#------------------------------------------------------------------------------ #$Date: 2021-10-14 02:13:55 +0300 (Thu, 14 Oct 2021) $ #$Revision: 269927 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708554.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_7708554 loop_ _publ_author_name 'Paderni, Daniele' 'Giorgi , Luca' 'Macedi, Eleonora' 'Formica, Mauro' 'Paoli, Paola' 'Rossi, Patrizia' 'Fusi, Vieri' _publ_section_title ; A selective fluorescent probe for GadoliniumIII in water based on a PdII -preorganized chromone-receptor ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT01753E _journal_year 2021 _chemical_formula_sum 'C24 H34 N2 O12 Pd' _chemical_formula_weight 648.93 _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' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-05-27 deposited with the CCDC. 2021-10-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.880(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.8990(5) _cell_length_b 9.2755(5) _cell_length_c 20.2093(19) _cell_measurement_reflns_used 6400 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 72.2660 _cell_measurement_theta_min 4.4320 _cell_volume 2558.6(3) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'PARST97 (Nardelli, 1995)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SIR-2004, (Burla, 2005)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.1241 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Onyx' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.1034 _diffrn_reflns_av_unetI/netI 0.0782 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 19062 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.480 _diffrn_reflns_theta_min 4.264 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 6.468 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.28586 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.685 _exptl_crystal_description prism _exptl_crystal_F_000 1336 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _refine_diff_density_max 0.943 _refine_diff_density_min -1.541 _refine_diff_density_rms 0.144 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 388 _refine_ls_number_reflns 5059 _refine_ls_number_restraints 18 _refine_ls_restrained_S_all 1.061 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_gt 0.0606 _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^)+(0.0593P)^2^+10.0468P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1317 _refine_ls_wR_factor_ref 0.1498 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3738 _reflns_number_total 5059 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01753e2.cif _cod_data_source_block '[Pd(H-2L2)](H2O)6' _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7708554 _shelx_shelxl_version_number 2018/3 _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. ; _shelx_res_file ; TITL SIR2014 run in space group P 21/n shelx.res created by SHELXL-2018/3 at 10:52:53 on 02-Jun-2020 CELL 1.54184 13.8990 9.2755 20.2093 90.000 100.880 90.000 ZERR 4.00 0.0005 0.0005 0.0019 0.000 0.005 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O PD UNIT 96 136 8 48 4 MERG 2 dfix 0.84 0.01 h1w1 o1w h1w2 o1w dfix 0.84 0.01 h2w1 o2w h2w2 o2w dfix 0.84 0.01 h3w1 o3w h3w2 o3w dfix 0.84 0.01 h4w1 o4w h4w2 o4w dfix 0.84 0.01 h5w1 o5w h5w2 o5w dfix 0.84 0.01 h6w1 o6w h6w2 o6w dang 1.24 0.01 h1w1 h1w2 dang 1.24 0.01 h2w1 h2w2 dang 1.24 0.01 h3w1 h3w2 dang 1.24 0.01 h4w1 h4w2 dang 1.24 0.01 h5w1 h5w2 dang 1.24 0.01 h6w1 h6w2 ACTA L.S. 300 TEMP -173.00 WGHT 0.059300 10.046800 FVAR 2.34727 PD1 5 0.363927 0.181199 0.692051 11.00000 0.03023 0.01798 = 0.01287 -0.00007 -0.00538 -0.00100 O1 4 0.424767 0.255739 0.783568 11.00000 0.03864 0.02200 = 0.01507 0.00011 -0.00393 -0.00327 O2 4 0.345923 0.015869 0.906691 11.00000 0.04072 0.01915 = 0.01447 0.00065 0.00019 -0.00279 O3 4 0.484666 0.401081 0.897428 11.00000 0.04958 0.02577 = 0.01900 -0.00108 -0.00882 -0.00745 O4 4 0.388384 0.377205 0.655667 11.00000 0.03471 0.01944 = 0.01418 -0.00194 -0.00427 -0.00702 O5 4 0.359049 0.336463 0.473783 11.00000 0.03915 0.02220 = 0.01139 -0.00118 -0.00438 -0.00163 O6 4 0.420241 0.649591 0.617366 11.00000 0.04660 0.01903 = 0.02070 0.00070 0.00026 0.00114 N1 3 0.345297 -0.018264 0.729974 11.00000 0.02365 0.02116 = 0.01356 0.00209 -0.00333 -0.00212 N2 3 0.301766 0.102389 0.600013 11.00000 0.03145 0.01634 = 0.01491 0.00119 -0.00199 0.00052 C1 1 0.278929 -0.098051 0.674850 11.00000 0.04287 0.01697 = 0.01888 0.00001 -0.00536 -0.00231 AFIX 23 H1A 2 0.286686 -0.203216 0.682378 11.00000 -1.20000 H1B 2 0.209863 -0.072479 0.675165 11.00000 -1.20000 AFIX 0 C2 1 0.300708 -0.014087 0.789808 11.00000 0.03207 0.02621 = 0.01693 -0.00154 -0.00305 -0.00694 AFIX 23 H2A 2 0.294313 -0.113840 0.805858 11.00000 -1.20000 H2B 2 0.234005 0.027049 0.777448 11.00000 -1.20000 AFIX 0 C3 1 0.358750 0.073664 0.846304 11.00000 0.03730 0.02014 = 0.01815 -0.00197 -0.00185 0.00081 C4 1 0.407641 0.197620 0.840695 11.00000 0.03234 0.02101 = 0.01374 -0.00121 -0.00512 0.00352 C5 1 0.445527 0.282519 0.901769 11.00000 0.03348 0.01952 = 0.01841 -0.00758 -0.00823 -0.00013 C6 1 0.427326 0.222170 0.964465 11.00000 0.02846 0.01819 = 0.01738 -0.00118 -0.00545 0.00722 C7 1 0.454048 0.294329 1.026150 11.00000 0.02909 0.02126 = 0.02069 0.00005 -0.00496 -0.00228 AFIX 43 H7 2 0.485424 0.385528 1.027281 11.00000 -1.20000 AFIX 0 C8 1 0.435838 0.236012 1.084816 11.00000 0.03572 0.03565 = 0.01695 -0.00596 -0.00410 -0.00157 AFIX 43 H8 2 0.453177 0.287446 1.125994 11.00000 -1.20000 AFIX 0 C9 1 0.391560 0.100272 1.083834 11.00000 0.02984 0.04239 = 0.01331 0.00168 -0.00520 -0.00089 AFIX 43 H9 2 0.381256 0.058482 1.124846 11.00000 -1.20000 AFIX 0 C10 1 0.362849 0.026769 1.024518 11.00000 0.03575 0.02612 = 0.02176 0.00341 -0.00399 -0.00526 AFIX 43 H10 2 0.331552 -0.064420 1.023810 11.00000 -1.20000 AFIX 0 C11 1 0.380834 0.089535 0.965020 11.00000 0.03628 0.01989 = 0.01603 -0.00427 -0.00652 0.00055 C12 1 0.443529 -0.092419 0.745886 11.00000 0.03914 0.02570 = 0.02304 -0.00319 -0.00699 0.00608 AFIX 33 H12A 2 0.472800 -0.094638 0.705418 11.00000 -1.50000 H12B 2 0.486748 -0.039567 0.781681 11.00000 -1.50000 H12C 2 0.434866 -0.191233 0.760899 11.00000 -1.50000 AFIX 0 C13 1 0.303935 -0.059219 0.608096 11.00000 0.03353 0.02303 = 0.01910 0.00400 -0.00500 -0.00196 AFIX 23 H13A 2 0.256124 -0.103948 0.571302 11.00000 -1.20000 H13B 2 0.369952 -0.096181 0.605535 11.00000 -1.20000 AFIX 0 C14 1 0.360865 0.143578 0.549439 11.00000 0.03832 0.01764 = 0.01746 -0.00151 -0.00071 0.00397 AFIX 23 H14A 2 0.331916 0.099655 0.505542 11.00000 -1.20000 H14B 2 0.428058 0.104987 0.563315 11.00000 -1.20000 AFIX 0 C15 1 0.365930 0.304183 0.541209 11.00000 0.03154 0.02188 = 0.01625 0.00482 -0.00508 -0.00250 C16 1 0.383496 0.405832 0.590580 11.00000 0.03322 0.02514 = 0.01604 -0.00117 -0.00599 0.00026 C17 1 0.397710 0.555782 0.573471 11.00000 0.03170 0.01892 = 0.02151 -0.00015 -0.00435 -0.00096 C18 1 0.387465 0.586366 0.501223 11.00000 0.02323 0.02207 = 0.01875 -0.00020 -0.00509 0.00128 C19 1 0.396797 0.726551 0.476612 11.00000 0.03002 0.02527 = 0.02037 0.00173 -0.00404 0.00401 AFIX 43 H19 2 0.411340 0.804414 0.507416 11.00000 -1.20000 AFIX 0 C20 1 0.385187 0.752265 0.408806 11.00000 0.03156 0.02520 = 0.02652 0.00358 -0.00481 -0.00191 AFIX 43 H20 2 0.389582 0.847793 0.392685 11.00000 -1.20000 AFIX 0 C21 1 0.366829 0.637193 0.363419 11.00000 0.03219 0.03455 = 0.01658 0.00612 -0.00353 0.00364 AFIX 43 H21 2 0.360363 0.654852 0.316482 11.00000 -1.20000 AFIX 0 C22 1 0.358130 0.500315 0.385726 11.00000 0.03543 0.02821 = 0.01231 0.00154 -0.00606 0.00175 AFIX 43 H22 2 0.344973 0.422729 0.354646 11.00000 -1.20000 AFIX 0 C23 1 0.368665 0.475460 0.454162 11.00000 0.02991 0.02217 = 0.01805 0.00450 -0.00374 -0.00189 C24 1 0.197642 0.151290 0.578632 11.00000 0.02846 0.02874 = 0.02211 -0.00104 -0.00917 -0.00210 AFIX 33 H24A 2 0.159762 0.122961 0.612802 11.00000 -1.50000 H24B 2 0.195962 0.256408 0.573666 11.00000 -1.50000 H24C 2 0.169188 0.106444 0.535459 11.00000 -1.50000 AFIX 0 O1W 4 0.632635 1.222555 0.808700 11.00000 0.03555 0.05071 = 0.05099 -0.00251 -0.00129 -0.00067 H1W1 2 0.639183 1.148667 0.785886 11.00000 -1.20000 H1W2 2 0.571206 1.225118 0.797653 11.00000 -1.20000 O2W 4 0.477537 0.556066 0.767117 11.00000 0.05022 0.02362 = 0.02122 -0.00015 -0.00206 -0.00706 H2W1 2 0.470091 0.526644 0.727451 11.00000 -1.20000 H2W2 2 0.485642 0.474859 0.785168 11.00000 -1.20000 O3W 4 0.760118 0.923175 0.605277 11.00000 0.05423 0.04169 = 0.03057 -0.00340 -0.00672 -0.00083 H3W1 2 0.784675 0.991882 0.629861 11.00000 -1.20000 H3W2 2 0.800197 0.861158 0.624167 11.00000 -1.20000 O4W 4 0.672922 0.953705 0.749483 11.00000 0.04362 0.05380 = 0.04109 -0.01512 -0.00151 -0.00327 H4W1 2 0.708057 0.991464 0.724117 11.00000 -1.20000 H4W2 2 0.637022 0.909012 0.717722 11.00000 -1.20000 O5W 4 0.673715 0.628691 0.781136 11.00000 0.04216 0.04663 = 0.03377 -0.00136 0.00104 0.00176 H5W1 2 0.612335 0.616516 0.775824 11.00000 -1.20000 H5W2 2 0.668123 0.712757 0.764149 11.00000 -1.20000 O6W 4 0.563154 0.884029 0.619268 11.00000 0.04126 0.03628 = 0.04525 -0.00672 0.00046 0.00398 H6W1 2 0.545279 0.796826 0.615540 11.00000 -1.20000 H6W2 2 0.620026 0.867502 0.612207 11.00000 -1.20000 HKLF 4 REM SIR2014 run in space group P 21/n REM wR2 = 0.1498, GooF = S = 1.063, Restrained GooF = 1.061 for all data REM R1 = 0.0606 for 3738 Fo > 4sig(Fo) and 0.0926 for all 5059 data REM 388 parameters refined using 18 restraints END WGHT 0.0593 10.0468 REM Highest difference peak 0.943, deepest hole -1.541, 1-sigma level 0.144 Q1 1 0.3063 0.2445 0.7035 11.00000 0.05 0.94 Q2 1 0.3818 0.0385 0.7114 11.00000 0.05 0.93 Q3 1 0.3101 0.1198 0.6983 11.00000 0.05 0.91 Q4 1 0.4202 0.1166 0.6810 11.00000 0.05 0.90 Q5 1 0.4630 0.1760 0.7028 11.00000 0.05 0.87 Q6 1 0.4307 0.2467 0.6741 11.00000 0.05 0.84 Q7 1 0.3433 0.3191 0.6703 11.00000 0.05 0.82 Q8 1 0.2649 0.1789 0.6838 11.00000 0.05 0.82 Q9 1 0.3678 0.4399 0.6927 11.00000 0.05 0.81 Q10 1 0.4322 0.0946 0.6718 11.00000 0.05 0.78 Q11 1 0.6433 0.7138 0.7591 11.00000 0.05 0.76 Q12 1 0.3843 0.3195 0.7107 11.00000 0.05 0.69 Q13 1 0.6832 0.9929 0.7008 11.00000 0.05 0.63 Q14 1 0.4788 0.2973 0.7749 11.00000 0.05 0.57 Q15 1 0.4972 0.0916 0.6807 11.00000 0.05 0.55 Q16 1 0.1991 0.0235 0.7280 11.00000 0.05 0.52 Q17 1 0.2791 -0.2395 0.8093 11.00000 0.05 0.50 Q18 1 0.2410 0.3147 0.6209 11.00000 0.05 0.47 Q19 1 0.4217 0.1851 0.8096 11.00000 0.05 0.46 Q20 1 0.3959 0.5699 0.5370 11.00000 0.05 0.46 ; _shelx_res_checksum 50276 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 Pd1 Pd 0.36393(4) 0.18120(5) 0.69205(2) 0.02159(16) Uani 1 1 d . . . . . O1 O 0.4248(3) 0.2557(4) 0.7836(2) 0.0264(10) Uani 1 1 d . . . . . O2 O 0.3459(3) 0.0159(4) 0.9067(2) 0.0254(10) Uani 1 1 d . . . . . O3 O 0.4847(4) 0.4011(5) 0.8974(2) 0.0334(12) Uani 1 1 d . . . . . O4 O 0.3884(3) 0.3772(4) 0.6557(2) 0.0239(10) Uani 1 1 d . . . . . O5 O 0.3590(3) 0.3365(4) 0.4738(2) 0.0254(10) Uani 1 1 d . . . . . O6 O 0.4202(4) 0.6496(4) 0.6174(2) 0.0296(11) Uani 1 1 d . . . . . N1 N 0.3453(4) -0.0183(5) 0.7300(2) 0.0203(11) Uani 1 1 d . . . . . N2 N 0.3018(4) 0.1024(5) 0.6000(2) 0.0217(12) Uani 1 1 d . . . . . C1 C 0.2789(5) -0.0981(6) 0.6748(3) 0.0277(16) Uani 1 1 d . . . . . H1A H 0.286686 -0.203216 0.682378 0.033 Uiso 1 1 calc R U . . . H1B H 0.209863 -0.072479 0.675165 0.033 Uiso 1 1 calc R U . . . C2 C 0.3007(5) -0.0141(7) 0.7898(3) 0.0261(15) Uani 1 1 d . . . . . H2A H 0.294313 -0.113840 0.805858 0.031 Uiso 1 1 calc R U . . . H2B H 0.234005 0.027049 0.777448 0.031 Uiso 1 1 calc R U . . . C3 C 0.3587(5) 0.0737(7) 0.8463(3) 0.0261(15) Uani 1 1 d . . . . . C4 C 0.4076(5) 0.1976(6) 0.8407(3) 0.0236(14) Uani 1 1 d . . . . . C5 C 0.4455(5) 0.2825(6) 0.9018(3) 0.0255(15) Uani 1 1 d . . . . . C6 C 0.4273(5) 0.2222(6) 0.9645(3) 0.0226(14) Uani 1 1 d . . . . . C7 C 0.4540(5) 0.2943(7) 1.0262(3) 0.0249(14) Uani 1 1 d . . . . . H7 H 0.485424 0.385528 1.027281 0.030 Uiso 1 1 calc R U . . . C8 C 0.4358(5) 0.2360(7) 1.0848(3) 0.0306(16) Uani 1 1 d . . . . . H8 H 0.453177 0.287446 1.125994 0.037 Uiso 1 1 calc R U . . . C9 C 0.3916(5) 0.1003(8) 1.0838(3) 0.0297(16) Uani 1 1 d . . . . . H9 H 0.381256 0.058482 1.124846 0.036 Uiso 1 1 calc R U . . . C10 C 0.3628(5) 0.0268(7) 1.0245(3) 0.0291(16) Uani 1 1 d . . . . . H10 H 0.331552 -0.064420 1.023810 0.035 Uiso 1 1 calc R U . . . C11 C 0.3808(5) 0.0895(6) 0.9650(3) 0.0256(15) Uani 1 1 d . . . . . C12 C 0.4435(5) -0.0924(7) 0.7459(3) 0.0310(16) Uani 1 1 d . . . . . H12A H 0.472800 -0.094638 0.705418 0.046 Uiso 1 1 calc R U . . . H12B H 0.486748 -0.039567 0.781681 0.046 Uiso 1 1 calc R U . . . H12C H 0.434866 -0.191233 0.760899 0.046 Uiso 1 1 calc R U . . . C13 C 0.3039(5) -0.0592(7) 0.6081(3) 0.0265(15) Uani 1 1 d . . . . . H13A H 0.256124 -0.103948 0.571302 0.032 Uiso 1 1 calc R U . . . H13B H 0.369952 -0.096181 0.605535 0.032 Uiso 1 1 calc R U . . . C14 C 0.3609(5) 0.1436(6) 0.5494(3) 0.0253(15) Uani 1 1 d . . . . . H14A H 0.331916 0.099655 0.505542 0.030 Uiso 1 1 calc R U . . . H14B H 0.428058 0.104987 0.563315 0.030 Uiso 1 1 calc R U . . . C15 C 0.3659(5) 0.3042(7) 0.5412(3) 0.0245(14) Uani 1 1 d . . . . . C16 C 0.3835(5) 0.4058(7) 0.5906(3) 0.0262(15) Uani 1 1 d . . . . . C17 C 0.3977(5) 0.5558(6) 0.5735(3) 0.0253(15) Uani 1 1 d . . . . . C18 C 0.3875(5) 0.5864(6) 0.5012(3) 0.0225(14) Uani 1 1 d . . . . . C19 C 0.3968(5) 0.7266(7) 0.4766(3) 0.0264(15) Uani 1 1 d . . . . . H19 H 0.411340 0.804414 0.507416 0.032 Uiso 1 1 calc R U . . . C20 C 0.3852(5) 0.7523(7) 0.4088(3) 0.0291(16) Uani 1 1 d . . . . . H20 H 0.389582 0.847793 0.392685 0.035 Uiso 1 1 calc R U . . . C21 C 0.3668(5) 0.6372(7) 0.3634(3) 0.0288(16) Uani 1 1 d . . . . . H21 H 0.360363 0.654852 0.316482 0.035 Uiso 1 1 calc R U . . . C22 C 0.3581(5) 0.5003(7) 0.3857(3) 0.0267(15) Uani 1 1 d . . . . . H22 H 0.344973 0.422729 0.354646 0.032 Uiso 1 1 calc R U . . . C23 C 0.3687(5) 0.4755(7) 0.4542(3) 0.0245(14) Uani 1 1 d . . . . . C24 C 0.1976(5) 0.1513(7) 0.5786(3) 0.0283(16) Uani 1 1 d . . . . . H24A H 0.159762 0.122961 0.612802 0.042 Uiso 1 1 calc R U . . . H24B H 0.195962 0.256408 0.573666 0.042 Uiso 1 1 calc R U . . . H24C H 0.169188 0.106444 0.535459 0.042 Uiso 1 1 calc R U . . . O1W O 0.6326(4) 1.2226(6) 0.8087(3) 0.0470(14) Uani 1 1 d D . . . . H1W1 H 0.639(5) 1.149(6) 0.786(4) 0.056 Uiso 1 1 d D U . . . H1W2 H 0.5712(10) 1.225(9) 0.798(4) 0.056 Uiso 1 1 d D U . . . O2W O 0.4775(4) 0.5561(5) 0.7671(2) 0.0328(12) Uani 1 1 d D . . . . H2W1 H 0.470(6) 0.527(6) 0.7275(10) 0.039 Uiso 1 1 d D U . . . H2W2 H 0.486(6) 0.475(3) 0.785(3) 0.039 Uiso 1 1 d D U . . . O3W O 0.7601(4) 0.9232(6) 0.6053(3) 0.0441(14) Uani 1 1 d D . . . . H3W1 H 0.785(5) 0.992(5) 0.630(3) 0.053 Uiso 1 1 d D U . . . H3W2 H 0.800(5) 0.861(5) 0.624(4) 0.053 Uiso 1 1 d D U . . . O4W O 0.6729(4) 0.9537(7) 0.7495(3) 0.0474(14) Uani 1 1 d D . . . . H4W1 H 0.708(5) 0.991(9) 0.724(3) 0.057 Uiso 1 1 d D U . . . H4W2 H 0.637(5) 0.909(8) 0.718(2) 0.057 Uiso 1 1 d D U . . . O5W O 0.6737(4) 0.6287(6) 0.7811(3) 0.0417(13) Uani 1 1 d D . . . . H5W1 H 0.6123(12) 0.617(7) 0.776(4) 0.050 Uiso 1 1 d D U . . . H5W2 H 0.668(5) 0.713(4) 0.764(4) 0.050 Uiso 1 1 d D U . . . O6W O 0.5632(4) 0.8840(6) 0.6193(3) 0.0419(13) Uani 1 1 d D . . . . H6W1 H 0.545(5) 0.797(3) 0.616(4) 0.050 Uiso 1 1 d D U . . . H6W2 H 0.620(2) 0.868(7) 0.612(4) 0.050 Uiso 1 1 d D U . . . 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 0.0302(3) 0.0180(2) 0.0129(2) -0.00007(18) -0.00538(17) -0.0010(2) O1 0.039(3) 0.022(2) 0.015(2) 0.0001(17) -0.0039(19) -0.003(2) O2 0.041(3) 0.019(2) 0.014(2) 0.0007(16) 0.0002(19) -0.003(2) O3 0.050(3) 0.026(2) 0.019(2) -0.0011(18) -0.009(2) -0.007(2) O4 0.035(3) 0.019(2) 0.014(2) -0.0019(16) -0.0043(19) -0.007(2) O5 0.039(3) 0.022(2) 0.011(2) -0.0012(17) -0.0044(18) -0.002(2) O6 0.047(3) 0.019(2) 0.021(2) 0.0007(17) 0.000(2) 0.001(2) N1 0.024(3) 0.021(2) 0.014(2) 0.002(2) -0.003(2) -0.002(2) N2 0.031(3) 0.016(2) 0.015(3) 0.0012(19) -0.002(2) 0.001(2) C1 0.043(4) 0.017(3) 0.019(3) 0.000(2) -0.005(3) -0.002(3) C2 0.032(4) 0.026(3) 0.017(3) -0.002(2) -0.003(3) -0.007(3) C3 0.037(4) 0.020(3) 0.018(3) -0.002(2) -0.002(3) 0.001(3) C4 0.032(4) 0.021(3) 0.014(3) -0.001(2) -0.005(3) 0.004(3) C5 0.033(4) 0.020(3) 0.018(3) -0.008(2) -0.008(3) 0.000(3) C6 0.028(4) 0.018(3) 0.017(3) -0.001(2) -0.005(3) 0.007(3) C7 0.029(4) 0.021(3) 0.021(3) 0.000(2) -0.005(3) -0.002(3) C8 0.036(4) 0.036(4) 0.017(3) -0.006(3) -0.004(3) -0.002(3) C9 0.030(4) 0.042(4) 0.013(3) 0.002(3) -0.005(3) -0.001(3) C10 0.036(4) 0.026(3) 0.022(3) 0.003(3) -0.004(3) -0.005(3) C11 0.036(4) 0.020(3) 0.016(3) -0.004(2) -0.007(3) 0.001(3) C12 0.039(4) 0.026(3) 0.023(3) -0.003(3) -0.007(3) 0.006(3) C13 0.034(4) 0.023(3) 0.019(3) 0.004(2) -0.005(3) -0.002(3) C14 0.038(4) 0.018(3) 0.017(3) -0.002(2) -0.001(3) 0.004(3) C15 0.032(4) 0.022(3) 0.016(3) 0.005(2) -0.005(3) -0.002(3) C16 0.033(4) 0.025(3) 0.016(3) -0.001(2) -0.006(3) 0.000(3) C17 0.032(4) 0.019(3) 0.022(3) 0.000(3) -0.004(3) -0.001(3) C18 0.023(3) 0.022(3) 0.019(3) 0.000(2) -0.005(3) 0.001(3) C19 0.030(4) 0.025(3) 0.020(3) 0.002(3) -0.004(3) 0.004(3) C20 0.032(4) 0.025(3) 0.027(4) 0.004(3) -0.005(3) -0.002(3) C21 0.032(4) 0.035(4) 0.017(3) 0.006(3) -0.004(3) 0.004(3) C22 0.035(4) 0.028(3) 0.012(3) 0.002(2) -0.006(3) 0.002(3) C23 0.030(4) 0.022(3) 0.018(3) 0.004(2) -0.004(3) -0.002(3) C24 0.028(4) 0.029(3) 0.022(3) -0.001(3) -0.009(3) -0.002(3) O1W 0.036(3) 0.051(3) 0.051(4) -0.003(3) -0.001(3) -0.001(3) O2W 0.050(3) 0.024(2) 0.021(2) -0.0001(19) -0.002(2) -0.007(2) O3W 0.054(4) 0.042(3) 0.031(3) -0.003(2) -0.007(2) -0.001(3) O4W 0.044(3) 0.054(4) 0.041(3) -0.015(3) -0.002(3) -0.003(3) O5W 0.042(3) 0.047(3) 0.034(3) -0.001(2) 0.001(3) 0.002(3) O6W 0.041(3) 0.036(3) 0.045(3) -0.007(2) 0.000(3) 0.004(3) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pd1 O4 87.40(17) . . ? O1 Pd1 N2 179.02(19) . . ? O4 Pd1 N2 93.58(18) . . ? O1 Pd1 N1 91.58(18) . . ? O4 Pd1 N1 177.6(2) . . ? N2 Pd1 N1 87.44(19) . . ? C4 O1 Pd1 123.0(4) . . ? C11 O2 C3 119.0(5) . . ? C16 O4 Pd1 124.1(4) . . ? C23 O5 C15 120.0(5) . . ? C2 N1 C1 109.3(5) . . ? C2 N1 C12 110.1(5) . . ? C1 N1 C12 109.8(5) . . ? C2 N1 Pd1 113.0(4) . . ? C1 N1 Pd1 105.8(3) . . ? C12 N1 Pd1 108.7(4) . . ? C14 N2 C24 110.8(5) . . ? C14 N2 C13 109.3(5) . . ? C24 N2 C13 109.3(5) . . ? C14 N2 Pd1 110.1(4) . . ? C24 N2 Pd1 112.0(4) . . ? C13 N2 Pd1 105.2(4) . . ? C13 C1 N1 109.6(5) . . ? N1 C2 C3 113.1(6) . . ? C4 C3 O2 123.9(5) . . ? C4 C3 C2 127.0(6) . . ? O2 C3 C2 108.8(5) . . ? O1 C4 C3 126.2(5) . . ? O1 C4 C5 114.5(5) . . ? C3 C4 C5 119.3(6) . . ? O3 C5 C6 123.8(5) . . ? O3 C5 C4 120.5(6) . . ? C6 C5 C4 115.6(5) . . ? C11 C6 C7 117.4(6) . . ? C11 C6 C5 120.4(5) . . ? C7 C6 C5 122.1(6) . . ? C8 C7 C6 121.3(6) . . ? C7 C8 C9 119.7(6) . . ? C10 C9 C8 120.9(6) . . ? C9 C10 C11 118.3(6) . . ? O2 C11 C6 121.6(6) . . ? O2 C11 C10 116.1(6) . . ? C6 C11 C10 122.2(6) . . ? C1 C13 N2 109.5(5) . . ? N2 C14 C15 112.1(5) . . ? C16 C15 O5 122.9(6) . . ? C16 C15 C14 127.7(6) . . ? O5 C15 C14 109.2(5) . . ? O4 C16 C15 123.7(6) . . ? O4 C16 C17 116.2(5) . . ? C15 C16 C17 120.1(6) . . ? O6 C17 C16 121.9(6) . . ? O6 C17 C18 122.7(6) . . ? C16 C17 C18 115.4(5) . . ? C23 C18 C19 117.4(6) . . ? C23 C18 C17 120.5(6) . . ? C19 C18 C17 122.2(6) . . ? C20 C19 C18 120.9(6) . . ? C19 C20 C21 119.7(6) . . ? C22 C21 C20 120.8(6) . . ? C21 C22 C23 119.2(6) . . ? O5 C23 C22 116.8(6) . . ? O5 C23 C18 121.1(5) . . ? C22 C23 C18 122.1(6) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 O1 2.006(4) . ? Pd1 O4 2.014(4) . ? Pd1 N2 2.033(5) . ? Pd1 N1 2.038(5) . ? O1 C4 1.336(8) . ? O2 C11 1.370(7) . ? O2 C3 1.375(8) . ? O3 C5 1.237(8) . ? O4 C16 1.331(8) . ? O5 C23 1.363(7) . ? O5 C15 1.381(7) . ? O6 C17 1.240(7) . ? N1 C2 1.460(8) . ? N1 C1 1.501(7) . ? N1 C12 1.508(8) . ? N2 C14 1.477(9) . ? N2 C24 1.500(8) . ? N2 C13 1.508(8) . ? C1 C13 1.499(9) . ? C2 C3 1.506(8) . ? C3 C4 1.351(9) . ? C4 C5 1.475(8) . ? C5 C6 1.450(9) . ? C6 C11 1.391(9) . ? C6 C7 1.402(8) . ? C7 C8 1.370(9) . ? C8 C9 1.400(10) . ? C9 C10 1.371(9) . ? C10 C11 1.400(9) . ? C14 C15 1.502(8) . ? C15 C16 1.361(9) . ? C16 C17 1.456(9) . ? C17 C18 1.468(9) . ? C18 C23 1.392(8) . ? C18 C19 1.407(9) . ? C19 C20 1.370(9) . ? C20 C21 1.399(9) . ? C21 C22 1.360(9) . ? C22 C23 1.382(8) . ?