1 d . . . . . H18 H 0.1762 0.2499 0.5885 0.096 Uiso 1 1 calc R U . . . C19 C 0.3137(11) 0.1847(5) 0.5761(8) 0.073(3) Uani 1 1 d . . . . . C20 C 0.3682(8) 0.1545(4) 0.4884(9) 0.065(2) Uani 1 1 d . . . . . H20 H 0.4382 0.1258 0.5220 0.078 Uiso 1 1 calc R U . . . C21 C 0.3206(8) 0.1657(3) 0.3473(8) 0.0530(18) Uani 1 1 d . . . . . H21 H 0.3601 0.1443 0.2878 0.064 Uiso 1 1 calc R U . . . N1 N 0.5771(5) 0.3997(2) 0.1809(5) 0.0327(10) Uani 1 1 d . . . . . N2 N 0.4962(5) 0.4067(2) -0.0944(5) 0.0322(10) Uani 1 1 d . . . . . N4 N 0.7083(8) 0.1026(3) 0.8761(6) 0.0542(16) Uani 1 1 d . . . . . O1 O 0.2696(5) 0.31594(19) -0.1099(4) 0.0406(10) Uani 1 1 d . . . . . O2 O 0.1086(5) 0.2447(2) -0.1496(5) 0.0523(12) Uani 1 1 d . . . . . O3 O 0.3583(9) 0.1770(4) 0.7174(6) 0.126(4) Uani 1 1 d . . . . . H3C H 0.4211 0.1515 0.7367 0.189 Uiso 1 1 calc R U . . . O5 O 0.6445(8) 0.1098(3) 0.7537(6) 0.096(2) Uani 1 1 d . . . . . O6 O 0.8304(8) 0.1231(4) 0.9154(9) 0.118(3) Uani 1 1 d . . . . . O7 O 0.6612(10) 0.0766(4) 0.9574(9) 0.139(4) Uani 1 1 d . . . . . Pd1 Pd 0.42237(5) 0.35553(2) 0.03779(4) 0.03096(14) Uani 1 1 d . . . . . N3 N 0.3475(5) 0.3010(2) 0.1632(5) 0.0339(11) Uani 1 1 d . . . . . H3A H 0.4178 0.2777 0.2162 0.05(2) Uiso 1 1 d D . . . . H3B H 0.3208 0.3215 0.2229 0.05(2) Uiso 1 1 d D . . . . O4 O 0.5321(10) 0.1330(5) 0.1448(9) 0.129(3) Uani 1 1 d D . . . . H4A H 0.568(6) 0.1662(13) 0.169(12) 0.193 Uiso 1 1 d D U . . . H4B H 0.570(15) 0.124(6) 0.082(12) 0.193 Uiso 1 1 d D U . . . C14A C 0.2234(16) 0.2670(6) 0.0805(10) 0.071(5) Uani 0.75(2) 1 d . . P B 1 H14A H 0.1489 0.2951 0.0883 0.085 Uiso 0.75(2) 1 calc DR U P B 1 C14B C 0.304(3) 0.2410(14) 0.077(3) 0.071(5) Uani 0.25(2) 1 d . . P B 2 H14B H 0.3799 0.2133 0.0713 0.085 Uiso 0.25(2) 1 calc DR U P 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 C1 0.043(3) 0.036(3) 0.035(3) 0.003(3) 0.004(3) 0.003(3) C2 0.053(4) 0.056(4) 0.032(3) -0.007(3) -0.001(3) 0.003(3) C3 0.046(4) 0.053(4) 0.048(4) -0.015(3) -0.001(3) -0.007(3) C4 0.036(3) 0.038(3) 0.053(4) -0.003(3) 0.006(3) 0.003(3) C5 0.047(4) 0.054(4) 0.070(5) -0.002(4) 0.010(4) -0.018(3) C6 0.052(4) 0.048(4) 0.075(5) 0.008(4) 0.022(4) -0.016(3) C7 0.042(3) 0.037(3) 0.055(4) 0.011(3) 0.019(3) 0.002(3) C8 0.059(4) 0.047(4) 0.055(4) 0.017(3) 0.026(4) 0.004(3) C9 0.053(4) 0.054(4) 0.041(4) 0.012(3) 0.016(3) 0.001(3) C10 0.040(3) 0.046(4) 0.036(3) 0.004(3) 0.007(3) 0.001(3) C11 0.032(3) 0.029(3) 0.039(3) 0.003(2) 0.010(3) 0.003(2) C12 0.034(3) 0.029(3) 0.041(3) 0.000(2) 0.010(3) 0.005(2) C13 0.038(3) 0.038(3) 0.036(3) -0.002(3) 0.007(3) -0.003(3) C15 0.086(6) 0.076(6) 0.047(4) 0.015(4) 0.002(4) -0.037(5) C16 0.050(4) 0.039(3) 0.040(3) 0.006(3) 0.012(3) -0.014(3) C17 0.058(5) 0.047(4) 0.087(6) 0.009(4) 0.037(4) -0.001(4) C18 0.123(8) 0.070(6) 0.075(6) -0.026(5) 0.073(6) -0.040(6) C19 0.079(6) 0.090(7) 0.043(4) 0.009(4) 0.007(4) -0.056(5) C20 0.051(4) 0.070(5) 0.065(5) 0.034(4) 0.000(4) -0.018(4) C21 0.064(5) 0.042(4) 0.063(5) 0.008(3) 0.033(4) -0.007(3) N1 0.033(3) 0.029(2) 0.034(3) 0.001(2) 0.005(2) 0.003(2) N2 0.031(2) 0.032(2) 0.033(3) 0.002(2) 0.008(2) 0.001(2) N4 0.066(4) 0.053(4) 0.048(4) 0.019(3) 0.023(3) 0.022(3) O1 0.043(2) 0.045(2) 0.027(2) 0.0035(18) 0.0001(18) -0.010(2) O2 0.055(3) 0.056(3) 0.038(2) -0.008(2) 0.000(2) -0.021(2) O3 0.132(6) 0.197(9) 0.037(3) 0.016(4) 0.003(4) -0.106(6) O5 0.123(6) 0.096(5) 0.055(4) 0.009(3) 0.002(4) 0.018(4) O6 0.077(5) 0.143(7) 0.117(6) 0.046(5) -0.001(5) -0.009(5) O7 0.151(8) 0.159(8) 0.124(7) 0.066(6) 0.067(6) -0.013(7) Pd1 0.0313(2) 0.0325(2) 0.0270(2) 0.00164(18) 0.00483(17) -0.00152(19) N3 0.035(3) 0.042(3) 0.023(2) 0.005(2) 0.004(2) -0.001(2) O4 0.106(6) 0.192(10) 0.097(6) -0.039(6) 0.042(5) -0.026(6) C14A 0.094(11) 0.084(10) 0.025(4) 0.005(5) 0.000(6) -0.063(8) C14B 0.094(11) 0.084(10) 0.025(4) 0.005(5) 0.000(6) -0.063(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N1 C1 C2 121.8(6) N1 C1 H1 119.1 C2 C1 H1 119.1 C3 C2 C1 120.1(6) C3 C2 H2 120.0 C1 C2 H2 120.0 C2 C3 C4 120.0(6) C2 C3 H3 120.0 C4 C3 H3 120.0 C3 C4 C12 116.3(6) C3 C4 C5 125.8(6) C12 C4 C5 117.8(6) C6 C5 C4 122.2(7) C6 C5 H5 118.9 C4 C5 H5 118.9 C5 C6 C7 121.4(6) C5 C6 H6 119.3 C7 C6 H6 119.3 C8 C7 C11 116.7(6) C8 C7 C6 125.7(6) C11 C7 C6 117.6(6) C9 C8 C7 120.3(6) C9 C8 H8 119.9 C7 C8 H8 119.9 C8 C9 C10 120.0(6) C8 C9 H9 120.0 C10 C9 H9 120.0 N2 C10 C9 121.2(6) N2 C10 H10 119.4 C9 C10 H10 119.4 N2 C11 C7 122.2(5) N2 C11 C12 116.8(5) C7 C11 C12 121.0(6) N1 C12 C4 123.0(6) N1 C12 C11 117.1(5) C4 C12 C11 119.9(6) O2 C13 O1 122.8(6) O2 C13 C14A 119.5(6) O1 C13 C14A 117.2(6) O2 C13 C14B 118.5(8) O1 C13 C14B 111.7(8) C14A C15 C16 119.3(7) C16 C15 C14B 111.3(13) C14A C15 H15A 107.5 C16 C15 H15A 107.5 C14A C15 H15B 107.5 C16 C15 H15B 107.5 H15A C15 H15B 107.0 C21 C16 C17 116.9(7) C21 C16 C15 120.7(7) C17 C16 C15 122.4(7) C16 C17 C18 121.5(8) C16 C17 H17 119.3 C18 C17 H17 119.3 C19 C18 C17 119.0(8) C19 C18 H18 120.5 C17 C18 H18 120.5 C20 C19 O3 123.2(11) C20 C19 C18 120.3(8) O3 C19 C18 116.5(11) C19 C20 C21 120.0(8) C19 C20 H20 120.0 C21 C20 H20 120.0 C16 C21 C20 122.2(7) C16 C21 H21 118.9 C20 C21 H21 118.9 C1 N1 C12 118.9(5) C1 N1 Pd1 129.0(4) C12 N1 Pd1 112.1(4) C10 N2 C11 119.6(5) C10 N2 Pd1 128.2(4) C11 N2 Pd1 112.2(4) O7 N4 O5 124.9(9) O7 N4 O6 118.8(8) O5 N4 O6 116.3(7) C13 O1 Pd1 116.0(4) C19 O3 H3C 109.5 O1 Pd1 N1 176.79(18) O1 Pd1 N2 95.32(18) N1 Pd1 N2 81.80(19) O1 Pd1 N3 82.50(18) N1 Pd1 N3 100.42(19) N2 Pd1 N3 177.15(19) C14A N3 Pd1 110.0(5) C14B N3 Pd1 105.6(10) C14A N3 H3A 112.6(7) C14B N3 H3A 82.1(15) Pd1 N3 H3A 112.0 C14A N3 H3B 109.1(8) C14B N3 H3B 139.2(9) Pd1 N3 H3B 109.0 H3A N3 H3B 103.0 H4A O4 H4B 102(3) C15 C14A C13 122.2(7) C15 C14A N3 121.2(7) C13 C14A N3 112.9(7) C15 C14A H14A 96.4 C13 C14A H14A 96.4 N3 C14A H14A 96.4 N3 C14B C15 100.9(12) N3 C14B C13 96(2) C15 C14B C13 97.4(17) N3 C14B H14B 119.4 C15 C14B H14B 119.4 C13 C14B H14B 119.4 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N1 1.320(7) C1 C2 1.394(9) C1 H1 0.9300 C2 C3 1.372(10) C2 H2 0.9300 C3 C4 1.403(9) C3 H3 0.9300 C4 C12 1.408(8) C4 C5 1.429(10) C5 C6 1.342(11) C5 H5 0.9300 C6 C7 1.429(10) C6 H6 0.9300 C7 C8 1.404(10) C7 C11 1.409(8) C8 C9 1.359(10) C8 H8 0.9300 C9 C10 1.399(9) C9 H9 0.9300 C10 N2 1.326(7) C10 H10 0.9300 C11 N2 1.362(7) C11 C12 1.420(8) C12 N1 1.368(7) C13 O2 1.215(7) C13 O1 1.290(7) C13 C14A 1.468(11) C13 C14B 1.70(4) C15 C14A 1.439(10) C15 C16 1.506(9) C15 C14B 1.683(19) C15 H15A 0.9700 C15 H15B 0.9700 C16 C21 1.362(10) C16 C17 1.377(10) C17 C18 1.392(12) C17 H17 0.9300 C18 C19 1.374(14) C18 H18 0.9300 C19 C20 1.334(13) C19 O3 1.373(9) C20 C21 1.384(10) C20 H20 0.9300 C21 H21 0.9300 N1 Pd1 2.024(5) N2 Pd1 2.034(5) N4 O7 1.194(8) N4 O5 1.221(8) N4 O6 1.224(9) O1 Pd1 1.989(4) O3 H3C 0.8200 Pd1 N3 2.036(5) N3 C14A 1.469(9) N3 C14B 1.60(2) N3 H3A 0.91 N3 H3B 0.85 O4 H4A 0.84(2) O4 H4B 0.84(2) C14A H14A 0.9800 C14B H14B 0.9800 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 C1 H1 O2 0.93 2.57 3.165(8) 122.3 4_666 C1 H1 O6 0.93 2.52 3.203(11) 130.0 4_565 C9 H9 O6 0.93 2.51 3.238(10) 135.1 4_564 O3 H3C O5 0.82 2.31 3.084(12) 156.3 . N3 H3A O2 0.91 2.02 2.881(6) 158.9(3) 4_666 N3 H3B O5 0.85 2.39 3.122(9) 144.3(3) 4_565 N3 H3B O6 0.85 2.28 3.104(9) 160.9(4) 4_565 O4 H4B O7 0.84(2) 2.02(5) 2.834(13) 162(14) 1_554 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion N1 C1 C2 C3 -1.2(10) C1 C2 C3 C4 0.7(11) C2 C3 C4 C12 0.0(10) C2 C3 C4 C5 -179.1(7) C3 C4 C5 C6 179.5(7) C12 C4 C5 C6 0.5(11) C4 C5 C6 C7 -1.5(12) C5 C6 C7 C8 -177.6(7) C5 C6 C7 C11 1.3(11) C11 C7 C8 C9 -0.2(10) C6 C7 C8 C9 178.7(7) C7 C8 C9 C10 0.4(11) C8 C9 C10 N2 0.0(10) C8 C7 C11 N2 -0.3(9) C6 C7 C11 N2 -179.3(6) C8 C7 C11 C12 178.8(6) C6 C7 C11 C12 -0.2(9) C3 C4 C12 N1 -0.3(9) C5 C4 C12 N1 178.8(6) C3 C4 C12 C11 -178.5(6) C5 C4 C12 C11 0.7(9) N2 C11 C12 N1 0.1(8) C7 C11 C12 N1 -179.1(5) N2 C11 C12 C4 178.4(5) C7 C11 C12 C4 -0.8(9) C14A C15 C16 C21 -100.8(12) C14B C15 C16 C21 -62.3(14) C14A C15 C16 C17 79.9(13) C14B C15 C16 C17 118.4(14) C21 C16 C17 C18 1.2(10) C15 C16 C17 C18 -179.5(7) C16 C17 C18 C19 -2.4(12) C17 C18 C19 C20 2.3(12) C17 C18 C19 O3 179.8(7) O3 C19 C20 C21 -178.4(7) C18 C19 C20 C21 -1.0(12) C17 C16 C21 C20 0.1(10) C15 C16 C21 C20 -179.2(6) C19 C20 C21 C16 -0.2(11) C2 C1 N1 C12 0.9(9) C2 C1 N1 Pd1 177.9(5) C4 C12 N1 C1 -0.1(8) C11 C12 N1 C1 178.1(5) C4 C12 N1 Pd1 -177.6(5) C11 C12 N1 Pd1 0.6(6) C9 C10 N2 C11 -0.6(9) C9 C10 N2 Pd1 -177.9(5) C7 C11 N2 C10 0.8(8) C12 C11 N2 C10 -178.4(5) C7 C11 N2 Pd1 178.4(4) C12 C11 N2 Pd1 -0.8(6) O2 C13 O1 Pd1 -177.5(5) C14A C13 O1 Pd1 11.0(11) C14B C13 O1 Pd1 -27.3(10) C16 C15 C14A C13 168.3(11) C14B C15 C14A C13 82(3) C16 C15 C14A N3 12(2) C14B C15 C14A N3 -74.4(17) O2 C13 C14A C15 16.2(19) O1 C13 C14A C15 -171.9(11) C14B C13 C14A C15 -82.4(18) O2 C13 C14A N3 174.6(9) O1 C13 C14A N3 -13.5(16) C14B C13 C14A N3 76.0(17) C14B N3 C14A C15 78(2) Pd1 N3 C14A C15 167.9(12) C14B N3 C14A C13 -80(3) Pd1 N3 C14A C13 9.2(15) C14A N3 C14B C15 -46.8(10) Pd1 N3 C14B C15 -149.5(14) C14A N3 C14B C13 52(2) Pd1 N3 C14B C13 -50.8(11) C14A C15 C14B N3 50.3(12) C16 C15 C14B N3 -61(2) C14A C15 C14B C13 -46.8(18) C16 C15 C14B C13 -157.8(8) O2 C13 C14B N3 -157.0(7) O1 C13 C14B N3 51.4(12) C14A C13 C14B N3 -55.5(12) O2 C13 C14B C15 -55.2(14) O1 C13 C14B C15 153.2(8) C14A C13 C14B C15 46.3(10)