#------------------------------------------------------------------------------ #$Date: 2023-03-19 01:49:38 +0200 (Sun, 19 Mar 2023) $ #$Revision: 281943 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/71/26/7712656.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_7712656 loop_ _publ_author_name 'Gumrukcu, Selin' 'Ozcesmeci, Mukaddes' 'Ko\,cyi\(git, Nil\"ufer' 'Kaya, Kerem' 'G\"ul, Ahmet' 'Sahin, Yucel' '\"Oz\,ce\,smeci, \.Ibrahim' _publ_section_title ; Synthesis, fabrication and characterization of 2-naphthyloxy group-substituted bis(2-pyridylimino)isoindoline and its derivatives as positive electrode for vanadium redox flow battery applications ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D2DT03547B _journal_year 2023 _chemical_formula_sum 'C30 H22 Cl N5 O Pd' _chemical_formula_weight 610.37 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2021-03-07 deposited with the CCDC. 2023-03-17 downloaded from the CCDC. ; _cell_angle_alpha 79.298(7) _cell_angle_beta 87.886(7) _cell_angle_gamma 70.496(7) _cell_formula_units_Z 2 _cell_length_a 8.6324(9) _cell_length_b 10.5581(12) _cell_length_c 16.7354(17) _cell_measurement_reflns_used 24 _cell_measurement_temperature 303(2) _cell_measurement_theta_max 26 _cell_measurement_theta_min 5 _cell_volume 1412.2(3) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 303(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type Bruker_D8_VENTURE _diffrn_measurement_method omega_scans _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1756 _diffrn_reflns_av_unetI/netI 0.1878 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 20957 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 24.996 _diffrn_reflns_theta_max 24.996 _diffrn_reflns_theta_min 2.218 _diffrn_source Sealed_Tube _exptl_absorpt_coefficient_mu 0.783 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.435 _exptl_crystal_description rod _exptl_crystal_F_000 616 _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_transmission_factor_max 0.955 _exptl_transmission_factor_min 0.878 _refine_diff_density_max 1.101 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.155 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 345 _refine_ls_number_reflns 4965 _refine_ls_number_restraints 417 _refine_ls_restrained_S_all 1.063 _refine_ls_R_factor_all 0.1901 _refine_ls_R_factor_gt 0.0824 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1111P)^2^+0.9952P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2033 _refine_ls_wR_factor_ref 0.2409 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2456 _reflns_number_total 4965 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d2dt03547b2.cif _cod_data_source_block 2_a _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi_scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_database_code 7712656 _shelx_shelxl_version_number 2014/7 _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 ; 2_a.res created by SHELXL-2014/7 TITL 2_a.res in P-1 CELL 0.71073 8.6324 10.5581 16.7354 79.298 87.886 70.496 ZERR 2.000 0.0009 0.0012 0.0017 0.007 0.007 0.007 LATT 1 SFAC C H Cl N O Pd UNIT 60 44 2 10 2 2 OMIT -2 50 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 DELU 0.005 $C SIMU 0.005 $C ISOR 0.05 $C TEMP 30.150 WGHT 0.111100 0.995200 FVAR 0.35298 PD 6 0.465651 0.258008 0.638089 11.00000 0.04693 0.04787 = 0.04511 -0.01156 0.00513 -0.02353 CL 3 0.495631 0.186424 0.778674 11.00000 0.10545 0.11178 = 0.05173 -0.01159 0.00950 -0.06174 N1 4 0.272129 0.187921 0.634841 11.00000 0.04236 0.03557 = 0.05962 -0.00636 0.01072 -0.01376 N3 4 0.487565 0.261695 0.523090 11.00000 0.05114 0.04197 = 0.03627 -0.00704 -0.00202 -0.02548 N5 4 0.631322 0.359261 0.634891 11.00000 0.05069 0.05084 = 0.04478 -0.00635 -0.00274 -0.02441 N4 4 0.705624 0.357487 0.493752 11.00000 0.05581 0.05609 = 0.03910 -0.01223 0.00280 -0.03231 N2 4 0.309716 0.138702 0.500592 11.00000 0.05110 0.05429 = 0.04336 -0.00621 0.00151 -0.02448 O1 5 0.757508 0.226663 0.193517 11.00000 0.12197 0.11749 = 0.06034 -0.05313 0.04367 -0.08385 C15 1 0.493329 0.194318 0.398727 11.00000 0.04809 0.05087 = 0.04583 -0.01176 0.00069 -0.02625 C8 1 0.714306 0.391542 0.569252 11.00000 0.05001 0.05071 = 0.04819 -0.01124 -0.00004 -0.02611 C14 1 0.602282 0.303554 0.474917 11.00000 0.04733 0.04758 = 0.04493 -0.01029 0.00321 -0.02779 C13 1 0.418245 0.196288 0.480397 11.00000 0.04590 0.04645 = 0.04454 -0.00969 0.00068 -0.02299 C18 1 0.468079 0.138522 0.333047 11.00000 0.05113 0.05563 = 0.04790 -0.01572 -0.00180 -0.02802 AFIX 43 H18 2 0.392747 0.092424 0.334928 11.00000 -1.20000 AFIX 0 C16 1 0.602946 0.264298 0.395101 11.00000 0.04795 0.05108 = 0.04517 -0.01122 0.00244 -0.02752 C10 1 0.818248 0.468349 0.573662 11.00000 0.05217 0.05416 = 0.04733 -0.01437 0.00003 -0.02657 AFIX 43 H10 2 0.873222 0.490522 0.527161 11.00000 -1.20000 AFIX 0 C6 1 0.233073 0.138891 0.571946 11.00000 0.04148 0.05060 = 0.05806 -0.01447 0.00290 -0.02075 C1 1 0.174575 0.190653 0.700834 11.00000 0.05141 0.06154 = 0.07507 -0.01707 0.01561 -0.02457 AFIX 43 H1 2 0.193718 0.231565 0.742377 11.00000 -1.20000 AFIX 0 C5 1 0.108492 0.082798 0.579691 11.00000 0.04306 0.05607 = 0.06515 -0.01325 0.00153 -0.02371 AFIX 43 H5 2 0.085706 0.047754 0.536186 11.00000 -1.20000 AFIX 0 C17 1 0.694695 0.282596 0.327226 11.00000 0.05214 0.05593 = 0.04563 -0.01213 0.00425 -0.02969 AFIX 43 H17 2 0.768256 0.330499 0.324507 11.00000 -1.20000 AFIX 0 C19 1 0.559386 0.154814 0.265707 11.00000 0.05638 0.05892 = 0.04663 -0.01641 -0.00193 -0.02664 AFIX 43 H19 2 0.546704 0.118196 0.220931 11.00000 -1.20000 AFIX 0 C20 1 0.668627 0.223672 0.262926 11.00000 0.05536 0.05844 = 0.04459 -0.01263 0.00321 -0.02638 C2 1 0.051378 0.137119 0.709254 11.00000 0.04912 0.06136 = 0.07213 -0.01381 0.01414 -0.02222 AFIX 43 H2 2 -0.010781 0.140670 0.755886 11.00000 -1.20000 AFIX 0 C7 1 0.656143 0.402516 0.702533 11.00000 0.05646 0.06437 = 0.04713 -0.01979 0.00777 -0.02474 AFIX 43 H7 2 0.602547 0.379916 0.749454 11.00000 -1.20000 AFIX 0 C3 1 0.017892 0.076055 0.647038 11.00000 0.04447 0.05903 = 0.07203 -0.00992 0.00774 -0.02226 C11 1 0.842118 0.510848 0.640477 11.00000 0.05510 0.05676 = 0.04835 -0.01927 -0.00099 -0.02544 C4 1 -0.112463 0.009997 0.655124 11.00000 0.04992 0.06670 = 0.08131 -0.00639 0.00519 -0.02781 AFIX 137 H4A 2 -0.176692 0.037118 0.605393 11.00000 -1.50000 H4B 2 -0.182482 0.038176 0.699011 11.00000 -1.50000 H4C 2 -0.061666 -0.087590 0.666146 11.00000 -1.50000 AFIX 0 C9 1 0.756043 0.477813 0.705490 11.00000 0.05796 0.06149 = 0.04949 -0.02224 0.00240 -0.02406 AFIX 43 H9 2 0.765364 0.507353 0.753534 11.00000 -1.20000 AFIX 0 C21 1 0.837970 0.320083 0.171274 11.00000 0.08832 0.09785 = 0.05132 -0.02467 0.01291 -0.04587 C12 1 0.960849 0.585152 0.644922 11.00000 0.06252 0.06892 = 0.06549 -0.01669 -0.00648 -0.03303 AFIX 137 H12A 2 1.067144 0.520365 0.662370 11.00000 -1.50000 H12B 2 0.923338 0.645896 0.683058 11.00000 -1.50000 H12C 2 0.968293 0.636903 0.592192 11.00000 -1.50000 AFIX 0 C22 1 0.999672 0.273619 0.155625 11.00000 0.08863 0.10250 = 0.05237 -0.02464 0.01218 -0.04432 AFIX 43 H22 2 1.057823 0.180334 0.165691 11.00000 -1.20000 AFIX 0 C24 1 1.079532 0.368298 0.123791 11.00000 0.08998 0.10927 = 0.05643 -0.02202 0.00902 -0.04865 C23 1 0.751898 0.459101 0.159454 11.00000 0.09164 0.10044 = 0.05692 -0.02307 0.01222 -0.04248 AFIX 43 H23 2 0.641483 0.489685 0.172398 11.00000 -1.20000 AFIX 0 C25 1 0.827312 0.550413 0.129270 11.00000 0.09765 0.10139 = 0.05939 -0.01682 0.00869 -0.04358 AFIX 43 H25 2 0.767738 0.643398 0.120725 11.00000 -1.20000 AFIX 0 C26 1 0.991988 0.507364 0.110916 11.00000 0.09684 0.10857 = 0.05935 -0.01517 0.00739 -0.04936 C28 1 1.324707 0.424128 0.075622 11.00000 0.09503 0.12585 = 0.07415 -0.01331 0.00817 -0.05267 AFIX 43 H28 2 1.435280 0.396433 0.062744 11.00000 -1.20000 AFIX 0 C30 1 1.232093 0.554753 0.064449 11.00000 0.10142 0.12314 = 0.07432 -0.00741 0.00772 -0.05394 AFIX 43 H30 2 1.283511 0.617941 0.043425 11.00000 -1.20000 AFIX 0 C29 1 1.075141 0.604430 0.079959 11.00000 0.10267 0.11603 = 0.06962 -0.00700 0.00655 -0.05186 AFIX 43 H29 2 1.019665 0.698145 0.071406 11.00000 -1.20000 AFIX 0 C27 1 1.247160 0.331807 0.107497 11.00000 0.09254 0.12051 = 0.06812 -0.01698 0.00890 -0.04969 AFIX 43 H27 2 1.310178 0.239612 0.118861 11.00000 -1.20000 AFIX 0 HKLF 4 REM 2_a.res in P-1 REM R1 = 0.0824 for 2456 Fo > 4sig(Fo) and 0.1901 for all 4965 data REM 345 parameters refined using 417 restraints END WGHT 0.1112 0.8952 REM Highest difference peak 1.101, deepest hole -0.739, 1-sigma level 0.155 Q1 1 0.8897 1.0186 0.0573 11.00000 0.05 1.10 Q2 1 1.1493 -0.0152 0.0404 11.00000 0.05 0.88 Q3 1 0.7336 0.0529 0.0434 11.00000 0.05 0.73 Q4 1 1.2324 0.9164 0.0455 11.00000 0.05 0.72 Q5 1 1.2035 0.9215 0.0054 11.00000 0.05 0.70 Q6 1 1.4837 0.0561 0.0034 11.00000 0.05 0.67 Q7 1 1.3911 0.8574 0.0113 11.00000 0.05 0.67 Q8 1 1.3069 0.9662 0.0096 11.00000 0.05 0.58 Q9 1 1.3765 0.0347 0.0065 11.00000 0.05 0.52 Q10 1 0.6240 0.9685 0.0223 11.00000 0.05 0.49 Q11 1 1.5767 0.0769 0.0392 11.00000 0.05 0.48 Q12 1 0.4381 0.4188 0.6162 11.00000 0.05 0.45 Q13 1 1.1193 0.5415 0.6046 11.00000 0.05 0.44 Q14 1 0.4036 0.2174 0.2902 11.00000 0.05 0.43 Q15 1 0.5806 0.2005 0.5676 11.00000 0.05 0.42 Q16 1 0.5176 0.2429 0.4816 11.00000 0.05 0.42 Q17 1 0.9828 0.5642 0.6962 11.00000 0.05 0.41 Q18 1 0.8531 0.6764 0.6395 11.00000 0.05 0.40 Q19 1 0.4760 0.3224 0.7233 11.00000 0.05 0.40 Q20 1 0.3781 0.3433 0.6436 11.00000 0.05 0.40 ; _shelx_res_checksum 28493 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Pd Pd 0.46565(11) 0.25801(9) 0.63809(5) 0.0444(4) Uani 1 1 d . . . . . Cl Cl 0.4956(5) 0.1864(4) 0.7787(2) 0.0838(11) Uani 1 1 d . . . . . N1 N 0.2721(10) 0.1879(8) 0.6348(6) 0.046(2) Uani 1 1 d . . . . . N3 N 0.4876(10) 0.2617(8) 0.5231(5) 0.041(2) Uani 1 1 d . . . . . N5 N 0.6313(11) 0.3593(9) 0.6349(5) 0.047(2) Uani 1 1 d . . . . . N4 N 0.7056(10) 0.3575(9) 0.4938(5) 0.046(2) Uani 1 1 d . . . . . N2 N 0.3097(11) 0.1387(9) 0.5006(5) 0.048(2) Uani 1 1 d . . . . . O1 O 0.7575(12) 0.2267(10) 0.1935(5) 0.085(3) Uani 1 1 d . . . . . C15 C 0.4933(13) 0.1943(11) 0.3987(6) 0.0454(16) Uani 1 1 d . U . . . C8 C 0.7143(13) 0.3915(11) 0.5693(7) 0.047(2) Uani 1 1 d . U . . . C14 C 0.6023(13) 0.3036(11) 0.4749(6) 0.0434(19) Uani 1 1 d . U . . . C13 C 0.4182(13) 0.1963(11) 0.4804(6) 0.043(2) Uani 1 1 d . U . . . C18 C 0.4681(13) 0.1385(11) 0.3330(6) 0.0480(18) Uani 1 1 d . U . . . H18 H 0.3927 0.0924 0.3349 0.058 Uiso 1 1 calc R U . . . C16 C 0.6029(13) 0.2643(11) 0.3951(6) 0.0450(16) Uani 1 1 d . U . . . C10 C 0.8182(13) 0.4683(11) 0.5737(7) 0.0482(19) Uani 1 1 d . U . . . H10 H 0.8732 0.4905 0.5272 0.058 Uiso 1 1 calc R U . . . C6 C 0.2331(13) 0.1389(11) 0.5719(7) 0.048(2) Uani 1 1 d . U . . . C1 C 0.1746(14) 0.1907(12) 0.7008(8) 0.061(2) Uani 1 1 d . U . . . H1 H 0.1937 0.2316 0.7424 0.073 Uiso 1 1 calc R U . . . C5 C 0.1085(13) 0.0828(11) 0.5797(7) 0.053(2) Uani 1 1 d . U . . . H5 H 0.0857 0.0478 0.5362 0.063 Uiso 1 1 calc R U . . . C17 C 0.6947(13) 0.2826(11) 0.3272(6) 0.0479(17) Uani 1 1 d . U . . . H17 H 0.7683 0.3305 0.3245 0.058 Uiso 1 1 calc R U . . . C19 C 0.5594(14) 0.1548(11) 0.2657(7) 0.0511(18) Uani 1 1 d . U . . . H19 H 0.5467 0.1182 0.2209 0.061 Uiso 1 1 calc R U . . . C20 C 0.6686(14) 0.2237(12) 0.2629(7) 0.0505(18) Uani 1 1 d . U . . . C2 C 0.0514(14) 0.1371(12) 0.7093(7) 0.060(2) Uani 1 1 d . U . . . H2 H -0.0108 0.1407 0.7559 0.072 Uiso 1 1 calc R U . . . C7 C 0.6561(14) 0.4025(12) 0.7025(7) 0.054(2) Uani 1 1 d . U . . . H7 H 0.6025 0.3799 0.7495 0.064 Uiso 1 1 calc R U . . . C3 C 0.0179(14) 0.0761(12) 0.6470(8) 0.0577(19) Uani 1 1 d . U . . . C11 C 0.8421(14) 0.5108(11) 0.6405(7) 0.0503(18) Uani 1 1 d . U . . . C4 C -0.1125(14) 0.0100(13) 0.6551(8) 0.065(3) Uani 1 1 d . U . . . H4A H -0.1767 0.0371 0.6054 0.097 Uiso 1 1 calc R U . . . H4B H -0.1825 0.0382 0.6990 0.097 Uiso 1 1 calc R U . . . H4C H -0.0617 -0.0876 0.6661 0.097 Uiso 1 1 calc R U . . . C9 C 0.7560(14) 0.4778(12) 0.7055(7) 0.054(2) Uani 1 1 d . U . . . H9 H 0.7654 0.5074 0.7535 0.064 Uiso 1 1 calc R U . . . C21 C 0.8380(18) 0.3201(16) 0.1713(7) 0.074(2) Uani 1 1 d . U . . . C12 C 0.9608(14) 0.5852(12) 0.6449(7) 0.062(3) Uani 1 1 d . U . . . H12A H 1.0671 0.5204 0.6624 0.093 Uiso 1 1 calc R U . . . H12B H 0.9233 0.6459 0.6831 0.093 Uiso 1 1 calc R U . . . H12C H 0.9683 0.6369 0.5922 0.093 Uiso 1 1 calc R U . . . C22 C 0.9997(17) 0.2736(16) 0.1556(7) 0.077(2) Uani 1 1 d . U . . . H22 H 1.0578 0.1803 0.1657 0.092 Uiso 1 1 calc R U . . . C24 C 1.0795(18) 0.3683(17) 0.1238(8) 0.081(2) Uani 1 1 d . U . . . C23 C 0.7519(18) 0.4591(15) 0.1595(7) 0.079(2) Uani 1 1 d . U . . . H23 H 0.6415 0.4897 0.1724 0.095 Uiso 1 1 calc R U . . . C25 C 0.8273(19) 0.5504(16) 0.1293(8) 0.083(2) Uani 1 1 d . U . . . H25 H 0.7677 0.6434 0.1207 0.100 Uiso 1 1 calc R U . . . C26 C 0.9920(19) 0.5074(17) 0.1109(8) 0.085(2) Uani 1 1 d . U . . . C28 C 1.325(2) 0.4241(18) 0.0756(9) 0.095(3) Uani 1 1 d . U . . . H28 H 1.4353 0.3964 0.0627 0.114 Uiso 1 1 calc R U . . . C30 C 1.232(2) 0.5548(18) 0.0644(9) 0.097(3) Uani 1 1 d . U . . . H30 H 1.2835 0.6179 0.0434 0.116 Uiso 1 1 calc R U . . . C29 C 1.075(2) 0.6044(18) 0.0800(8) 0.094(2) Uani 1 1 d . U . . . H29 H 1.0197 0.6981 0.0714 0.112 Uiso 1 1 calc R U . . . C27 C 1.2472(19) 0.3318(18) 0.1075(8) 0.090(2) Uani 1 1 d . U . . . H27 H 1.3102 0.2396 0.1189 0.108 Uiso 1 1 calc R 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 Pd 0.0469(6) 0.0479(6) 0.0451(6) -0.0116(4) 0.0051(4) -0.0235(4) Cl 0.105(3) 0.112(3) 0.052(2) -0.012(2) 0.0095(19) -0.062(3) N1 0.042(5) 0.036(5) 0.060(6) -0.006(5) 0.011(5) -0.014(4) N3 0.051(6) 0.042(5) 0.036(5) -0.007(4) -0.002(4) -0.025(5) N5 0.051(6) 0.051(6) 0.045(6) -0.006(5) -0.003(5) -0.024(5) N4 0.056(6) 0.056(6) 0.039(5) -0.012(5) 0.003(5) -0.032(5) N2 0.051(6) 0.054(6) 0.043(6) -0.006(5) 0.002(5) -0.024(5) O1 0.122(8) 0.117(8) 0.060(6) -0.053(5) 0.044(5) -0.084(7) C15 0.048(4) 0.051(4) 0.046(3) -0.012(3) 0.001(3) -0.026(3) C8 0.050(5) 0.051(5) 0.048(5) -0.011(4) 0.000(4) -0.026(4) C14 0.047(5) 0.048(5) 0.045(4) -0.010(4) 0.003(4) -0.028(4) C13 0.046(5) 0.046(5) 0.045(4) -0.010(4) 0.001(4) -0.023(4) C18 0.051(4) 0.056(4) 0.048(4) -0.016(3) -0.002(3) -0.028(3) C16 0.048(4) 0.051(4) 0.045(3) -0.011(3) 0.002(3) -0.028(3) C10 0.052(4) 0.054(4) 0.047(4) -0.014(4) 0.000(4) -0.027(4) C6 0.041(5) 0.051(5) 0.058(5) -0.014(4) 0.003(4) -0.021(4) C1 0.051(5) 0.062(5) 0.075(6) -0.017(5) 0.016(5) -0.025(4) C5 0.043(4) 0.056(4) 0.065(4) -0.013(4) 0.002(4) -0.024(4) C17 0.052(4) 0.056(4) 0.046(4) -0.012(3) 0.004(3) -0.030(3) C19 0.056(4) 0.059(4) 0.047(4) -0.016(4) -0.002(3) -0.027(3) C20 0.055(4) 0.058(4) 0.045(4) -0.013(3) 0.003(3) -0.026(3) C2 0.049(4) 0.061(5) 0.072(5) -0.014(4) 0.014(4) -0.022(4) C7 0.056(5) 0.064(5) 0.047(5) -0.020(4) 0.008(4) -0.025(4) C3 0.044(4) 0.059(4) 0.072(5) -0.010(4) 0.008(3) -0.022(3) C11 0.055(4) 0.057(4) 0.048(4) -0.019(3) -0.001(3) -0.025(3) C4 0.050(6) 0.067(7) 0.081(7) -0.006(6) 0.005(5) -0.028(5) C9 0.058(5) 0.061(5) 0.049(4) -0.022(4) 0.002(4) -0.024(4) C21 0.088(5) 0.098(5) 0.051(4) -0.025(4) 0.013(4) -0.046(5) C12 0.063(6) 0.069(7) 0.065(6) -0.017(5) -0.006(5) -0.033(5) C22 0.089(5) 0.102(5) 0.052(4) -0.025(4) 0.012(4) -0.044(4) C24 0.090(5) 0.109(5) 0.056(4) -0.022(4) 0.009(4) -0.049(4) C23 0.092(5) 0.100(5) 0.057(5) -0.023(5) 0.012(4) -0.042(4) C25 0.098(5) 0.101(5) 0.059(5) -0.017(4) 0.009(4) -0.044(4) C26 0.097(5) 0.109(5) 0.059(4) -0.015(4) 0.007(4) -0.049(4) C28 0.095(5) 0.126(6) 0.074(5) -0.013(5) 0.008(5) -0.053(5) C30 0.101(5) 0.123(5) 0.074(5) -0.007(5) 0.008(5) -0.054(5) C29 0.103(5) 0.116(5) 0.070(5) -0.007(5) 0.007(5) -0.052(5) C27 0.093(5) 0.121(5) 0.068(5) -0.017(5) 0.009(4) -0.050(4) 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' Cl Cl 0.1484 0.1585 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Pd N5 89.8(3) . . ? N3 Pd N1 88.9(3) . . ? N5 Pd N1 170.6(3) . . ? N3 Pd Cl 162.4(3) . . ? N5 Pd Cl 92.8(3) . . ? N1 Pd Cl 91.3(3) . . ? C6 N1 C1 117.2(9) . . ? C6 N1 Pd 125.0(7) . . ? C1 N1 Pd 117.8(8) . . ? C13 N3 C14 108.7(8) . . ? C13 N3 Pd 124.2(7) . . ? C14 N3 Pd 125.7(7) . . ? C8 N5 C7 116.3(9) . . ? C8 N5 Pd 125.3(7) . . ? C7 N5 Pd 118.4(7) . . ? C14 N4 C8 123.7(9) . . ? C13 N2 C6 124.4(9) . . ? C20 O1 C21 122.1(9) . . ? C16 C15 C18 121.3(10) . . ? C16 C15 C13 106.9(9) . . ? C18 C15 C13 131.8(9) . . ? N5 C8 N4 125.4(9) . . ? N5 C8 C10 119.8(10) . . ? N4 C8 C10 114.7(9) . . ? N4 C14 N3 129.2(10) . . ? N4 C14 C16 121.4(9) . . ? N3 C14 C16 109.1(8) . . ? N2 C13 N3 130.6(10) . . ? N2 C13 C15 120.6(9) . . ? N3 C13 C15 108.7(9) . . ? C19 C18 C15 116.9(9) . . ? C19 C18 H18 121.6 . . ? C15 C18 H18 121.6 . . ? C15 C16 C17 122.4(10) . . ? C15 C16 C14 106.5(9) . . ? C17 C16 C14 131.0(9) . . ? C11 C10 C8 123.6(10) . . ? C11 C10 H10 118.2 . . ? C8 C10 H10 118.2 . . ? N2 C6 N1 124.3(9) . . ? N2 C6 C5 116.0(10) . . ? N1 C6 C5 119.7(10) . . ? C2 C1 N1 123.6(12) . . ? C2 C1 H1 118.2 . . ? N1 C1 H1 118.2 . . ? C3 C5 C6 123.6(11) . . ? C3 C5 H5 118.2 . . ? C6 C5 H5 118.2 . . ? C16 C17 C20 115.0(9) . . ? C16 C17 H17 122.5 . . ? C20 C17 H17 122.5 . . ? C20 C19 C18 121.4(10) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 O1 115.3(10) . . ? C19 C20 C17 123.1(10) . . ? O1 C20 C17 121.6(9) . . ? C1 C2 C3 119.6(11) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? N5 C7 C9 123.1(10) . . ? N5 C7 H7 118.5 . . ? C9 C7 H7 118.5 . . ? C5 C3 C2 115.8(10) . . ? C5 C3 C4 122.6(11) . . ? C2 C3 C4 121.6(10) . . ? C10 C11 C9 115.3(10) . . ? C10 C11 C12 122.5(10) . . ? C9 C11 C12 122.1(10) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C11 C9 C7 121.8(11) . . ? C11 C9 H9 119.1 . . ? C7 C9 H9 119.1 . . ? C22 C21 O1 118.6(14) . . ? C22 C21 C23 120.7(14) . . ? O1 C21 C23 120.5(13) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C21 C22 C24 119.2(15) . . ? C21 C22 H22 120.4 . . ? C24 C22 H22 120.4 . . ? C26 C24 C27 116.2(14) . . ? C26 C24 C22 119.7(14) . . ? C27 C24 C22 124.0(16) . . ? C25 C23 C21 120.4(15) . . ? C25 C23 H23 119.8 . . ? C21 C23 H23 119.8 . . ? C23 C25 C26 120.8(16) . . ? C23 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C25 C26 C24 119.1(14) . . ? C25 C26 C29 121.3(16) . . ? C24 C26 C29 119.6(15) . . ? C30 C28 C27 115.9(16) . . ? C30 C28 H28 122.0 . . ? C27 C28 H28 122.0 . . ? C29 C30 C28 126.8(17) . . ? C29 C30 H30 116.6 . . ? C28 C30 H30 116.6 . . ? C30 C29 C26 117.4(17) . . ? C30 C29 H29 121.3 . . ? C26 C29 H29 121.3 . . ? C28 C27 C24 124.0(17) . . ? C28 C27 H27 118.0 . . ? C24 C27 H27 118.0 . . ? 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 Pd N3 1.921(8) . ? Pd N5 2.046(8) . ? Pd N1 2.047(8) . ? Pd Cl 2.330(3) . ? N1 C6 1.354(13) . ? N1 C1 1.363(13) . ? N3 C13 1.355(12) . ? N3 C14 1.388(12) . ? N5 C8 1.342(12) . ? N5 C7 1.346(13) . ? N4 C14 1.283(12) . ? N4 C8 1.387(13) . ? N2 C13 1.282(12) . ? N2 C6 1.344(13) . ? O1 C20 1.370(12) . ? O1 C21 1.377(15) . ? C15 C16 1.375(13) . ? C15 C18 1.395(14) . ? C15 C13 1.492(14) . ? C8 C10 1.408(13) . ? C14 C16 1.470(14) . ? C18 C19 1.369(13) . ? C18 H18 0.9300 . ? C16 C17 1.382(13) . ? C10 C11 1.326(14) . ? C10 H10 0.9300 . ? C6 C5 1.382(14) . ? C1 C2 1.353(14) . ? C1 H1 0.9300 . ? C5 C3 1.353(14) . ? C5 H5 0.9300 . ? C17 C20 1.398(14) . ? C17 H17 0.9300 . ? C19 C20 1.365(14) . ? C19 H19 0.9300 . ? C2 C3 1.407(16) . ? C2 H2 0.9300 . ? C7 C9 1.362(14) . ? C7 H7 0.9300 . ? C3 C4 1.500(14) . ? C11 C9 1.353(14) . ? C11 C12 1.495(14) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C9 H9 0.9300 . ? C21 C22 1.350(17) . ? C21 C23 1.386(19) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C22 C24 1.412(18) . ? C22 H22 0.9300 . ? C24 C26 1.39(2) . ? C24 C27 1.398(18) . ? C23 C25 1.350(17) . ? C23 H23 0.9300 . ? C25 C26 1.382(18) . ? C25 H25 0.9300 . ? C26 C29 1.449(19) . ? C28 C30 1.32(2) . ? C28 C27 1.378(18) . ? C28 H28 0.9300 . ? C30 C29 1.315(19) . ? C30 H30 0.9300 . ? C29 H29 0.9300 . ? C27 H27 0.9300 . ?