#------------------------------------------------------------------------------ #$Date: 2015-01-23 12:30:19 +0000 (Fri, 23 Jan 2015) $ #$Revision: 130086 $ #$URL: svn://www.crystallography.net/cod/cif/7/11/20/7112073.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_7112073 loop_ _publ_author_name 'Fengrui Qu' 'Julia R. Khusnutdinova' 'Nigam P. Rath' 'Liviu M. Mirica' _publ_section_title ; Dioxygen activation by an organometallic Pd(II) precursor: formation of a Pd(IV)-OH complex and its C-O bond formation reactivity ; _journal_name_full Chem.Commun. _journal_page_first 3036 _journal_paper_doi 10.1039/c3cc49387c _journal_volume 50 _journal_year 2014 _chemical_formula_moiety 'C19 H33 I N3 Pd, I' _chemical_formula_sum 'C19 H33 I2 N3 Pd' _chemical_formula_weight 663.68 _chemical_name_systematic ; ? ; _space_group_IT_number 29 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2ac' _symmetry_space_group_name_H-M 'P c a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 16.110(2) _cell_length_b 8.7912(14) _cell_length_c 15.537(2) _cell_measurement_reflns_used 9050 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 39.01 _cell_measurement_theta_min 2.32 _cell_volume 2200.4(5) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 159143 _diffrn_reflns_theta_full 39.06 _diffrn_reflns_theta_max 39.06 _diffrn_reflns_theta_min 2.32 _exptl_absorpt_coefficient_mu 3.657 _exptl_absorpt_correction_T_max 0.6304 _exptl_absorpt_correction_T_min 0.3363 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'sadabs v2008/1' _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.003 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description rectangular _exptl_crystal_F_000 1280 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _refine_diff_density_max 1.407 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.106 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.010(8) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 238 _refine_ls_number_reflns 12564 _refine_ls_number_restraints 10 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.0218 _refine_ls_R_factor_gt 0.0196 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+0.7295P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0391 _reflns_number_gt 12029 _reflns_number_total 12564 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL lm23312/lt/x8/Fengrui/Me3tacnPd(IV) in Pca2(1) CELL 0.71073 16.1097 8.7912 15.5366 90.000 90.000 90.000 ZERR 4.00 0.0024 0.0014 0.0023 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, -Y, Z SYMM 0.5-X, Y, 0.5+Z SFAC C H N PD I UNIT 76 132 12 4 8 TEMP -173.0 SIZE 0.139 0.157 0.381 omit -3.0 L.S. 20 acta wpdb -2 list 4 bond $h HTAB conf more 2 FMAP 2 PLAN 10 delu $pd $i eadp pd1 pd1' eadp i1 i1' sadi 0.005 pd1 i1 pd1' i1' sadi pd1 n1 pd1' n1 sadi pd1 n2 pd1' n2 sadi pd1 n3 pd1' n3 sadi pd1 c4 pd1' c4 sadi pd1 c1 pd1' c1 sadi pd1 c11 pd1' c11 WGHT 0.016700 0.729500 FVAR 0.08067 0.96745 part 1 PD1 4 0.764656 0.652695 0.978732 21.00000 0.00644 0.00846 = 0.00869 -0.00132 0.00013 -0.00007 I1 5 0.858396 0.508756 1.086958 21.00000 0.01056 0.01021 = 0.01103 -0.00028 -0.00018 0.00066 part 2 PD1' 4 0.748967 0.667266 0.977412 -21.00000 0.00644 0.00846 = 0.00869 -0.00132 0.00013 -0.00007 I1' 5 0.850372 0.543349 1.083661 -21.00000 0.01056 0.01021 = 0.01103 -0.00028 -0.00018 0.00066 part 0 I2 5 0.523695 0.272226 0.746431 11.00000 0.01093 0.02389 = 0.01945 -0.00863 0.00000 -0.00067 N1 3 0.783064 0.499983 0.865833 11.00000 0.00997 0.01497 = 0.01118 -0.00311 0.00019 0.00098 N2 3 0.676507 0.760066 0.889829 11.00000 0.01278 0.01781 = 0.01207 -0.00175 -0.00093 0.00394 C3 1 0.809547 0.932782 1.068214 11.00000 0.01127 0.01017 = 0.01699 -0.00094 -0.00133 -0.00108 N3 3 0.654202 0.490286 0.996668 11.00000 0.01011 0.01369 = 0.01451 -0.00431 0.00103 -0.00253 C4 1 0.749350 0.817650 1.067910 11.00000 0.01067 0.00951 = 0.01177 -0.00088 0.00009 -0.00034 C17 1 0.626940 0.450559 1.084720 11.00000 0.01588 0.01785 = 0.01649 -0.00406 0.00371 -0.00720 AFIX 137 H17A 2 0.600483 0.539143 1.111435 11.00000 -1.50000 H17B 2 0.675137 0.419802 1.119046 11.00000 -1.50000 H17C 2 0.587130 0.366401 1.082036 11.00000 -1.50000 AFIX 0 C5 1 0.679810 0.829892 1.120796 11.00000 0.01230 0.01387 = 0.01263 -0.00249 0.00117 -0.00117 AFIX 43 H5 2 0.639621 0.750823 1.121573 11.00000 -1.20000 AFIX 0 C1 1 0.865369 0.786076 0.947176 11.00000 0.01226 0.01365 = 0.01645 0.00007 0.00417 -0.00214 AFIX 23 H1A 2 0.915112 0.720227 0.943749 11.00000 -1.20000 H1B 2 0.856032 0.829754 0.889247 11.00000 -1.20000 AFIX 0 C14 1 0.721328 0.374210 0.867604 11.00000 0.01199 0.01672 = 0.01687 -0.00838 -0.00018 -0.00211 AFIX 23 H14A 2 0.748220 0.279469 0.847381 11.00000 -1.20000 H14B 2 0.675541 0.398384 0.827365 11.00000 -1.20000 AFIX 0 C13 1 0.685834 0.347979 0.956272 11.00000 0.01314 0.01386 = 0.01984 -0.00704 0.00284 -0.00396 AFIX 23 H13A 2 0.639903 0.273503 0.952239 11.00000 -1.20000 H13B 2 0.729365 0.303615 0.993593 11.00000 -1.20000 AFIX 0 C15 1 0.867813 0.436494 0.856487 11.00000 0.01054 0.01572 = 0.01456 -0.00230 0.00123 0.00239 AFIX 137 H15A 2 0.870678 0.374781 0.804041 11.00000 -1.50000 H15B 2 0.880760 0.372863 0.906508 11.00000 -1.50000 H15C 2 0.908038 0.519856 0.852731 11.00000 -1.50000 AFIX 0 C2 1 0.883456 0.916251 1.009854 11.00000 0.01046 0.01104 = 0.02163 0.00040 0.00222 -0.00268 C11 1 0.593879 0.722332 0.927711 11.00000 0.01032 0.02234 = 0.01643 -0.00419 -0.00139 0.00503 AFIX 23 H11A 2 0.549862 0.755290 0.887346 11.00000 -1.20000 H11B 2 0.586758 0.780288 0.981844 11.00000 -1.20000 AFIX 0 C9 1 0.767352 0.604173 0.792394 11.00000 0.01566 0.02294 = 0.01027 -0.00216 -0.00124 0.00387 AFIX 23 H9A 2 0.766287 0.544691 0.738299 11.00000 -1.20000 H9B 2 0.813302 0.678602 0.788312 11.00000 -1.20000 AFIX 0 C8 1 0.798613 1.059188 1.121663 11.00000 0.01739 0.01212 = 0.01835 -0.00450 -0.00258 -0.00085 AFIX 43 H8 2 0.839517 1.137003 1.122809 11.00000 -1.20000 AFIX 0 C18 1 0.962613 0.887852 1.063159 11.00000 0.01202 0.01792 = 0.03728 -0.00412 -0.00444 -0.00109 AFIX 137 H18A 2 0.971601 0.973389 1.102519 11.00000 -1.50000 H18B 2 1.010344 0.878239 1.024433 11.00000 -1.50000 H18C 2 0.956237 0.793864 1.096425 11.00000 -1.50000 AFIX 0 C6 1 0.669088 0.957854 1.172546 11.00000 0.01728 0.01680 = 0.01371 -0.00457 0.00218 0.00132 AFIX 43 H6 2 0.620954 0.966807 1.207506 11.00000 -1.20000 AFIX 0 C12 1 0.582908 0.554301 0.946548 11.00000 0.00950 0.02285 = 0.01827 -0.00538 -0.00051 -0.00087 AFIX 23 H12A 2 0.530988 0.539274 0.979559 11.00000 -1.20000 H12B 2 0.577559 0.498252 0.891559 11.00000 -1.20000 AFIX 0 C10 1 0.686024 0.688628 0.802191 11.00000 0.01800 0.02547 = 0.01082 -0.00203 -0.00254 0.00690 AFIX 23 H10A 2 0.682705 0.769081 0.757737 11.00000 -1.20000 H10B 2 0.639556 0.616998 0.792391 11.00000 -1.20000 AFIX 0 C7 1 0.728252 1.071913 1.173220 11.00000 0.02118 0.01334 = 0.01696 -0.00677 0.00031 0.00043 AFIX 43 H7 2 0.720889 1.158763 1.208794 11.00000 -1.20000 AFIX 0 C19 1 0.897936 1.061867 0.956962 11.00000 0.02245 0.01400 = 0.03320 0.00421 0.00849 -0.00504 AFIX 137 H19A 2 0.846679 1.089413 0.926779 11.00000 -1.50000 H19B 2 0.942193 1.044020 0.914881 11.00000 -1.50000 H19C 2 0.914157 1.144894 0.995545 11.00000 -1.50000 AFIX 0 C16 1 0.682543 0.927231 0.882205 11.00000 0.02335 0.01823 = 0.01854 0.00289 -0.00115 0.00619 AFIX 137 H16A 2 0.635370 0.965552 0.848799 11.00000 -1.50000 H16B 2 0.734431 0.954141 0.853012 11.00000 -1.50000 H16C 2 0.681833 0.972874 0.939747 11.00000 -1.50000 HKLF 4 REM lm23312/lt/x8/Fengrui/Me3tacnPd(IV) in Pca2(1) REM R1 = 0.0196 for 12029 Fo > 4sig(Fo) and 0.0218 for all 12564 data REM 238 parameters refined using 10 restraints END WGHT 0.0167 0.7307 REM Highest difference peak 1.407, deepest hole -0.690, 1-sigma level 0.106 Q1 1 0.7532 0.6016 1.0022 11.00000 0.05 1.41 Q2 1 0.7299 0.6584 0.9961 11.00000 0.05 1.05 Q3 1 0.5272 0.3322 0.7165 11.00000 0.05 0.94 Q4 1 0.8225 0.5178 1.0693 11.00000 0.05 0.93 Q5 1 0.4920 0.2284 0.7504 11.00000 0.05 0.91 Q6 1 0.7434 0.6209 0.9561 11.00000 0.05 0.85 Q7 1 0.8580 0.4370 1.0656 11.00000 0.05 0.84 Q8 1 0.5209 0.2076 0.7740 11.00000 0.05 0.81 Q9 1 0.5280 0.2149 0.7168 11.00000 0.05 0.75 Q10 1 0.8284 0.5093 1.1225 11.00000 0.05 0.71 ; _[local]_cod_data_source_file c3cc49387c.txt _[local]_cod_data_source_block l23312 _[local]_cod_cif_authors_sg_H-M Pca2(1) _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'no' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_original_cell_volume 2200.3(6) _cod_database_code 7112073 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.76466(2) 0.65269(3) 0.978732(10) 0.00786(3) Uani 0.967(2) 1 d PDU A 1 I1 I 0.858396(13) 0.50876(5) 1.086958(9) 0.01060(4) Uani 0.967(2) 1 d PDU A 1 Pd1' Pd 0.7490(5) 0.6673(7) 0.9774(4) 0.00786(3) Uani 0.033(2) 1 d PDU A 2 I1' I 0.8504(3) 0.5433(11) 1.0837(4) 0.01060(4) Uani 0.033(2) 1 d PDU A 2 I2 I 0.523695(6) 0.272226(13) 0.746431(9) 0.01809(2) Uani 1 1 d . . . N1 N 0.78306(8) 0.49998(15) 0.86583(9) 0.0120(2) Uani 1 1 d D . . N2 N 0.67651(8) 0.76007(16) 0.88983(9) 0.0142(2) Uani 1 1 d D . . C3 C 0.80955(9) 0.93278(17) 1.06821(10) 0.0128(3) Uani 1 1 d . A . N3 N 0.65420(8) 0.49029(15) 0.99667(10) 0.0128(2) Uani 1 1 d D . . C4 C 0.74935(9) 0.81765(16) 1.06791(10) 0.0106(2) Uani 1 1 d D . . C17 C 0.62694(9) 0.45056(18) 1.08472(13) 0.0167(3) Uani 1 1 d . A . H17A H 0.6005 0.5391 1.1114 0.025 Uiso 1 1 calc R . . H17B H 0.6751 0.4198 1.1190 0.025 Uiso 1 1 calc R . . H17C H 0.5871 0.3664 1.0820 0.025 Uiso 1 1 calc R . . C5 C 0.67981(9) 0.82989(17) 1.12080(11) 0.0129(2) Uani 1 1 d . A . H5 H 0.6396 0.7508 1.1216 0.016 Uiso 1 1 calc R . . C1 C 0.86537(9) 0.78608(18) 0.94718(12) 0.0141(3) Uani 1 1 d D . . H1A H 0.9151 0.7202 0.9437 0.017 Uiso 1 1 calc R A 1 H1B H 0.8560 0.8298 0.8892 0.017 Uiso 1 1 calc R A 1 C14 C 0.72133(9) 0.37421(18) 0.86760(11) 0.0152(3) Uani 1 1 d . A . H14A H 0.7482 0.2795 0.8474 0.018 Uiso 1 1 calc R . . H14B H 0.6755 0.3984 0.8274 0.018 Uiso 1 1 calc R . . C13 C 0.68583(10) 0.34798(18) 0.95627(12) 0.0156(3) Uani 1 1 d . A . H13A H 0.6399 0.2735 0.9522 0.019 Uiso 1 1 calc R . . H13B H 0.7294 0.3036 0.9936 0.019 Uiso 1 1 calc R . . C15 C 0.86781(9) 0.43649(18) 0.85649(11) 0.0136(2) Uani 1 1 d . A . H15A H 0.8707 0.3748 0.8040 0.020 Uiso 1 1 calc R . . H15B H 0.8808 0.3729 0.9065 0.020 Uiso 1 1 calc R . . H15C H 0.9080 0.5199 0.8527 0.020 Uiso 1 1 calc R . . C2 C 0.88346(9) 0.91625(18) 1.00985(12) 0.0144(3) Uani 1 1 d . A . C11 C 0.59388(9) 0.7223(2) 0.92771(12) 0.0164(3) Uani 1 1 d D A . H11A H 0.5499 0.7553 0.8873 0.020 Uiso 1 1 calc R . . H11B H 0.5868 0.7803 0.9818 0.020 Uiso 1 1 calc R . . C9 C 0.76735(10) 0.6042(2) 0.79239(11) 0.0163(3) Uani 1 1 d . A . H9A H 0.7663 0.5447 0.7383 0.020 Uiso 1 1 calc R . . H9B H 0.8133 0.6786 0.7883 0.020 Uiso 1 1 calc R . . C8 C 0.79861(10) 1.05919(18) 1.12166(12) 0.0160(3) Uani 1 1 d . . . H8 H 0.8395 1.1370 1.1228 0.019 Uiso 1 1 calc R A . C18 C 0.96261(10) 0.8879(2) 1.06316(14) 0.0224(4) Uani 1 1 d . . . H18A H 0.9716 0.9734 1.1025 0.034 Uiso 1 1 calc R A . H18B H 1.0103 0.8782 1.0244 0.034 Uiso 1 1 calc R . . H18C H 0.9562 0.7939 1.0964 0.034 Uiso 1 1 calc R . . C6 C 0.66909(10) 0.95785(19) 1.17255(11) 0.0159(3) Uani 1 1 d . . . H6 H 0.6210 0.9668 1.2075 0.019 Uiso 1 1 calc R A . C12 C 0.58291(9) 0.5543(2) 0.94655(12) 0.0169(3) Uani 1 1 d . A . H12A H 0.5310 0.5393 0.9796 0.020 Uiso 1 1 calc R . . H12B H 0.5776 0.4983 0.8916 0.020 Uiso 1 1 calc R . . C10 C 0.68602(11) 0.6886(2) 0.80219(11) 0.0181(3) Uani 1 1 d . A . H10A H 0.6827 0.7691 0.7577 0.022 Uiso 1 1 calc R . . H10B H 0.6396 0.6170 0.7924 0.022 Uiso 1 1 calc R . . C7 C 0.72825(11) 1.07191(19) 1.17322(12) 0.0172(3) Uani 1 1 d . A . H7 H 0.7209 1.1588 1.2088 0.021 Uiso 1 1 calc R . . C19 C 0.89794(12) 1.0619(2) 0.95696(15) 0.0232(4) Uani 1 1 d . . . H19A H 0.8467 1.0894 0.9268 0.035 Uiso 1 1 calc R A . H19B H 0.9422 1.0440 0.9149 0.035 Uiso 1 1 calc R . . H19C H 0.9142 1.1449 0.9955 0.035 Uiso 1 1 calc R . . C16 C 0.68254(12) 0.9272(2) 0.88220(12) 0.0200(3) Uani 1 1 d . A . H16A H 0.6354 0.9656 0.8488 0.030 Uiso 1 1 calc R . . H16B H 0.7344 0.9541 0.8530 0.030 Uiso 1 1 calc R . . H16C H 0.6818 0.9729 0.9397 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.00644(7) 0.00846(5) 0.00869(4) -0.00132(4) 0.00013(5) -0.00007(5) I1 0.01056(4) 0.01021(9) 0.01103(4) -0.00028(5) -0.00018(4) 0.00066(5) Pd1' 0.00644(7) 0.00846(5) 0.00869(4) -0.00132(4) 0.00013(5) -0.00007(5) I1' 0.01056(4) 0.01021(9) 0.01103(4) -0.00028(5) -0.00018(4) 0.00066(5) I2 0.01093(3) 0.02389(5) 0.01945(5) -0.00863(4) 0.00000(4) -0.00067(3) N1 0.0100(5) 0.0150(5) 0.0112(6) -0.0031(4) 0.0002(4) 0.0010(4) N2 0.0128(5) 0.0178(6) 0.0121(6) -0.0017(5) -0.0009(4) 0.0039(4) C3 0.0113(5) 0.0102(5) 0.0170(7) -0.0009(5) -0.0013(5) -0.0011(4) N3 0.0101(4) 0.0137(5) 0.0145(6) -0.0043(4) 0.0010(4) -0.0025(4) C4 0.0107(5) 0.0095(5) 0.0118(6) -0.0009(4) 0.0001(4) -0.0003(4) C17 0.0159(6) 0.0179(6) 0.0165(7) -0.0041(6) 0.0037(6) -0.0072(5) C5 0.0123(5) 0.0139(6) 0.0126(7) -0.0025(5) 0.0012(5) -0.0012(4) C1 0.0123(6) 0.0137(6) 0.0164(7) 0.0001(5) 0.0042(5) -0.0021(4) C14 0.0120(6) 0.0167(6) 0.0169(7) -0.0084(6) -0.0002(5) -0.0021(5) C13 0.0131(6) 0.0139(6) 0.0198(8) -0.0070(5) 0.0028(5) -0.0040(5) C15 0.0105(5) 0.0157(6) 0.0146(7) -0.0023(5) 0.0012(5) 0.0024(4) C2 0.0105(5) 0.0110(6) 0.0216(8) 0.0004(5) 0.0022(5) -0.0027(4) C11 0.0103(5) 0.0223(7) 0.0164(7) -0.0042(6) -0.0014(5) 0.0050(5) C9 0.0157(6) 0.0229(7) 0.0103(6) -0.0022(5) -0.0012(5) 0.0039(5) C8 0.0174(6) 0.0121(6) 0.0183(8) -0.0045(5) -0.0026(5) -0.0009(5) C18 0.0120(6) 0.0179(7) 0.0373(11) -0.0041(7) -0.0044(6) -0.0011(5) C6 0.0173(6) 0.0168(7) 0.0137(7) -0.0046(5) 0.0022(5) 0.0013(5) C12 0.0095(5) 0.0228(7) 0.0183(7) -0.0054(6) -0.0005(5) -0.0009(5) C10 0.0180(7) 0.0255(8) 0.0108(7) -0.0020(6) -0.0025(5) 0.0069(6) C7 0.0212(7) 0.0133(6) 0.0170(8) -0.0068(5) 0.0003(5) 0.0004(5) C19 0.0224(8) 0.0140(7) 0.0332(11) 0.0042(6) 0.0085(7) -0.0050(6) C16 0.0234(7) 0.0182(7) 0.0185(8) 0.0029(6) -0.0012(6) 0.0062(6) 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 C4 Pd1 C1 81.42(6) C4 Pd1 N2 92.52(6) C1 Pd1 N2 96.60(6) C4 Pd1 N1 171.17(6) C1 Pd1 N1 92.91(6) N2 Pd1 N1 81.36(5) C4 Pd1 N3 105.56(6) C1 Pd1 N3 172.63(6) N2 Pd1 N3 80.94(6) N1 Pd1 N3 79.88(5) C4 Pd1 I1 88.66(4) C1 Pd1 I1 88.48(5) N2 Pd1 I1 174.90(4) N1 Pd1 I1 97.99(4) N3 Pd1 I1 93.97(4) C4 Pd1' N2 102.8(4) C4 Pd1' C1 80.1(2) N2 Pd1' C1 99.3(3) C4 Pd1' N3 112.8(3) N2 Pd1' N3 88.6(3) C1 Pd1' N3 163.2(4) C4 Pd1' N1 165.9(4) N2 Pd1' N1 83.5(2) C1 Pd1' N1 86.6(3) N3 Pd1' N1 79.58(19) C4 Pd1' I1' 79.6(3) N2 Pd1' I1' 176.2(3) C1 Pd1' I1' 78.2(3) N3 Pd1' I1' 93.1(2) N1 Pd1' I1' 93.5(2) C15 N1 C9 108.30(13) C15 N1 C14 109.74(12) C9 N1 C14 111.03(13) C15 N1 Pd1 115.25(10) C9 N1 Pd1 102.15(9) C14 N1 Pd1 110.14(10) C15 N1 Pd1' 121.7(2) C9 N1 Pd1' 98.14(19) C14 N1 Pd1' 107.26(17) C16 N2 C11 108.14(13) C16 N2 C10 109.59(14) C11 N2 C10 110.75(13) C16 N2 Pd1' 115.36(19) C11 N2 Pd1' 99.4(2) C10 N2 Pd1' 113.0(2) C16 N2 Pd1 115.83(11) C11 N2 Pd1 103.49(10) C10 N2 Pd1 108.88(9) C8 C3 C4 119.25(15) C8 C3 C2 122.32(14) C4 C3 C2 118.42(13) C17 N3 C13 107.04(13) C17 N3 C12 110.00(12) C13 N3 C12 111.04(13) C17 N3 Pd1' 119.93(19) C13 N3 Pd1' 107.4(2) C12 N3 Pd1' 101.3(2) C17 N3 Pd1 119.27(10) C13 N3 Pd1 101.88(9) C12 N3 Pd1 107.30(10) C5 C4 C3 119.90(14) C5 C4 Pd1' 118.7(2) C3 C4 Pd1' 120.0(2) C5 C4 Pd1 123.91(11) C3 C4 Pd1 115.85(11) N3 C17 H17A 109.5 N3 C17 H17B 109.5 H17A C17 H17B 109.5 N3 C17 H17C 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 C4 C5 C6 120.15(14) C4 C5 H5 119.9 C6 C5 H5 119.9 C2 C1 Pd1 115.08(11) C2 C1 Pd1' 112.4(2) C2 C1 H1A 108.5 Pd1 C1 H1A 108.5 Pd1' C1 H1A 115.1 C2 C1 H1B 108.5 Pd1 C1 H1B 108.5 Pd1' C1 H1B 104.4 H1A C1 H1B 107.5 N1 C14 C13 112.57(13) N1 C14 H14A 109.1 C13 C14 H14A 109.1 N1 C14 H14B 109.1 C13 C14 H14B 109.1 H14A C14 H14B 107.8 N3 C13 C14 112.70(14) N3 C13 H13A 109.1 C14 C13 H13A 109.1 N3 C13 H13B 109.1 C14 C13 H13B 109.1 H13A C13 H13B 107.8 N1 C15 H15A 109.5 N1 C15 H15B 109.5 H15A C15 H15B 109.5 N1 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 C3 C2 C1 107.77(12) C3 C2 C19 111.20(13) C1 C2 C19 108.12(16) C3 C2 C18 110.30(15) C1 C2 C18 112.23(13) C19 C2 C18 107.24(14) N2 C11 C12 113.36(13) N2 C11 H11A 108.9 C12 C11 H11A 108.9 N2 C11 H11B 108.9 C12 C11 H11B 108.9 H11A C11 H11B 107.7 N1 C9 C10 111.89(14) N1 C9 H9A 109.2 C10 C9 H9A 109.2 N1 C9 H9B 109.2 C10 C9 H9B 109.2 H9A C9 H9B 107.9 C7 C8 C3 120.53(15) C7 C8 H8 119.7 C3 C8 H8 119.7 C2 C18 H18A 109.5 C2 C18 H18B 109.5 H18A C18 H18B 109.5 C2 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 C7 C6 C5 120.27(15) C7 C6 H6 119.9 C5 C6 H6 119.9 N3 C12 C11 112.16(13) N3 C12 H12A 109.2 C11 C12 H12A 109.2 N3 C12 H12B 109.2 C11 C12 H12B 109.2 H12A C12 H12B 107.9 N2 C10 C9 112.54(13) N2 C10 H10A 109.1 C9 C10 H10A 109.1 N2 C10 H10B 109.1 C9 C10 H10B 109.1 H10A C10 H10B 107.8 C6 C7 C8 119.88(15) C6 C7 H7 120.1 C8 C7 H7 120.1 C2 C19 H19A 109.5 C2 C19 H19B 109.5 H19A C19 H19B 109.5 C2 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 N2 C16 H16A 109.5 N2 C16 H16B 109.5 H16A C16 H16B 109.5 N2 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Pd1 C4 2.0207(15) Pd1 C1 2.0610(15) Pd1 N2 2.1944(14) Pd1 N1 2.2287(14) Pd1 N3 2.2983(13) Pd1 I1 2.5902(3) Pd1' C4 1.930(6) Pd1' N2 1.970(8) Pd1' C1 2.197(6) Pd1' N3 2.200(6) Pd1' N1 2.339(7) Pd1' I1' 2.565(4) N1 C15 1.4821(19) N1 C9 1.485(2) N1 C14 1.487(2) N2 C16 1.478(2) N2 C11 1.493(2) N2 C10 1.507(2) C3 C8 1.398(2) C3 C4 1.402(2) C3 C2 1.504(2) N3 C17 1.479(2) N3 C13 1.490(2) N3 C12 1.497(2) C4 C5 1.393(2) C17 H17A 0.9800 C17 H17B 0.9800 C17 H17C 0.9800 C5 C6 1.393(2) C5 H5 0.9500 C1 C2 1.531(2) C1 H1A 0.9900 C1 H1B 0.9900 C14 C13 1.509(2) C14 H14A 0.9900 C14 H14B 0.9900 C13 H13A 0.9900 C13 H13B 0.9900 C15 H15A 0.9800 C15 H15B 0.9800 C15 H15C 0.9800 C2 C19 1.539(2) C2 C18 1.541(2) C11 C12 1.516(3) C11 H11A 0.9900 C11 H11B 0.9900 C9 C10 1.514(2) C9 H9A 0.9900 C9 H9B 0.9900 C8 C7 1.392(2) C8 H8 0.9500 C18 H18A 0.9800 C18 H18B 0.9800 C18 H18C 0.9800 C6 C7 1.383(2) C6 H6 0.9500 C12 H12A 0.9900 C12 H12B 0.9900 C10 H10A 0.9900 C10 H10B 0.9900 C7 H7 0.9500 C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 C16 H16A 0.9800 C16 H16B 0.9800 C16 H16C 0.9800 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 C1 Pd1 N1 C15 52.02(12) N2 Pd1 N1 C15 148.26(12) N3 Pd1 N1 C15 -129.48(12) I1 Pd1 N1 C15 -36.85(11) C1 Pd1 N1 C9 -65.15(10) N2 Pd1 N1 C9 31.09(9) N3 Pd1 N1 C9 113.35(10) I1 Pd1 N1 C9 -154.02(9) C1 Pd1 N1 C14 176.82(11) N2 Pd1 N1 C14 -86.94(11) N3 Pd1 N1 C14 -4.68(10) I1 Pd1 N1 C14 87.95(10) C1 Pd1 N1 Pd1' -118.1(12) N2 Pd1 N1 Pd1' -21.9(12) N3 Pd1 N1 Pd1' 60.4(12) I1 Pd1 N1 Pd1' 153.0(12) C4 Pd1' N1 C15 27.4(16) N2 Pd1' N1 C15 145.11(17) C1 Pd1' N1 C15 45.4(3) N3 Pd1' N1 C15 -125.12(18) I1' Pd1' N1 C15 -32.6(3) C4 Pd1' N1 C9 -90.1(15) N2 Pd1' N1 C9 27.6(2) C1 Pd1' N1 C9 -72.1(2) N3 Pd1' N1 C9 117.40(18) I1' Pd1' N1 C9 -150.1(2) C4 Pd1' N1 C14 154.8(14) N2 Pd1' N1 C14 -87.45(19) C1 Pd1' N1 C14 172.80(17) N3 Pd1' N1 C14 2.3(2) I1' Pd1' N1 C14 94.8(3) C4 Pd1' N1 Pd1 37.9(11) N2 Pd1' N1 Pd1 155.6(13) C1 Pd1' N1 Pd1 55.9(11) N3 Pd1' N1 Pd1 -114.6(13) I1' Pd1' N1 Pd1 -22.1(11) C4 Pd1' N2 C16 35.4(3) C1 Pd1' N2 C16 -46.4(3) N3 Pd1' N2 C16 148.51(15) N1 Pd1' N2 C16 -131.82(15) C4 Pd1' N2 C11 -79.9(3) C1 Pd1' N2 C11 -161.7(2) N3 Pd1' N2 C11 33.2(2) N1 Pd1' N2 C11 112.83(16) C4 Pd1' N2 C10 162.6(2) C1 Pd1' N2 C10 80.8(2) N3 Pd1' N2 C10 -84.3(2) N1 Pd1' N2 C10 -4.6(2) C4 Pd1' N2 Pd1 132(2) C1 Pd1' N2 Pd1 50.4(18) N3 Pd1' N2 Pd1 -114.7(19) N1 Pd1' N2 Pd1 -35.1(18) C4 Pd1 N2 C16 41.84(12) C1 Pd1 N2 C16 -39.81(13) N1 Pd1 N2 C16 -131.76(12) N3 Pd1 N2 C16 147.20(12) C4 Pd1 N2 C11 -76.31(10) C1 Pd1 N2 C11 -157.96(10) N1 Pd1 N2 C11 110.08(10) N3 Pd1 N2 C11 29.05(10) C4 Pd1 N2 C10 165.85(11) C1 Pd1 N2 C10 84.19(12) N1 Pd1 N2 C10 -7.76(11) N3 Pd1 N2 C10 -88.80(11) C4 Pd1 N2 Pd1' -43.7(19) C1 Pd1 N2 Pd1' -125.3(19) N1 Pd1 N2 Pd1' 142.7(19) N3 Pd1 N2 Pd1' 61.7(19) C4 Pd1' N3 C17 -28.1(5) N2 Pd1' N3 C17 -131.41(18) C1 Pd1' N3 C17 110.1(11) N1 Pd1' N3 C17 144.89(14) I1' Pd1' N3 C17 51.9(2) C4 Pd1' N3 C13 -150.5(3) N2 Pd1' N3 C13 106.2(2) C1 Pd1' N3 C13 -12.3(13) N1 Pd1' N3 C13 22.6(2) I1' Pd1' N3 C13 -70.4(2) C4 Pd1' N3 C12 93.0(3) N2 Pd1' N3 C12 -10.3(3) C1 Pd1' N3 C12 -128.8(12) N1 Pd1' N3 C12 -93.95(19) I1' Pd1' N3 C12 173.10(18) C4 Pd1' N3 Pd1 -114.5(16) N2 Pd1' N3 Pd1 142.2(16) C1 Pd1' N3 Pd1 23.7(7) N1 Pd1' N3 Pd1 58.6(14) I1' Pd1' N3 Pd1 -34.4(13) C4 Pd1 N3 C17 -41.21(12) N2 Pd1 N3 C17 -131.31(12) N1 Pd1 N3 C17 145.93(12) I1 Pd1 N3 C17 48.50(11) C4 Pd1 N3 C13 -158.67(10) N2 Pd1 N3 C13 111.23(11) N1 Pd1 N3 C13 28.46(10) I1 Pd1 N3 C13 -68.96(10) C4 Pd1 N3 C12 84.60(11) N2 Pd1 N3 C12 -5.50(10) N1 Pd1 N3 C12 -88.26(10) I1 Pd1 N3 C12 174.32(10) C4 Pd1 N3 Pd1' 56.3(14) N2 Pd1 N3 Pd1' -33.8(14) N1 Pd1 N3 Pd1' -116.6(14) I1 Pd1 N3 Pd1' 146.0(14) C8 C3 C4 C5 -0.3(2) C2 C3 C4 C5 -179.58(15) C8 C3 C4 Pd1' 165.7(3) C2 C3 C4 Pd1' -13.6(3) C8 C3 C4 Pd1 173.26(12) C2 C3 C4 Pd1 -6.06(18) N2 Pd1' C4 C5 76.0(3) C1 Pd1' C4 C5 173.33(14) N3 Pd1' C4 C5 -17.9(5) N1 Pd1' C4 C5 -168.4(14) I1' Pd1' C4 C5 -107.0(3) N2 Pd1' C4 C3 -90.2(3) C1 Pd1' C4 C3 7.2(3) N3 Pd1' C4 C3 175.9(2) N1 Pd1' C4 C3 25.4(16) I1' Pd1' C4 C3 86.9(2) N2 Pd1' C4 Pd1 -150.4(14) C1 Pd1' C4 Pd1 -53.0(12) N3 Pd1' C4 Pd1 115.7(14) N1 Pd1' C4 Pd1 -34.8(11) I1' Pd1' C4 Pd1 26.7(12) C1 Pd1 C4 C5 171.86(14) N2 Pd1 C4 C5 75.56(14) N3 Pd1 C4 C5 -5.74(14) I1 Pd1 C4 C5 -99.48(13) C1 Pd1 C4 C3 -1.37(12) N2 Pd1 C4 C3 -97.67(12) N3 Pd1 C4 C3 -178.97(11) I1 Pd1 C4 C3 87.29(11) C1 Pd1 C4 Pd1' 122.0(13) N2 Pd1 C4 Pd1' 25.7(13) N3 Pd1 C4 Pd1' -55.6(13) I1 Pd1 C4 Pd1' -149.4(13) C3 C4 C5 C6 1.4(2) Pd1' C4 C5 C6 -164.7(3) Pd1 C4 C5 C6 -171.56(12) C4 Pd1 C1 C2 8.25(12) N2 Pd1 C1 C2 99.81(12) N1 Pd1 C1 C2 -178.55(12) I1 Pd1 C1 C2 -80.63(11) C4 Pd1 C1 Pd1' -60.1(14) N2 Pd1 C1 Pd1' 31.5(14) N1 Pd1 C1 Pd1' 113.1(14) I1 Pd1 C1 Pd1' -148.9(14) C4 Pd1' C1 C2 0.0(3) N2 Pd1' C1 C2 101.5(2) N3 Pd1' C1 C2 -141.4(11) N1 Pd1' C1 C2 -175.67(15) I1' Pd1' C1 C2 -81.41(19) C4 Pd1' C1 Pd1 114.4(15) N2 Pd1' C1 Pd1 -144.1(16) N3 Pd1' C1 Pd1 -27.0(8) N1 Pd1' C1 Pd1 -61.3(14) I1' Pd1' C1 Pd1 33.0(13) C15 N1 C14 C13 106.80(15) C9 N1 C14 C13 -133.50(14) Pd1 N1 C14 C13 -21.10(16) Pd1' N1 C14 C13 -27.3(2) C17 N3 C13 C14 -176.11(13) C12 N3 C13 C14 63.81(16) Pd1' N3 C13 C14 -46.1(2) Pd1 N3 C13 C14 -50.17(14) N1 C14 C13 N3 51.02(18) C8 C3 C2 C1 -167.21(15) C4 C3 C2 C1 12.1(2) C8 C3 C2 C19 -48.9(2) C4 C3 C2 C19 130.41(16) C8 C3 C2 C18 69.96(19) C4 C3 C2 C18 -110.75(16) Pd1 C1 C2 C3 -12.77(16) Pd1' C1 C2 C3 -6.0(3) Pd1 C1 C2 C19 -133.06(12) Pd1' C1 C2 C19 -126.3(2) Pd1 C1 C2 C18 108.86(14) Pd1' C1 C2 C18 115.6(2) C16 N2 C11 C12 -174.71(14) C10 N2 C11 C12 65.19(18) Pd1' N2 C11 C12 -54.0(2) Pd1 N2 C11 C12 -51.34(15) C15 N1 C9 C10 -173.27(14) C14 N1 C9 C10 66.18(17) Pd1 N1 C9 C10 -51.21(15) Pd1' N1 C9 C10 -45.9(2) C4 C3 C8 C7 -0.9(2) C2 C3 C8 C7 178.42(16) C4 C5 C6 C7 -1.4(3) C17 N3 C12 C11 111.17(15) C13 N3 C12 C11 -130.52(15) Pd1' N3 C12 C11 -16.7(2) Pd1 N3 C12 C11 -19.99(16) N2 C11 C12 N3 50.14(19) C16 N2 C10 C9 109.77(17) C11 N2 C10 C9 -131.01(16) Pd1' N2 C10 C9 -20.4(3) Pd1 N2 C10 C9 -17.85(18) N1 C9 C10 N2 49.0(2) C5 C6 C7 C8 0.3(3) C3 C8 C7 C6 0.8(3)