#------------------------------------------------------------------------------ #$Date: 2014-03-11 07:04:49 +0000 (Tue, 11 Mar 2014) $ #$Revision: 104428 $ #$URL: svn://www.crystallography.net/cod/cif/7/11/20/7112072.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_7112072 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_volume 50 _journal_year 2014 _chemical_formula_moiety 'C19 H34 N3 O Pd, Cl O4' _chemical_formula_sum 'C19 H34 Cl N3 O5 Pd' _chemical_formula_weight 526.34 _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 16.768(5) _cell_length_b 8.477(2) _cell_length_c 14.704(4) _cell_measurement_reflns_used 9351 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.15 _cell_measurement_theta_min 2.69 _cell_volume 2090.1(10) _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 0.992 _diffrn_measured_fraction_theta_max 0.992 _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 0.0682 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 54583 _diffrn_reflns_theta_full 27.58 _diffrn_reflns_theta_max 27.58 _diffrn_reflns_theta_min 2.40 _exptl_absorpt_coefficient_mu 1.052 _exptl_absorpt_correction_T_max 0.8675 _exptl_absorpt_correction_T_min 0.8324 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'sadabs v2008/1' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_meas no _exptl_crystal_density_method 'not measured' _exptl_crystal_description rectangular _exptl_crystal_F_000 1088 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _refine_diff_density_max 0.273 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.060 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.005(18) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 268 _refine_ls_number_reflns 4780 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0215 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+0.3130P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.0498 _reflns_number_gt 4446 _reflns_number_total 4780 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL lm15612/lt/smart/Fengrui/Me3tacnPdIVOH in Pca2(1) CELL 0.71073 16.7685 8.4769 14.7041 90.000 90.000 90.000 ZERR 4.00 0.0045 0.0024 0.0043 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 O CL PD UNIT 76 136 12 20 4 4 TEMP -173.140 SIZE 0.139 0.148 0.181 OMIT -3.0 L.S. 10 PLAN 5 EQIV $1 -x+1, -y+1, z+1/2 HTAB C12 O1_$1 EQIV $2 x+1/2, -y+1, z HTAB C15 O3_$2 HTAB C17 O1 EQIV $3 x, y-1, z HTAB C18 O2_$3 HTAB C18 O4_$3 HTAB C19 O3_$2 EQIV $4 -x+1, -y+1, z-1/2 HTAB O1 O5_$4 acta wpdb -2 list 4 bond $h htab conf more 2 fmap 2 WGHT 0.023900 0.313000 FVAR 0.12600 PD1 6 0.517330 0.396461 0.499806 11.00000 0.01418 0.01038 = 0.01335 -0.00072 -0.00016 0.00005 CL1 5 0.339192 0.952540 0.729491 11.00000 0.02516 0.01957 = 0.02129 0.00155 0.00308 -0.00187 O1 4 0.569084 0.383226 0.376104 11.00000 0.02062 0.01356 = 0.01426 0.00190 0.00057 -0.00109 AFIX 147 H1 2 0.591693 0.295355 0.370398 11.00000 -1.50000 AFIX 0 rem located H1 2 0.589574 0.292207 0.379915 11.00000 0.04634 O2 4 0.281644 1.072925 0.709606 11.00000 0.03532 0.02929 = 0.05313 0.00533 0.01087 0.01167 O3 4 0.306656 0.801346 0.703521 11.00000 0.04284 0.02307 = 0.06958 -0.00587 -0.00856 -0.01025 O4 4 0.411291 0.980216 0.679858 11.00000 0.02846 0.03256 = 0.04209 0.01388 0.01264 0.00257 O5 4 0.356735 0.948680 0.825050 11.00000 0.06724 0.06903 = 0.02438 -0.00076 -0.00162 0.00444 N1 3 0.584469 0.623408 0.526381 11.00000 0.01643 0.01476 = 0.02010 -0.00322 -0.00081 -0.00058 N2 3 0.473128 0.439956 0.632282 11.00000 0.01862 0.01574 = 0.01709 -0.00107 0.00176 0.00149 N3 3 0.620868 0.300025 0.576629 11.00000 0.01612 0.01639 = 0.01534 -0.00139 0.00070 0.00096 C1 1 0.416108 0.462516 0.435162 11.00000 0.01670 0.01610 = 0.01495 0.00090 -0.00085 -0.00006 C2 1 0.390528 0.618382 0.424122 11.00000 0.02438 0.01332 = 0.02033 -0.00015 -0.00007 -0.00058 AFIX 43 H2 2 0.420006 0.701896 0.451067 11.00000 -1.20000 AFIX 0 C3 1 0.322424 0.652021 0.374117 11.00000 0.02169 0.01710 = 0.01867 0.00283 0.00336 0.00538 AFIX 43 H3 2 0.305725 0.758446 0.367245 11.00000 -1.20000 AFIX 0 C4 1 0.278433 0.532078 0.334039 11.00000 0.01847 0.02253 = 0.01722 0.00180 -0.00108 0.00292 AFIX 43 H4 2 0.232248 0.556099 0.299279 11.00000 -1.20000 AFIX 0 C5 1 0.302745 0.375466 0.345311 11.00000 0.01970 0.01816 = 0.01826 0.00084 -0.00091 -0.00298 AFIX 43 H5 2 0.272785 0.292939 0.318050 11.00000 -1.20000 AFIX 0 C6 1 0.370887 0.339008 0.396437 11.00000 0.01557 0.01461 = 0.01666 0.00004 0.00099 -0.00062 C7 1 0.397293 0.171387 0.414715 11.00000 0.02142 0.01076 = 0.01818 -0.00029 -0.00151 -0.00241 C8 1 0.467941 0.176326 0.480811 11.00000 0.02047 0.01081 = 0.02283 0.00046 -0.00237 -0.00164 AFIX 23 H8A 2 0.509927 0.104384 0.457998 11.00000 -1.20000 H8B 2 0.450018 0.135558 0.540501 11.00000 -1.20000 AFIX 0 C9 1 0.327846 0.078456 0.458643 11.00000 0.02265 0.01778 = 0.02776 0.00292 0.00035 -0.00471 AFIX 137 H9A 2 0.283849 0.069464 0.415081 11.00000 -1.50000 H9B 2 0.309364 0.134241 0.513081 11.00000 -1.50000 H9C 2 0.346338 -0.027199 0.475592 11.00000 -1.50000 AFIX 0 C10 1 0.421566 0.087959 0.326067 11.00000 0.02667 0.01789 = 0.02152 -0.00060 -0.00174 0.00252 AFIX 137 H10A 2 0.466424 0.144189 0.298243 11.00000 -1.50000 H10B 2 0.376288 0.087337 0.283928 11.00000 -1.50000 H10C 2 0.437454 -0.020814 0.339536 11.00000 -1.50000 AFIX 0 C11 1 0.554747 0.689556 0.613463 11.00000 0.03057 0.01646 = 0.02637 -0.00918 0.00053 -0.00135 AFIX 23 H11A 2 0.548273 0.805113 0.607091 11.00000 -1.20000 H11B 2 0.594660 0.670037 0.661781 11.00000 -1.20000 AFIX 0 C12 1 0.475014 0.616747 0.641647 11.00000 0.03151 0.01862 = 0.02486 -0.00720 0.00462 0.00286 AFIX 23 H12A 2 0.463932 0.645028 0.705737 11.00000 -1.20000 H12B 2 0.432098 0.662617 0.603718 11.00000 -1.20000 AFIX 0 C13 1 0.527480 0.363658 0.701503 11.00000 0.02844 0.03216 = 0.01416 0.00408 0.00147 0.00546 AFIX 23 H13A 2 0.560263 0.446436 0.730796 11.00000 -1.20000 H13B 2 0.494488 0.313644 0.749316 11.00000 -1.20000 AFIX 0 C14 1 0.581895 0.241187 0.660985 11.00000 0.02374 0.02282 = 0.01663 0.00342 -0.00047 -0.00087 AFIX 23 H14A 2 0.623340 0.212378 0.705967 11.00000 -1.20000 H14B 2 0.550741 0.145104 0.646751 11.00000 -1.20000 AFIX 0 C15 1 0.678195 0.431025 0.597587 11.00000 0.01842 0.02372 = 0.02527 -0.00364 -0.00488 -0.00231 AFIX 23 H15A 2 0.669325 0.468090 0.660628 11.00000 -1.20000 H15B 2 0.733466 0.390612 0.593415 11.00000 -1.20000 AFIX 0 C16 1 0.668266 0.566104 0.533515 11.00000 0.01614 0.01797 = 0.03031 -0.00054 0.00036 -0.00236 AFIX 23 H16A 2 0.702579 0.654297 0.553935 11.00000 -1.20000 H16B 2 0.686792 0.533427 0.472426 11.00000 -1.20000 AFIX 0 C17 1 0.583540 0.741080 0.451934 11.00000 0.02910 0.01739 = 0.02622 0.00494 -0.00171 -0.00463 AFIX 137 H17A 2 0.532101 0.795952 0.451536 11.00000 -1.50000 H17B 2 0.591400 0.687450 0.393576 11.00000 -1.50000 H17C 2 0.626505 0.817701 0.461430 11.00000 -1.50000 AFIX 0 C18 1 0.389429 0.390015 0.649495 11.00000 0.02242 0.02495 = 0.02704 0.00203 0.00762 0.00029 AFIX 137 H18A 2 0.385757 0.274816 0.645773 11.00000 -1.50000 H18B 2 0.354311 0.437510 0.603796 11.00000 -1.50000 H18C 2 0.373081 0.424821 0.710255 11.00000 -1.50000 AFIX 0 C19 1 0.664498 0.170058 0.531756 11.00000 0.02042 0.02352 = 0.02666 -0.00362 -0.00364 0.00721 AFIX 137 H19A 2 0.688508 0.208644 0.475211 11.00000 -1.50000 H19B 2 0.627406 0.083991 0.517940 11.00000 -1.50000 H19C 2 0.706509 0.131362 0.572365 11.00000 -1.50000 HKLF 4 REM lm15612/lt/smart/Fengrui/Me3tacnPdIVOH in Pca2(1) REM R1 = 0.0215 for 4446 Fo > 4sig(Fo) and 0.0247 for all 4780 data REM 268 parameters refined using 1 restraints END WGHT 0.0239 0.3129 REM Highest difference peak 0.273, deepest hole -0.516, 1-sigma level 0.060 Q1 1 0.5828 0.3578 0.3507 11.00000 0.05 0.27 Q2 1 0.4737 0.3982 0.5764 11.00000 0.05 0.27 Q3 1 0.5299 0.3863 0.3805 11.00000 0.05 0.26 Q4 1 0.5776 0.3379 0.5415 11.00000 0.05 0.26 Q5 1 0.4754 0.4016 0.4253 11.00000 0.05 0.24 ; _[local]_cod_data_source_file c3cc49387c.txt _[local]_cod_data_source_block l15612 _[local]_cod_cif_authors_sg_H-M Pca2(1) _cod_database_code 7112072 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 Pd1 Pd 0.517330(9) 0.396461(16) 0.499806(16) 0.01264(5) Uani 1 1 d . Cl1 Cl 0.33919(4) 0.95254(7) 0.72949(4) 0.02201(13) Uani 1 1 d . O1 O 0.56908(11) 0.38323(19) 0.37610(11) 0.0161(4) Uani 1 1 d . H1 H 0.5917 0.2954 0.3704 0.024 Uiso 1 1 calc R O2 O 0.28164(13) 1.0729(2) 0.70961(15) 0.0392(5) Uani 1 1 d . O3 O 0.30666(13) 0.8013(2) 0.70352(16) 0.0452(6) Uani 1 1 d . O4 O 0.41129(13) 0.9802(2) 0.67986(14) 0.0344(5) Uani 1 1 d . O5 O 0.35673(16) 0.9487(3) 0.82505(15) 0.0536(6) Uani 1 1 d . N1 N 0.58447(13) 0.6234(2) 0.52638(13) 0.0171(5) Uani 1 1 d . N2 N 0.47313(12) 0.4400(2) 0.63228(14) 0.0171(4) Uani 1 1 d . N3 N 0.62087(12) 0.3000(2) 0.57663(13) 0.0160(4) Uani 1 1 d . C1 C 0.41611(14) 0.4625(3) 0.43516(16) 0.0159(5) Uani 1 1 d . C2 C 0.39053(16) 0.6184(3) 0.42412(17) 0.0193(5) Uani 1 1 d . H2 H 0.4200 0.7019 0.4511 0.023 Uiso 1 1 calc R C3 C 0.32242(16) 0.6520(3) 0.37412(16) 0.0192(5) Uani 1 1 d . H3 H 0.3057 0.7584 0.3672 0.023 Uiso 1 1 calc R C4 C 0.27843(15) 0.5321(3) 0.33404(16) 0.0194(5) Uani 1 1 d . H4 H 0.2322 0.5561 0.2993 0.023 Uiso 1 1 calc R C5 C 0.30275(15) 0.3755(3) 0.34531(16) 0.0187(5) Uani 1 1 d . H5 H 0.2728 0.2929 0.3180 0.022 Uiso 1 1 calc R C6 C 0.37089(15) 0.3390(3) 0.39644(16) 0.0156(5) Uani 1 1 d . C7 C 0.39729(15) 0.1714(3) 0.41471(16) 0.0168(5) Uani 1 1 d . C8 C 0.46794(14) 0.1763(3) 0.48081(15) 0.0180(6) Uani 1 1 d . H8A H 0.5099 0.1044 0.4580 0.022 Uiso 1 1 calc R H8B H 0.4500 0.1356 0.5405 0.022 Uiso 1 1 calc R C9 C 0.32785(16) 0.0785(3) 0.45864(18) 0.0227(6) Uani 1 1 d . H9A H 0.2838 0.0695 0.4151 0.034 Uiso 1 1 calc R H9B H 0.3094 0.1342 0.5131 0.034 Uiso 1 1 calc R H9C H 0.3463 -0.0272 0.4756 0.034 Uiso 1 1 calc R C10 C 0.42157(17) 0.0880(3) 0.32607(17) 0.0220(6) Uani 1 1 d . H10A H 0.4664 0.1442 0.2982 0.033 Uiso 1 1 calc R H10B H 0.3763 0.0873 0.2839 0.033 Uiso 1 1 calc R H10C H 0.4375 -0.0208 0.3395 0.033 Uiso 1 1 calc R C11 C 0.55475(17) 0.6896(3) 0.61346(17) 0.0245(6) Uani 1 1 d . H11A H 0.5483 0.8051 0.6071 0.029 Uiso 1 1 calc R H11B H 0.5947 0.6700 0.6618 0.029 Uiso 1 1 calc R C12 C 0.47501(17) 0.6167(3) 0.6416(2) 0.0250(6) Uani 1 1 d . H12A H 0.4639 0.6450 0.7057 0.030 Uiso 1 1 calc R H12B H 0.4321 0.6626 0.6037 0.030 Uiso 1 1 calc R C13 C 0.52748(17) 0.3637(3) 0.70150(18) 0.0249(6) Uani 1 1 d . H13A H 0.5603 0.4464 0.7308 0.030 Uiso 1 1 calc R H13B H 0.4945 0.3136 0.7493 0.030 Uiso 1 1 calc R C14 C 0.58189(15) 0.2412(3) 0.66098(16) 0.0211(5) Uani 1 1 d . H14A H 0.6233 0.2124 0.7060 0.025 Uiso 1 1 calc R H14B H 0.5507 0.1451 0.6468 0.025 Uiso 1 1 calc R C15 C 0.67819(16) 0.4310(3) 0.59759(18) 0.0225(6) Uani 1 1 d . H15A H 0.6693 0.4681 0.6606 0.027 Uiso 1 1 calc R H15B H 0.7335 0.3906 0.5934 0.027 Uiso 1 1 calc R C16 C 0.66827(15) 0.5661(3) 0.53352(19) 0.0215(5) Uani 1 1 d . H16A H 0.7026 0.6543 0.5539 0.026 Uiso 1 1 calc R H16B H 0.6868 0.5334 0.4724 0.026 Uiso 1 1 calc R C17 C 0.58354(17) 0.7411(3) 0.45193(17) 0.0242(6) Uani 1 1 d . H17A H 0.5321 0.7960 0.4515 0.036 Uiso 1 1 calc R H17B H 0.5914 0.6874 0.3936 0.036 Uiso 1 1 calc R H17C H 0.6265 0.8177 0.4614 0.036 Uiso 1 1 calc R C18 C 0.38943(17) 0.3900(3) 0.6495(2) 0.0248(6) Uani 1 1 d . H18A H 0.3858 0.2748 0.6458 0.037 Uiso 1 1 calc R H18B H 0.3543 0.4375 0.6038 0.037 Uiso 1 1 calc R H18C H 0.3731 0.4248 0.7103 0.037 Uiso 1 1 calc R C19 C 0.66450(16) 0.1701(3) 0.53176(18) 0.0235(6) Uani 1 1 d . H19A H 0.6885 0.2086 0.4752 0.035 Uiso 1 1 calc R H19B H 0.6274 0.0840 0.5179 0.035 Uiso 1 1 calc R H19C H 0.7065 0.1314 0.5724 0.035 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 0.01418(8) 0.01038(7) 0.01335(7) -0.00072(9) -0.00016(10) 0.00005(6) Cl1 0.0252(3) 0.0196(3) 0.0213(3) 0.0015(2) 0.0031(3) -0.0019(3) O1 0.0206(10) 0.0136(8) 0.0143(8) 0.0019(6) 0.0006(7) -0.0011(7) O2 0.0353(13) 0.0293(11) 0.0531(15) 0.0053(10) 0.0109(11) 0.0117(9) O3 0.0428(13) 0.0231(11) 0.0696(16) -0.0059(11) -0.0086(12) -0.0103(10) O4 0.0285(11) 0.0326(12) 0.0421(12) 0.0139(9) 0.0126(9) 0.0026(9) O5 0.0672(18) 0.0690(16) 0.0244(11) -0.0008(12) -0.0016(12) 0.0044(14) N1 0.0164(10) 0.0148(10) 0.0201(11) -0.0032(7) -0.0008(8) -0.0006(8) N2 0.0186(11) 0.0157(10) 0.0171(10) -0.0011(8) 0.0018(8) 0.0015(8) N3 0.0161(10) 0.0164(10) 0.0153(10) -0.0014(8) 0.0007(8) 0.0010(8) C1 0.0167(12) 0.0161(11) 0.0149(11) 0.0009(9) -0.0009(9) -0.0001(10) C2 0.0244(14) 0.0133(12) 0.0203(13) -0.0001(9) -0.0001(11) -0.0006(10) C3 0.0217(13) 0.0171(12) 0.0187(12) 0.0028(10) 0.0034(10) 0.0054(10) C4 0.0185(13) 0.0225(13) 0.0172(12) 0.0018(10) -0.0011(10) 0.0029(10) C5 0.0197(13) 0.0182(12) 0.0183(12) 0.0008(9) -0.0009(10) -0.0030(10) C6 0.0156(13) 0.0146(12) 0.0167(12) 0.0000(9) 0.0010(9) -0.0006(10) C7 0.0214(13) 0.0108(11) 0.0182(12) -0.0003(9) -0.0015(10) -0.0024(10) C8 0.0205(12) 0.0108(10) 0.0228(17) 0.0005(9) -0.0024(9) -0.0016(9) C9 0.0226(14) 0.0178(13) 0.0278(13) 0.0029(10) 0.0003(11) -0.0047(11) C10 0.0267(15) 0.0179(13) 0.0215(13) -0.0006(10) -0.0017(11) 0.0025(11) C11 0.0306(15) 0.0165(13) 0.0264(14) -0.0092(10) 0.0005(12) -0.0014(12) C12 0.0315(17) 0.0186(14) 0.0249(14) -0.0072(11) 0.0046(11) 0.0029(11) C13 0.0284(16) 0.0322(15) 0.0142(12) 0.0041(10) 0.0015(10) 0.0055(12) C14 0.0237(14) 0.0228(13) 0.0166(12) 0.0034(10) -0.0005(10) -0.0009(11) C15 0.0184(13) 0.0237(13) 0.0253(13) -0.0036(11) -0.0049(11) -0.0023(11) C16 0.0161(13) 0.0180(12) 0.0303(13) -0.0005(10) 0.0004(10) -0.0024(10) C17 0.0291(15) 0.0174(12) 0.0262(14) 0.0049(10) -0.0017(11) -0.0046(12) C18 0.0224(15) 0.0250(14) 0.0270(15) 0.0020(11) 0.0076(12) 0.0003(11) C19 0.0204(13) 0.0235(13) 0.0267(12) -0.0036(10) -0.0036(10) 0.0072(11) 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' Cl Cl 0.1484 0.1585 '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 O1 Pd1 C1 87.29(9) O1 Pd1 C8 90.02(8) C1 Pd1 C8 81.36(9) O1 Pd1 N2 171.73(8) C1 Pd1 N2 95.18(9) C8 Pd1 N2 98.15(9) O1 Pd1 N3 95.83(7) C1 Pd1 N3 173.45(8) C8 Pd1 N3 92.85(8) N2 Pd1 N3 82.54(8) O1 Pd1 N1 89.37(7) C1 Pd1 N1 105.25(9) C8 Pd1 N1 173.32(8) N2 Pd1 N1 82.37(8) N3 Pd1 N1 80.60(7) O4 Cl1 O2 110.34(12) O4 Cl1 O5 109.24(15) O2 Cl1 O5 110.70(14) O4 Cl1 O3 109.25(14) O2 Cl1 O3 108.86(14) O5 Cl1 O3 108.41(15) Pd1 O1 H1 109.5 C17 N1 C11 112.32(19) C17 N1 C16 106.3(2) C11 N1 C16 112.3(2) C17 N1 Pd1 116.08(15) C11 N1 Pd1 107.64(15) C16 N1 Pd1 101.78(14) C18 N2 C12 106.7(2) C18 N2 C13 109.4(2) C12 N2 C13 110.6(2) C18 N2 Pd1 115.94(16) C12 N2 Pd1 104.49(16) C13 N2 Pd1 109.51(15) C19 N3 C14 109.86(19) C19 N3 C15 109.04(19) C14 N3 C15 110.99(19) C19 N3 Pd1 115.67(15) C14 N3 Pd1 101.74(14) C15 N3 Pd1 109.39(15) C2 C1 C6 119.3(2) C2 C1 Pd1 124.96(18) C6 C1 Pd1 115.74(17) C3 C2 C1 120.5(2) C3 C2 H2 119.7 C1 C2 H2 119.7 C4 C3 C2 120.8(2) C4 C3 H3 119.6 C2 C3 H3 119.6 C3 C4 C5 119.4(2) C3 C4 H4 120.3 C5 C4 H4 120.3 C4 C5 C6 120.7(2) C4 C5 H5 119.7 C6 C5 H5 119.7 C5 C6 C1 119.4(2) C5 C6 C7 122.7(2) C1 C6 C7 117.9(2) C6 C7 C8 108.26(19) C6 C7 C10 111.0(2) C8 C7 C10 110.2(2) C6 C7 C9 109.4(2) C8 C7 C9 109.32(19) C10 C7 C9 108.6(2) C7 C8 Pd1 114.92(16) C7 C8 H8A 108.5 Pd1 C8 H8A 108.5 C7 C8 H8B 108.5 Pd1 C8 H8B 108.5 H8A C8 H8B 107.5 C7 C9 H9A 109.5 C7 C9 H9B 109.5 H9A C9 H9B 109.5 C7 C9 H9C 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 C7 C10 H10A 109.5 C7 C10 H10B 109.5 H10A C10 H10B 109.5 C7 C10 H10C 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 N1 C11 C12 112.0(2) N1 C11 H11A 109.2 C12 C11 H11A 109.2 N1 C11 H11B 109.2 C12 C11 H11B 109.2 H11A C11 H11B 107.9 N2 C12 C11 113.3(2) N2 C12 H12A 108.9 C11 C12 H12A 108.9 N2 C12 H12B 108.9 C11 C12 H12B 108.9 H12A C12 H12B 107.7 C14 C13 N2 113.2(2) C14 C13 H13A 108.9 N2 C13 H13A 108.9 C14 C13 H13B 108.9 N2 C13 H13B 108.9 H13A C13 H13B 107.7 N3 C14 C13 111.4(2) N3 C14 H14A 109.3 C13 C14 H14A 109.3 N3 C14 H14B 109.3 C13 C14 H14B 109.3 H14A C14 H14B 108.0 C16 C15 N3 111.5(2) C16 C15 H15A 109.3 N3 C15 H15A 109.3 C16 C15 H15B 109.3 N3 C15 H15B 109.3 H15A C15 H15B 108.0 N1 C16 C15 113.6(2) N1 C16 H16A 108.9 C15 C16 H16A 108.9 N1 C16 H16B 108.9 C15 C16 H16B 108.9 H16A C16 H16B 107.7 N1 C17 H17A 109.5 N1 C17 H17B 109.5 H17A C17 H17B 109.5 N1 C17 H17C 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 N2 C18 H18A 109.5 N2 C18 H18B 109.5 H18A C18 H18B 109.5 N2 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 N3 C19 H19A 109.5 N3 C19 H19B 109.5 H19A C19 H19B 109.5 N3 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Pd1 O1 2.0185(17) Pd1 C1 2.024(2) Pd1 C8 2.061(2) Pd1 N2 2.117(2) Pd1 N3 2.227(2) Pd1 N1 2.263(2) Cl1 O4 1.432(2) Cl1 O2 1.435(2) Cl1 O5 1.436(2) Cl1 O3 1.444(2) O1 H1 0.8400 N1 C17 1.481(3) N1 C11 1.484(3) N1 C16 1.490(3) N2 C18 1.488(3) N2 C12 1.505(3) N2 C13 1.512(3) N3 C19 1.478(3) N3 C14 1.488(3) N3 C15 1.501(3) C1 C2 1.399(3) C1 C6 1.413(3) C2 C3 1.388(4) C2 H2 0.9500 C3 C4 1.388(4) C3 H3 0.9500 C4 C5 1.399(3) C4 H4 0.9500 C5 C6 1.402(4) C5 H5 0.9500 C6 C7 1.512(3) C7 C8 1.533(3) C7 C10 1.538(3) C7 C9 1.547(3) C8 H8A 0.9900 C8 H8B 0.9900 C9 H9A 0.9800 C9 H9B 0.9800 C9 H9C 0.9800 C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 C11 C12 1.530(4) C11 H11A 0.9900 C11 H11B 0.9900 C12 H12A 0.9900 C12 H12B 0.9900 C13 C14 1.505(4) C13 H13A 0.9900 C13 H13B 0.9900 C14 H14A 0.9900 C14 H14B 0.9900 C15 C16 1.492(4) C15 H15A 0.9900 C15 H15B 0.9900 C16 H16A 0.9900 C16 H16B 0.9900 C17 H17A 0.9800 C17 H17B 0.9800 C17 H17C 0.9800 C18 H18A 0.9800 C18 H18B 0.9800 C18 H18C 0.9800 C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 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 C12 H12A O1 0.99 2.58 3.526(3) 160.6 2_665 C15 H15B O3 0.99 2.60 3.309(3) 128.3 3_565 C17 H17B O1 0.98 2.62 3.241(3) 121.6 . C18 H18A O2 0.98 2.62 3.358(3) 132.3 1_545 C18 H18A O4 0.98 2.58 3.522(3) 160.4 1_545 C19 H19C O3 0.98 2.62 3.481(3) 146.8 3_565 O1 H1 O5 0.84 2.34 3.167(3) 168.4 2_664 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 O1 Pd1 N1 C17 46.41(18) C1 Pd1 N1 C17 -40.61(19) N2 Pd1 N1 C17 -133.93(19) N3 Pd1 N1 C17 142.42(19) O1 Pd1 N1 C11 173.23(16) C1 Pd1 N1 C11 86.21(17) N2 Pd1 N1 C11 -7.11(16) N3 Pd1 N1 C11 -90.75(16) O1 Pd1 N1 C16 -68.56(15) C1 Pd1 N1 C16 -155.58(15) N2 Pd1 N1 C16 111.10(16) N3 Pd1 N1 C16 27.45(15) C1 Pd1 N2 C18 41.39(18) C8 Pd1 N2 C18 -40.61(18) N3 Pd1 N2 C18 -132.43(18) N1 Pd1 N2 C18 146.12(18) C1 Pd1 N2 C12 -75.75(17) C8 Pd1 N2 C12 -157.74(16) N3 Pd1 N2 C12 110.44(16) N1 Pd1 N2 C12 28.99(16) C1 Pd1 N2 C13 165.76(17) C8 Pd1 N2 C13 83.77(17) N3 Pd1 N2 C13 -8.05(16) N1 Pd1 N2 C13 -89.50(17) O1 Pd1 N3 C19 -38.62(17) C8 Pd1 N3 C19 51.68(18) N2 Pd1 N3 C19 149.54(18) N1 Pd1 N3 C19 -127.01(17) O1 Pd1 N3 C14 -157.62(14) C8 Pd1 N3 C14 -67.31(15) N2 Pd1 N3 C14 30.54(14) N1 Pd1 N3 C14 113.99(15) O1 Pd1 N3 C15 84.93(15) C8 Pd1 N3 C15 175.24(16) N2 Pd1 N3 C15 -86.91(16) N1 Pd1 N3 C15 -3.46(15) O1 Pd1 C1 C2 -97.5(2) C8 Pd1 C1 C2 172.1(2) N2 Pd1 C1 C2 74.6(2) N1 Pd1 C1 C2 -8.9(2) O1 Pd1 C1 C6 80.20(18) C8 Pd1 C1 C6 -10.23(18) N2 Pd1 C1 C6 -107.71(18) N1 Pd1 C1 C6 168.81(17) C6 C1 C2 C3 -1.3(4) Pd1 C1 C2 C3 176.29(19) C1 C2 C3 C4 -0.1(4) C2 C3 C4 C5 0.8(4) C3 C4 C5 C6 -0.1(4) C4 C5 C6 C1 -1.3(4) C4 C5 C6 C7 176.8(2) C2 C1 C6 C5 2.0(4) Pd1 C1 C6 C5 -175.82(18) C2 C1 C6 C7 -176.2(2) Pd1 C1 C6 C7 6.0(3) C5 C6 C7 C8 -173.9(2) C1 C6 C7 C8 4.3(3) C5 C6 C7 C10 65.0(3) C1 C6 C7 C10 -116.8(2) C5 C6 C7 C9 -54.8(3) C1 C6 C7 C9 123.3(2) C6 C7 C8 Pd1 -12.4(2) C10 C7 C8 Pd1 109.17(19) C9 C7 C8 Pd1 -131.54(17) O1 Pd1 C8 C7 -74.61(17) C1 Pd1 C8 C7 12.65(17) N2 Pd1 C8 C7 106.70(17) N3 Pd1 C8 C7 -170.44(17) C17 N1 C11 C12 111.9(2) C16 N1 C11 C12 -128.3(2) Pd1 N1 C11 C12 -17.1(2) C18 N2 C12 C11 -172.3(2) C13 N2 C12 C11 68.8(3) Pd1 N2 C12 C11 -49.0(2) N1 C11 C12 N2 45.6(3) C18 N2 C13 C14 111.1(2) C12 N2 C13 C14 -131.6(2) Pd1 N2 C13 C14 -17.0(3) C19 N3 C14 C13 -171.9(2) C15 N3 C14 C13 67.4(3) Pd1 N3 C14 C13 -48.9(2) N2 C13 C14 N3 47.0(3) C19 N3 C15 C16 104.9(3) C14 N3 C15 C16 -134.0(2) Pd1 N3 C15 C16 -22.5(2) C17 N1 C16 C15 -172.6(2) C11 N1 C16 C15 64.2(3) Pd1 N1 C16 C15 -50.6(2) N3 C15 C16 N1 52.1(3)