Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Dominique Matt' 'Alan Dedieu' 'Pierre Kuhn' 'Antonio J. Mota' 'Markus Neuburger' 'Richard Welter' _publ_contact_author_name 'Monsr Dominique MATT' _publ_contact_author_address ; Universite Louis Pasteur UMR 7513 CNRS 1 rue Blasie Pascal Strasbourg Cedex 67008 FRANCE ; _publ_contact_author_email DMATT@CHIMIE.U-STRASBG.FR _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Can weak interactions modify the binding properties of a strong nitrogen donor ? Unusual N-coordination of a phosphoranylidene-substituted pyrazolone unit towards palladium (II) centres: an experimental and theoretical study. ; data_DmbaY1Py _database_code_depnum_ccdc_archive 'CCDC 271195' _audit_creation_date 05-02-23 _audit_creation_method CRYSTALS_ver_12.24 _oxford_structure_analysis_title '2231421 DmbaY1Py_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 9.5561(1) _cell_length_b 16.2957(2) _cell_length_c 11.0233(1) _cell_angle_alpha 90 _cell_angle_beta 110.4610(7) _cell_angle_gamma 90 _cell_volume 1608.29(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C37 H35 Cl1 N3 O1 P1 Pd1' _chemical_formula_moiety 'C37 H35 Cl1 N3 O1 P1 Pd1' _chemical_compound_source ? _chemical_formula_weight 710.53 _cell_measurement_reflns_used 7329 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_min 0.09 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_max 0.31 _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 0.744 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.94 # Sheldrick geometric definitions 0.86 0.94 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' _computing_data_collection 'COLLECT (Nonius BV, 1997)' _computing_data_reduction 'EvalCCD (Duisenberg, Kroon-Batenburg and Schreurs, 2003)' _computing_cell_refinement 'EvalCCD (Duisenberg, Kroon-Batenburg and Schreurs, 2003)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 173 _diffrn_reflns_number 71068 _reflns_number_total 7233 _diffrn_reflns_av_R_equivalents 0.096 # Number of reflections with Friedels Law is 7629 # Number of reflections without Friedels Law is 7233 # Theoretical number of reflections is about 3695 _diffrn_reflns_theta_min 3.185 _diffrn_reflns_theta_max 27.500 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.500 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _reflns_limit_h_min -12 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.67 _refine_diff_density_max 0.77 _refine_ls_number_reflns 7026 _refine_ls_number_restraints 77 _refine_ls_number_parameters 426 #_refine_ls_R_factor_ref 0.0236 _refine_ls_wR_factor_ref 0.0254 _refine_ls_goodness_of_fit_ref 1.0672 #_reflns_number_all 7555 _refine_ls_R_factor_all 0.0265 _refine_ls_wR_factor_all 0.0281 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 7026 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_gt 0.0254 _refine_ls_shift/su_max 0.000686 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration unk _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.224 -0.288E-01 0.483E-01 -0.516E-01 ; _refine_special_details ; The crystal investigated was found to be twinned by a rotation of 3.2 degrees. Intensity data for the two lattices related by the twin law 0.978 -0.007 -0.050 0.011 0.999 -0.020 0.067 0.010 1.019 were integrated using EvalCCD, refinement including the data obtained from both lattices was carried out using CRYSTALS. In order to represent the correct geometry around C6 the refinement of the disorder should have been extended to the whole aromatic ring (C1 to C6). As the positions of the disordered phenyl ring would have come very near the ring has been refined as non disordered. ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. EvalCCD: An intensity evaluation method: EVAL-14. Albert J. M. Duisenberg, Loes M.J. Kroon-Batenburg and Antoine M.M. Schreurs, J.Appl.Cryst 36 (2003) p.220-229 Nonius BV, COLLECT Software, (1997-2001) Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Pd1 Pd 0.338468(17) 0.86129(3) 0.305352(14) 0.0227 1.0000 Uani D . . . . . Cl1 Cl 0.21149(10) 0.99012(5) 0.22345(7) 0.0444 1.0000 Uani . . . . . . C1 C 0.4513(3) 0.75887(16) 0.3658(3) 0.0268 1.0000 Uani . . . . . . C2 C 0.5005(3) 0.72511(17) 0.4867(3) 0.0342 1.0000 Uani . . . . . . C3 C 0.5873(4) 0.65394(19) 0.5140(4) 0.0428 1.0000 Uani . . . . . . C4 C 0.6272(3) 0.61636(19) 0.4190(4) 0.0455 1.0000 Uani . . . . . . C5 C 0.5780(3) 0.6496(3) 0.2968(4) 0.0555 1.0000 Uani . . . . . . C6 C 0.4888(3) 0.7198(2) 0.2679(3) 0.0486 1.0000 Uani D U . . . . C10 C 0.6152(3) 0.96616(17) 0.4869(2) 0.0284 1.0000 Uani . . . . . . C11 C 0.5205(3) 0.93233(14) 0.5583(2) 0.0205 1.0000 Uani . . . . . . C12 C 0.5492(3) 0.92480(15) 0.6922(2) 0.0230 1.0000 Uani . . . . . . C13 C 0.4249(3) 0.88240(15) 0.7057(2) 0.0269 1.0000 Uani . . . . . . C14 C 0.1792(3) 0.84305(14) 0.5386(2) 0.0262 1.0000 Uani . . . . . . C15 C 0.0715(3) 0.88068(16) 0.4359(2) 0.0322 1.0000 Uani . . . . . . C16 C -0.0759(3) 0.8544(3) 0.4009(2) 0.0390 1.0000 Uani . . . . . . C17 C -0.1149(3) 0.7923(2) 0.4668(3) 0.0422 1.0000 Uani . . . . . . C18 C -0.0064(4) 0.7548(2) 0.5689(3) 0.0429 1.0000 Uani . . . . . . C19 C 0.1419(3) 0.77973(18) 0.6058(3) 0.0340 1.0000 Uani . . . . . . C20 C 0.8452(3) 0.99187(16) 0.7746(2) 0.0240 1.0000 Uani . . . . . . C21 C 0.8134(3) 1.07257(16) 0.7322(3) 0.0288 1.0000 Uani . . . . . . C22 C 0.9069(3) 1.11460(17) 0.6828(3) 0.0339 1.0000 Uani . . . . . . C23 C 1.0348(3) 1.0759(2) 0.6776(3) 0.0401 1.0000 Uani . . . . . . C24 C 1.0674(3) 0.9962(2) 0.7215(3) 0.0412 1.0000 Uani . . . . . . C25 C 0.9719(3) 0.95334(18) 0.7697(3) 0.0317 1.0000 Uani . . . . . . C26 C 0.6889(3) 1.00333(16) 0.9528(2) 0.0282 1.0000 Uani . . . . . . C27 C 0.5504(3) 1.01787(18) 0.9626(3) 0.0357 1.0000 Uani . . . . . . C28 C 0.5424(5) 1.0620(2) 1.0680(4) 0.0527 1.0000 Uani . . . . . . C29 C 0.6702(5) 1.0893(2) 1.1624(4) 0.0593 1.0000 Uani . . . . . . C30 C 0.8061(5) 1.0744(3) 1.1526(3) 0.0566 1.0000 Uani . . . . . . C31 C 0.8179(4) 1.0311(2) 1.0481(3) 0.0425 1.0000 Uani . . . . . . C32 C 0.7729(3) 0.84155(15) 0.8962(2) 0.0293 1.0000 Uani . . . . . . C33 C 0.7833(4) 0.77741(19) 0.8159(3) 0.0370 1.0000 Uani . . . . . . C34 C 0.8210(4) 0.7002(2) 0.8653(3) 0.0476 1.0000 Uani . . . . . . C35 C 0.8437(5) 0.6836(2) 0.9938(4) 0.0578 1.0000 Uani . . . . . . C36 C 0.8298(6) 0.7457(3) 1.0729(4) 0.0678 1.0000 Uani . . . . . . C37 C 0.7962(4) 0.8255(2) 1.0255(3) 0.0480 1.0000 Uani . . . . . . N1 N 0.3260(3) 0.81720(14) 0.1271(2) 0.0415 1.0000 Uani D U . . . . N2 N 0.3896(2) 0.90144(13) 0.49151(19) 0.0219 1.0000 Uani . . . . . . N3 N 0.3287(2) 0.87068(18) 0.57891(17) 0.0248 1.0000 Uani . . . . . . O1 O 0.39813(19) 0.8608(2) 0.80235(15) 0.0380 1.0000 Uani . . . . . . P1 P 0.70966(7) 0.94036(5) 0.82605(6) 0.0221 1.0000 Uani . . . . . . C7 C 0.3717(10) 0.7268(5) 0.1358(6) 0.0364 0.3000 Uani D U . . . . C8 C 0.2017(10) 0.8347(5) 0.0184(7) 0.0458 0.3000 Uani D U . . . . C9 C 0.4712(8) 0.8617(7) 0.1127(6) 0.0357 0.3000 Uani D U . . . . C70 C 0.4490(5) 0.7705(3) 0.1395(4) 0.0520 0.7000 Uani D U . . . . C80 C 0.1825(5) 0.7636(3) 0.0814(4) 0.0440 0.7000 Uani D U . . . . C90 C 0.2888(7) 0.8836(3) 0.0252(4) 0.0594 0.7000 Uani D U . . . . H21 H 0.4736 0.7519 0.5572 0.0423 1.0000 Uiso . . . . . . H31 H 0.6209 0.6301 0.6032 0.0517 1.0000 Uiso . . . . . . H41 H 0.6907 0.5659 0.4385 0.0539 1.0000 Uiso . . . . . . H51 H 0.6067 0.6230 0.2272 0.0647 1.0000 Uiso . . . . . . H101 H 0.5599 0.9621 0.3916 0.0339 1.0000 Uiso . . . . . . H102 H 0.6389 1.0250 0.5113 0.0339 1.0000 Uiso . . . . . . H103 H 0.7101 0.9340 0.5101 0.0339 1.0000 Uiso . . . . . . H151 H 0.0989 0.9262 0.3875 0.0389 1.0000 Uiso . . . . . . H161 H -0.1547 0.8811 0.3263 0.0455 1.0000 Uiso . . . . . . H171 H -0.2214 0.7744 0.4411 0.0513 1.0000 Uiso . . . . . . H181 H -0.0345 0.7093 0.6167 0.0535 1.0000 Uiso . . . . . . H191 H 0.2206 0.7524 0.6798 0.0423 1.0000 Uiso . . . . . . H211 H 0.7222 1.1002 0.7375 0.0345 1.0000 Uiso . . . . . . H221 H 0.8832 1.1723 0.6512 0.0407 1.0000 Uiso . . . . . . H231 H 1.1032 1.1058 0.6419 0.0496 1.0000 Uiso . . . . . . H241 H 1.1601 0.9691 0.7185 0.0507 1.0000 Uiso . . . . . . H251 H 0.9948 0.8955 0.8003 0.0366 1.0000 Uiso . . . . . . H271 H 0.4573 0.9969 0.8948 0.0449 1.0000 Uiso . . . . . . H281 H 0.4429 1.0739 1.0750 0.0694 1.0000 Uiso . . . . . . H291 H 0.6635 1.1203 1.2385 0.0767 1.0000 Uiso . . . . . . H301 H 0.8986 1.0947 1.2216 0.0666 1.0000 Uiso . . . . . . H311 H 0.9180 1.0202 1.0415 0.0493 1.0000 Uiso . . . . . . H331 H 0.7632 0.7879 0.7219 0.0403 1.0000 Uiso . . . . . . H341 H 0.8323 0.6552 0.8077 0.0517 1.0000 Uiso . . . . . . H351 H 0.8702 0.6269 1.0288 0.0655 1.0000 Uiso . . . . . . H361 H 0.8437 0.7337 1.1652 0.0805 1.0000 Uiso . . . . . . H371 H 0.7889 0.8707 1.0843 0.0574 1.0000 Uiso . . . . . . H71 H 0.4129 0.7124 0.0670 0.0435 0.3000 Uiso . . . . . . H72 H 0.2843 0.6904 0.1279 0.0435 0.3000 Uiso . . . . . . H81 H 0.1769 0.8942 0.0177 0.0474 0.3000 Uiso . . . . . . H82 H 0.2233 0.8206 -0.0614 0.0474 0.3000 Uiso . . . . . . H83 H 0.1147 0.8012 0.0211 0.0474 0.3000 Uiso . . . . . . H91 H 0.4549 0.9222 0.1058 0.0459 0.3000 Uiso . . . . . . H92 H 0.5611 0.8488 0.1901 0.0459 0.3000 Uiso . . . . . . H93 H 0.4867 0.8409 0.0328 0.0459 0.3000 Uiso . . . . . . H701 H 0.5348 0.8069 0.1433 0.0632 0.7000 Uiso . . . . . . H702 H 0.4271 0.7325 0.0639 0.0632 0.7000 Uiso . . . . . . H801 H 0.0937 0.7986 0.0728 0.0488 0.7000 Uiso . . . . . . H802 H 0.1708 0.7384 -0.0044 0.0488 0.7000 Uiso . . . . . . H803 H 0.1910 0.7192 0.1462 0.0488 0.7000 Uiso . . . . . . H901 H 0.1974 0.9137 0.0246 0.0750 0.7000 Uiso . . . . . . H902 H 0.3744 0.9229 0.0452 0.0750 0.7000 Uiso . . . . . . H903 H 0.2703 0.8583 -0.0617 0.0750 0.7000 Uiso . . . . . . 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 0.02329(7) 0.02661(8) 0.01766(7) -0.00098(9) 0.00631(5) -0.00533(9) Cl1 0.0558(4) 0.0290(3) 0.0345(3) 0.0098(3) -0.0015(3) 0.0003(3) C1 0.0167(10) 0.0287(12) 0.0345(13) -0.0084(10) 0.0082(9) -0.0025(9) C2 0.0418(15) 0.0219(12) 0.0419(15) 0.0013(10) 0.0185(12) 0.0004(11) C3 0.0420(16) 0.0265(14) 0.0609(19) 0.0041(13) 0.0192(15) -0.0009(12) C4 0.0293(13) 0.0269(14) 0.079(2) -0.0165(14) 0.0166(14) -0.0042(11) C5 0.0259(14) 0.073(3) 0.063(2) -0.037(2) 0.0093(14) 0.0042(15) C6 0.0293(14) 0.074(2) 0.0385(15) -0.0225(15) 0.0066(12) 0.0115(14) C10 0.0283(12) 0.0353(13) 0.0214(11) 0.0004(9) 0.0084(9) -0.0078(10) C11 0.0211(10) 0.0180(10) 0.0220(10) 0.0004(8) 0.0071(8) 0.0024(8) C12 0.0227(11) 0.0242(11) 0.0211(10) -0.0035(8) 0.0063(8) 0.0006(9) C13 0.0263(11) 0.0322(15) 0.0227(10) -0.0024(8) 0.0092(9) -0.0003(9) C14 0.0215(10) 0.0307(16) 0.0278(10) -0.0087(9) 0.0105(9) -0.0017(8) C15 0.0273(11) 0.0396(18) 0.0305(11) -0.0038(10) 0.0112(9) -0.0023(10) C16 0.0236(10) 0.0554(19) 0.0349(12) -0.0096(17) 0.0063(9) -0.0028(16) C17 0.0268(13) 0.0488(18) 0.0528(18) -0.0143(14) 0.0159(13) -0.0126(12) C18 0.0396(16) 0.0372(16) 0.0572(19) -0.0045(14) 0.0236(14) -0.0116(12) C19 0.0329(13) 0.0313(13) 0.0413(14) -0.0027(11) 0.0173(12) -0.0016(11) C20 0.0206(10) 0.0277(12) 0.0208(10) -0.0029(9) 0.0034(9) -0.0013(9) C21 0.0247(12) 0.0282(13) 0.0335(13) -0.0054(10) 0.0100(10) -0.0024(10) C22 0.0343(13) 0.0293(13) 0.0382(14) -0.0043(11) 0.0129(11) -0.0085(11) C23 0.0314(14) 0.0506(18) 0.0423(16) -0.0112(14) 0.0179(12) -0.0120(13) C24 0.0309(14) 0.0527(18) 0.0433(16) -0.0136(14) 0.0169(12) -0.0006(13) C25 0.0261(12) 0.0363(14) 0.0290(12) -0.0068(11) 0.0050(10) 0.0040(11) C26 0.0384(13) 0.0226(12) 0.0246(11) -0.0020(9) 0.0121(10) -0.0023(10) C27 0.0426(15) 0.0299(13) 0.0399(15) -0.0063(11) 0.0209(12) -0.0029(11) C28 0.069(2) 0.0451(19) 0.059(2) -0.0170(16) 0.0418(19) -0.0081(16) C29 0.094(3) 0.049(2) 0.0482(19) -0.0248(16) 0.042(2) -0.020(2) C30 0.075(3) 0.057(2) 0.0337(16) -0.0195(15) 0.0144(16) -0.0213(19) C31 0.0446(17) 0.0482(19) 0.0304(15) -0.0103(14) 0.0078(13) -0.0090(14) C32 0.0313(12) 0.0259(15) 0.0256(11) 0.0028(8) 0.0037(9) 0.0033(9) C33 0.0437(17) 0.0292(14) 0.0277(13) -0.0018(11) -0.0007(12) 0.0005(13) C34 0.0521(19) 0.0292(15) 0.0481(18) -0.0036(13) 0.0008(15) 0.0027(13) C35 0.075(3) 0.0270(16) 0.062(2) 0.0139(15) 0.012(2) 0.0105(16) C36 0.108(4) 0.045(2) 0.047(2) 0.0225(17) 0.024(2) 0.024(2) C37 0.074(2) 0.0347(15) 0.0351(15) 0.0089(13) 0.0184(16) 0.0158(16) N1 0.0685(17) 0.0338(13) 0.0227(10) -0.0046(9) 0.0165(11) -0.0136(12) N2 0.0234(9) 0.0225(9) 0.0204(9) -0.0013(7) 0.0082(7) 0.0004(8) N3 0.0231(8) 0.0309(12) 0.0220(8) -0.0022(9) 0.0099(6) -0.0001(9) O1 0.0381(8) 0.0555(11) 0.0237(7) -0.0033(13) 0.0148(6) -0.0133(14) P1 0.0233(3) 0.0217(3) 0.0193(3) -0.0011(2) 0.0051(2) -0.0003(2) C7 0.053(5) 0.032(4) 0.023(4) -0.006(3) 0.011(3) -0.009(4) C8 0.061(6) 0.038(5) 0.020(4) 0.002(3) -0.009(4) -0.003(4) C9 0.047(4) 0.044(4) 0.024(3) 0.001(5) 0.022(3) -0.011(6) C70 0.044(2) 0.079(3) 0.035(2) -0.015(2) 0.0173(19) 0.013(2) C80 0.044(2) 0.040(2) 0.038(2) -0.0104(18) 0.0016(18) -0.0078(18) C90 0.102(4) 0.060(4) 0.026(2) 0.0038(19) 0.034(2) -0.010(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3758(3) loop_ _oxford_twin_element_scale_factors 0.5000(4) 0.5000(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 . Cl1 . 2.4349(7) yes Pd1 . C1 . 1.972(3) yes Pd1 . N1 . 2.056(2) yes Pd1 . N2 . 2.0437(19) yes C1 . C2 . 1.365(4) yes C1 . C6 . 1.402(4) yes C2 . C3 . 1.397(4) yes C2 . H21 . 1.000 no C3 . C4 . 1.377(5) yes C3 . H31 . 1.000 no C4 . C5 . 1.374(6) yes C4 . H41 . 1.000 no C5 . C6 . 1.395(5) yes C5 . H51 . 0.999 no C6 . C7 . 1.499(7) yes C6 . C70 . 1.567(6) yes C10 . C11 . 1.497(3) yes C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C11 . C12 . 1.409(3) yes C11 . N2 . 1.310(3) yes C12 . C13 . 1.426(3) yes C12 . P1 . 1.735(2) yes C13 . N3 . 1.392(3) yes C13 . O1 . 1.231(3) yes C14 . C15 . 1.379(4) yes C14 . C19 . 1.388(4) yes C14 . N3 . 1.413(3) yes C15 . C16 . 1.392(4) yes C15 . H151 . 1.000 no C16 . C17 . 1.372(5) yes C16 . H161 . 1.000 no C17 . C18 . 1.378(5) yes C17 . H171 . 1.000 no C18 . C19 . 1.391(4) yes C18 . H181 . 1.000 no C19 . H191 . 1.000 no C20 . C21 . 1.393(4) yes C20 . C25 . 1.382(3) yes C20 . P1 . 1.794(3) yes C21 . C22 . 1.380(4) yes C21 . H211 . 1.000 no C22 . C23 . 1.394(4) yes C22 . H221 . 1.001 no C23 . C24 . 1.383(5) yes C23 . H231 . 1.000 no C24 . C25 . 1.393(4) yes C24 . H241 . 1.000 no C25 . H251 . 0.999 no C26 . C27 . 1.385(4) yes C26 . C31 . 1.387(4) yes C26 . P1 . 1.800(3) yes C27 . C28 . 1.391(4) yes C27 . H271 . 1.000 no C28 . C29 . 1.373(6) yes C28 . H281 . 1.000 no C29 . C30 . 1.362(6) yes C29 . H291 . 1.000 no C30 . C31 . 1.389(5) yes C30 . H301 . 1.000 no C31 . H311 . 1.000 no C32 . C33 . 1.396(4) yes C32 . C37 . 1.389(4) yes C32 . P1 . 1.797(2) yes C33 . C34 . 1.369(4) yes C33 . H331 . 1.000 no C34 . C35 . 1.382(6) yes C34 . H341 . 1.000 no C35 . C36 . 1.372(6) yes C35 . H351 . 1.000 no C36 . C37 . 1.396(5) yes C36 . H361 . 0.999 no C37 . H371 . 1.000 no N1 . C7 . 1.530(8) yes N1 . C8 . 1.390(7) yes N1 . C9 . 1.622(7) yes N1 . C70 . 1.367(5) yes N1 . C80 . 1.554(5) yes N1 . C90 . 1.510(5) yes N2 . N3 . 1.383(3) yes C7 . H71 . 0.997 no C7 . H72 . 1.004 no C8 . H81 . 0.998 no C8 . H82 . 0.999 no C8 . H83 . 1.003 no C9 . H91 . 0.997 no C9 . H92 . 0.999 no C9 . H93 . 1.002 no C70 . H701 . 1.001 no C70 . H702 . 1.000 no C80 . H801 . 0.999 no C80 . H802 . 1.001 no C80 . H803 . 0.999 no C90 . H901 . 1.000 no C90 . H902 . 1.001 no C90 . H903 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Pd1 . C1 . 176.02(8) yes Cl1 . Pd1 . N1 . 95.28(7) yes C1 . Pd1 . N1 . 82.49(10) yes Cl1 . Pd1 . N2 . 90.55(6) yes C1 . Pd1 . N2 . 91.22(9) yes N1 . Pd1 . N2 . 170.1(1) yes Pd1 . C1 . C2 . 129.2(2) yes Pd1 . C1 . C6 . 112.4(2) yes C2 . C1 . C6 . 118.3(3) yes C1 . C2 . C3 . 121.4(3) yes C1 . C2 . H21 . 119.281 no C3 . C2 . H21 . 119.334 no C2 . C3 . C4 . 120.5(3) yes C2 . C3 . H31 . 119.757 no C4 . C3 . H31 . 119.760 no C3 . C4 . C5 . 118.6(3) yes C3 . C4 . H41 . 120.721 no C5 . C4 . H41 . 120.635 no C4 . C5 . C6 . 121.3(3) yes C4 . C5 . H51 . 119.335 no C6 . C5 . H51 . 119.356 no C1 . C6 . C5 . 119.8(3) yes C1 . C6 . C7 . 114.1(4) yes C5 . C6 . C7 . 118.3(4) yes C1 . C6 . C70 . 114.1(3) yes C5 . C6 . C70 . 125.0(3) yes C11 . C10 . H101 . 109.455 no C11 . C10 . H102 . 109.484 no H101 . C10 . H102 . 109.442 no C11 . C10 . H103 . 109.490 no H101 . C10 . H103 . 109.477 no H102 . C10 . H103 . 109.479 no C10 . C11 . C12 . 130.6(2) yes C10 . C11 . N2 . 118.7(2) yes C12 . C11 . N2 . 110.7(2) yes C11 . C12 . C13 . 106.7(2) yes C11 . C12 . P1 . 131.92(18) yes C13 . C12 . P1 . 120.19(18) yes C12 . C13 . N3 . 104.10(19) yes C12 . C13 . O1 . 131.4(2) yes N3 . C13 . O1 . 124.4(2) yes C15 . C14 . C19 . 120.8(2) yes C15 . C14 . N3 . 119.9(2) yes C19 . C14 . N3 . 119.3(2) yes C14 . C15 . C16 . 118.9(3) yes C14 . C15 . H151 . 120.560 no C16 . C15 . H151 . 120.539 no C15 . C16 . C17 . 121.1(3) yes C15 . C16 . H161 . 119.488 no C17 . C16 . H161 . 119.420 no C16 . C17 . C18 . 119.6(3) yes C16 . C17 . H171 . 120.224 no C18 . C17 . H171 . 120.201 no C17 . C18 . C19 . 120.5(3) yes C17 . C18 . H181 . 119.721 no C19 . C18 . H181 . 119.735 no C18 . C19 . C14 . 119.1(3) yes C18 . C19 . H191 . 120.446 no C14 . C19 . H191 . 120.427 no C21 . C20 . C25 . 120.5(2) yes C21 . C20 . P1 . 116.78(18) yes C25 . C20 . P1 . 122.6(2) yes C20 . C21 . C22 . 120.3(2) yes C20 . C21 . H211 . 119.832 no C22 . C21 . H211 . 119.828 no C21 . C22 . C23 . 119.3(3) yes C21 . C22 . H221 . 120.321 no C23 . C22 . H221 . 120.387 no C22 . C23 . C24 . 120.3(3) yes C22 . C23 . H231 . 119.828 no C24 . C23 . H231 . 119.849 no C23 . C24 . C25 . 120.4(3) yes C23 . C24 . H241 . 119.804 no C25 . C24 . H241 . 119.808 no C24 . C25 . C20 . 119.2(3) yes C24 . C25 . H251 . 120.402 no C20 . C25 . H251 . 120.439 no C27 . C26 . C31 . 120.4(3) yes C27 . C26 . P1 . 121.7(2) yes C31 . C26 . P1 . 117.6(2) yes C26 . C27 . C28 . 119.1(3) yes C26 . C27 . H271 . 120.490 no C28 . C27 . H271 . 120.414 no C27 . C28 . C29 . 120.5(3) yes C27 . C28 . H281 . 119.769 no C29 . C28 . H281 . 119.751 no C28 . C29 . C30 . 120.1(3) yes C28 . C29 . H291 . 119.950 no C30 . C29 . H291 . 119.934 no C29 . C30 . C31 . 120.8(3) yes C29 . C30 . H301 . 119.584 no C31 . C30 . H301 . 119.573 no C30 . C31 . C26 . 119.1(3) yes C30 . C31 . H311 . 120.462 no C26 . C31 . H311 . 120.486 no C33 . C32 . C37 . 119.3(3) yes C33 . C32 . P1 . 119.1(2) yes C37 . C32 . P1 . 121.3(2) yes C32 . C33 . C34 . 120.2(3) yes C32 . C33 . H331 . 119.882 no C34 . C33 . H331 . 119.887 no C33 . C34 . C35 . 120.8(3) yes C33 . C34 . H341 . 119.584 no C35 . C34 . H341 . 119.622 no C34 . C35 . C36 . 119.5(3) yes C34 . C35 . H351 . 120.287 no C36 . C35 . H351 . 120.238 no C35 . C36 . C37 . 120.7(3) yes C35 . C36 . H361 . 119.682 no C37 . C36 . H361 . 119.647 no C36 . C37 . C32 . 119.5(3) yes C36 . C37 . H371 . 120.236 no C32 . C37 . H371 . 120.265 no Pd1 . N1 . C7 . 110.9(3) yes Pd1 . N1 . C8 . 119.9(4) yes C7 . N1 . C8 . 113.0(4) yes Pd1 . N1 . C9 . 99.9(3) yes C7 . N1 . C9 . 101.6(4) yes C8 . N1 . C9 . 109.1(4) yes Pd1 . N1 . C70 . 109.8(2) yes Pd1 . N1 . C80 . 104.9(2) yes C70 . N1 . C80 . 110.5(3) yes Pd1 . N1 . C90 . 112.4(2) yes C70 . N1 . C90 . 116.3(3) yes C80 . N1 . C90 . 102.1(3) yes C11 . N2 . Pd1 . 122.28(16) yes C11 . N2 . N3 . 107.42(19) yes Pd1 . N2 . N3 . 124.92(16) yes C14 . N3 . C13 . 126.85(19) yes C14 . N3 . N2 . 121.50(19) yes C13 . N3 . N2 . 111.02(19) yes C26 . P1 . C32 . 106.77(12) yes C26 . P1 . C20 . 105.46(12) yes C32 . P1 . C20 . 112.57(12) yes C26 . P1 . C12 . 116.02(12) yes C32 . P1 . C12 . 107.42(12) yes C20 . P1 . C12 . 108.72(11) yes N1 . C7 . C6 . 103.6(4) yes N1 . C7 . H71 . 111.088 no C6 . C7 . H71 . 111.215 no N1 . C7 . H72 . 110.682 no C6 . C7 . H72 . 110.775 no H71 . C7 . H72 . 109.412 no N1 . C8 . H81 . 109.560 no N1 . C8 . H82 . 109.552 no H81 . C8 . H82 . 109.706 no N1 . C8 . H83 . 109.304 no H81 . C8 . H83 . 109.363 no H82 . C8 . H83 . 109.341 no N1 . C9 . H91 . 109.497 no N1 . C9 . H92 . 109.401 no H91 . C9 . H92 . 109.791 no N1 . C9 . H93 . 109.222 no H91 . C9 . H93 . 109.528 no H92 . C9 . H93 . 109.387 no C6 . C70 . N1 . 108.2(3) yes C6 . C70 . H701 . 109.798 no N1 . C70 . H701 . 109.736 no C6 . C70 . H702 . 109.874 no N1 . C70 . H702 . 109.825 no H701 . C70 . H702 . 109.394 no N1 . C80 . H801 . 109.448 no N1 . C80 . H802 . 109.356 no H801 . C80 . H802 . 109.496 no N1 . C80 . H803 . 109.442 no H801 . C80 . H803 . 109.607 no H802 . C80 . H803 . 109.478 no N1 . C90 . H901 . 109.534 no N1 . C90 . H902 . 109.447 no H901 . C90 . H902 . 109.433 no N1 . C90 . H903 . 109.515 no H901 . C90 . H903 . 109.490 no H902 . C90 . H903 . 109.407 no data_welt28 _database_code_depnum_ccdc_archive 'CCDC 271196' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H50 Cl14 N4 O2 P2 Pd' _chemical_formula_sum 'C60 H50 Cl14 N4 O2 P2 Pd' _chemical_formula_weight 1523.68 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' P P 0.1023 0.0942 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4860(4) _cell_length_b 11.1350(5) _cell_length_c 18.4870(8) _cell_angle_alpha 76.56(5) _cell_angle_beta 87.92(5) _cell_angle_gamma 67.80(5) _cell_volume 1940.57(14) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12929 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.801 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8557 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.2844 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 27.41 _reflns_number_total 8556 _reflns_number_gt 5324 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8556 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1438 _refine_ls_R_factor_gt 0.0915 _refine_ls_wR_factor_ref 0.2418 _refine_ls_wR_factor_gt 0.2190 _refine_ls_goodness_of_fit_ref 0.835 _refine_ls_restrained_S_all 0.835 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Pd Pd 1.0000 0.5000 1.0000 0.0477(3) Uani 1 2 d S . . P P 0.82264(18) 0.4276(2) 0.73152(11) 0.0499(5) Uani 1 1 d . . . O O 0.9085(5) 0.6935(6) 0.7111(3) 0.0619(14) Uani 1 1 d . . . N1 N 0.9223(6) 0.6454(6) 0.8410(3) 0.0515(15) Uani 1 1 d . . . N2 N 0.8951(6) 0.5574(6) 0.9008(3) 0.0511(15) Uani 1 1 d . . . Cl1 Cl 1.19960(19) 0.4007(3) 0.94273(13) 0.0784(7) Uani 1 1 d . . . Cl2 Cl 0.4286(7) 0.9120(5) 0.9517(3) 0.186(2) Uani 1 1 d . . . Cl3 Cl 0.4354(5) 0.6634(5) 0.9381(3) 0.1580(16) Uani 1 1 d . . . Cl4 Cl 0.5472(3) 0.8132(4) 0.8269(2) 0.1262(13) Uani 1 1 d . . . Cl5 Cl 1.2542(4) 0.5072(4) 0.6651(3) 0.1436(14) Uani 1 1 d . . . Cl6 Cl 1.2704(3) 0.7590(4) 0.6505(2) 0.1150(11) Uani 1 1 d . . . Cl7 Cl 1.1496(5) 0.6992(6) 0.5323(2) 0.1636(18) Uani 1 1 d . . . C11 C 0.6949(7) 0.3637(7) 0.7699(4) 0.0495(17) Uani 1 1 d . . . C8 C 0.8536(7) 0.5122(7) 0.7915(4) 0.0493(17) Uani 1 1 d . . . C7 C 0.8963(7) 0.6239(8) 0.7732(4) 0.0555(19) Uani 1 1 d . . . C16 C 0.7178(9) 0.2281(10) 0.7838(5) 0.072(2) Uani 1 1 d . . . H16 H 0.7993 0.1666 0.7689 0.086 Uiso 1 1 calc . . . C24 C 0.8536(9) 0.5654(9) 0.5910(5) 0.064(2) Uani 1 1 d . . . H24 H 0.9461 0.5399 0.6089 0.077 Uiso 1 1 calc . . . C22 C 0.9803(9) 0.2228(10) 0.6664(5) 0.077(3) Uani 1 1 d . . . H22 H 0.8969 0.2428 0.6391 0.092 Uiso 1 1 calc . . . C17 C 0.9797(7) 0.2908(8) 0.7192(5) 0.0560(19) Uani 1 1 d . . . C23 C 0.7604(7) 0.5298(7) 0.6374(4) 0.0528(18) Uani 1 1 d . . . C18 C 1.0976(8) 0.2638(9) 0.7640(6) 0.081(3) Uani 1 1 d . . . H18 H 1.0962 0.3100 0.8014 0.097 Uiso 1 1 calc . . . C12 C 0.5755(8) 0.4513(9) 0.7913(5) 0.069(2) Uani 1 1 d . . . H12 H 0.5600 0.5434 0.7820 0.083 Uiso 1 1 calc . . . C30 C 1.1686(10) 0.6809(10) 0.6250(6) 0.083(3) Uani 1 1 d . . . H30 H 1.0757 0.7144 0.6458 0.100 Uiso 1 1 calc . . . C28 C 0.6281(8) 0.5588(9) 0.6110(5) 0.070(2) Uani 1 1 d . . . H28 H 0.5645 0.5346 0.6431 0.084 Uiso 1 1 calc . . . C9 C 0.8610(8) 0.4721(8) 0.8697(4) 0.0570(19) Uani 1 1 d . . . C2 C 1.0653(11) 0.7744(11) 0.8194(6) 0.086(3) Uani 1 1 d . . . H2 H 1.1132 0.7213 0.7861 0.103 Uiso 1 1 calc . . . C3 C 1.1061(14) 0.8703(14) 0.8297(8) 0.104(4) Uani 1 1 d . . . H3 H 1.1800 0.8865 0.8037 0.125 Uiso 1 1 calc . . . C6 C 0.8913(10) 0.8217(10) 0.9025(6) 0.082(3) Uani 1 1 d . . . H6 H 0.8174 0.8038 0.9276 0.098 Uiso 1 1 calc . . . C13 C 0.4768(9) 0.4055(12) 0.8266(6) 0.083(3) Uani 1 1 d . . . H13 H 0.3948 0.4665 0.8413 0.100 Uiso 1 1 calc . . . C26 C 0.6761(12) 0.6688(10) 0.4920(6) 0.088(3) Uani 1 1 d . . . H26 H 0.6441 0.7206 0.4429 0.106 Uiso 1 1 calc . . . C1 C 0.9588(8) 0.7503(8) 0.8544(5) 0.059(2) Uani 1 1 d . . . C20 C 1.2183(11) 0.0956(12) 0.6918(8) 0.107(4) Uani 1 1 d . . . H20 H 1.3013 0.0298 0.6815 0.129 Uiso 1 1 calc . . . C5 C 0.9295(14) 0.9244(11) 0.9165(7) 0.101(4) Uani 1 1 d . . . H5 H 0.8824 0.9771 0.9501 0.121 Uiso 1 1 calc . . . C4 C 1.0384(15) 0.9431(12) 0.8785(8) 0.109(4) Uani 1 1 d . . . H4 H 1.0675 1.0101 0.8870 0.130 Uiso 1 1 calc . . . C15 C 0.6186(11) 0.1853(11) 0.8198(6) 0.087(3) Uani 1 1 d . . . H15 H 0.6342 0.0930 0.8309 0.104 Uiso 1 1 calc . . . C27 C 0.5907(11) 0.6215(14) 0.5391(7) 0.105(4) Uani 1 1 d . . . H27 H 0.5026 0.6340 0.5200 0.126 Uiso 1 1 calc . . . C19 C 1.2197(9) 0.1609(12) 0.7485(8) 0.101(4) Uani 1 1 d . . . H19 H 1.3032 0.1362 0.7769 0.122 Uiso 1 1 calc . . . C14 C 0.4974(11) 0.2741(13) 0.8400(6) 0.092(3) Uani 1 1 d . . . H14 H 0.4293 0.2434 0.8630 0.111 Uiso 1 1 calc . . . C10 C 0.8392(11) 0.3564(10) 0.9211(6) 0.084(3) Uani 1 1 d . . . H10A H 0.9184 0.2738 0.9208 0.126 Uiso 1 1 calc . . . H10B H 0.7551 0.3495 0.9044 0.126 Uiso 1 1 calc . . . H10C H 0.8298 0.3703 0.9718 0.126 Uiso 1 1 calc . . . C21 C 1.1001(13) 0.1256(11) 0.6521(7) 0.095(3) Uani 1 1 d . . . H21 H 1.0996 0.0801 0.6146 0.114 Uiso 1 1 calc . . . C25 C 0.8113(11) 0.6379(10) 0.5189(5) 0.081(3) Uani 1 1 d . . . H25 H 0.8730 0.6669 0.4875 0.098 Uiso 1 1 calc . . . C29 C 0.5184(12) 0.7721(12) 0.9179(8) 0.110(4) Uani 1 1 d . . . H29 H 0.6106 0.7266 0.9457 0.132 Uiso 1 1 calc . . . 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 0.0451(4) 0.0611(5) 0.0382(5) -0.0044(4) 0.0043(3) -0.0260(4) P 0.0425(9) 0.0598(12) 0.0477(12) -0.0087(9) 0.0043(8) -0.0224(9) O 0.066(3) 0.077(4) 0.043(3) 0.003(3) 0.002(2) -0.037(3) N1 0.057(3) 0.060(4) 0.043(4) -0.003(3) 0.004(3) -0.035(3) N2 0.050(3) 0.067(4) 0.032(3) 0.006(3) -0.007(3) -0.028(3) Cl1 0.0498(10) 0.1081(18) 0.0568(14) -0.0102(12) 0.0150(9) -0.0138(11) Cl2 0.263(6) 0.144(4) 0.142(4) -0.050(3) -0.003(4) -0.057(4) Cl3 0.172(4) 0.151(3) 0.161(4) -0.005(3) 0.033(3) -0.094(3) Cl4 0.104(2) 0.119(2) 0.126(3) 0.002(2) 0.021(2) -0.0281(19) Cl5 0.147(3) 0.105(2) 0.171(4) -0.009(2) -0.021(3) -0.050(2) Cl6 0.105(2) 0.118(2) 0.146(3) -0.050(2) 0.036(2) -0.0617(19) Cl7 0.185(4) 0.220(5) 0.098(3) 0.008(3) -0.003(3) -0.117(4) C11 0.045(4) 0.059(4) 0.050(5) -0.007(3) 0.003(3) -0.030(3) C8 0.055(4) 0.050(4) 0.043(4) -0.003(3) 0.003(3) -0.024(3) C7 0.050(4) 0.074(5) 0.040(5) -0.002(4) 0.000(3) -0.029(4) C16 0.067(5) 0.089(7) 0.073(6) -0.018(5) 0.011(4) -0.046(5) C24 0.072(5) 0.086(6) 0.043(5) -0.009(4) 0.003(4) -0.042(5) C22 0.074(5) 0.088(7) 0.060(6) -0.026(5) 0.012(5) -0.018(5) C17 0.044(4) 0.065(5) 0.054(5) -0.002(4) 0.009(3) -0.023(4) C23 0.055(4) 0.055(4) 0.047(5) -0.011(3) 0.007(3) -0.021(4) C18 0.047(4) 0.068(6) 0.117(9) 0.002(5) 0.000(5) -0.025(4) C12 0.063(5) 0.090(6) 0.075(6) -0.022(5) 0.020(4) -0.052(5) C30 0.070(5) 0.088(7) 0.088(8) 0.000(6) 0.006(5) -0.038(5) C28 0.054(4) 0.087(6) 0.047(5) -0.007(4) -0.004(4) -0.008(4) C9 0.055(4) 0.073(5) 0.047(5) -0.002(4) -0.003(3) -0.035(4) C2 0.106(7) 0.109(8) 0.078(7) -0.030(6) 0.026(6) -0.077(7) C3 0.130(10) 0.114(9) 0.105(10) -0.015(8) 0.017(8) -0.093(8) C6 0.085(6) 0.071(6) 0.092(8) -0.007(5) -0.001(6) -0.038(5) C13 0.058(5) 0.113(8) 0.093(8) -0.037(7) 0.024(5) -0.043(5) C26 0.104(8) 0.077(6) 0.059(6) -0.008(5) -0.010(6) -0.012(6) C1 0.059(4) 0.069(5) 0.053(5) -0.014(4) 0.010(4) -0.030(4) C20 0.073(7) 0.091(8) 0.133(12) -0.015(8) 0.048(7) -0.014(6) C5 0.141(10) 0.073(7) 0.100(9) -0.027(6) 0.000(8) -0.047(7) C4 0.132(10) 0.088(8) 0.109(10) 0.025(7) -0.035(8) -0.070(8) C15 0.091(7) 0.089(7) 0.089(8) -0.001(6) 0.014(6) -0.057(6) C27 0.072(6) 0.144(11) 0.079(8) -0.011(7) -0.009(6) -0.029(7) C19 0.043(5) 0.091(8) 0.149(12) -0.022(8) 0.006(6) -0.006(5) C14 0.083(7) 0.124(9) 0.088(8) 0.004(7) 0.008(6) -0.077(7) C10 0.108(7) 0.088(7) 0.066(6) 0.001(5) -0.001(5) -0.057(6) C21 0.105(8) 0.084(7) 0.087(8) -0.019(6) 0.020(7) -0.026(6) C25 0.100(7) 0.085(6) 0.055(6) -0.005(5) 0.008(5) -0.037(6) C29 0.088(7) 0.105(9) 0.129(11) 0.001(8) -0.002(7) -0.043(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N2 2.013(6) . ? Pd N2 2.013(6) 2_767 ? Pd Cl1 2.315(2) . ? Pd Cl1 2.315(2) 2_767 ? P C8 1.721(8) . ? P C11 1.794(7) . ? P C17 1.823(8) . ? P C23 1.830(8) . ? O C7 1.259(9) . ? N1 C7 1.384(10) . ? N1 N2 1.396(8) . ? N1 C1 1.433(10) . ? N2 C9 1.372(10) . ? Cl2 C29 1.734(14) . ? Cl3 C29 1.710(13) . ? Cl4 C29 1.685(14) . ? Cl5 C30 1.779(11) . ? Cl6 C30 1.746(11) . ? Cl7 C30 1.689(12) . ? C11 C12 1.377(11) . ? C11 C16 1.398(12) . ? C8 C9 1.408(10) . ? C8 C7 1.442(11) . ? C16 C15 1.389(13) . ? C16 H16 0.9500 . ? C24 C25 1.378(13) . ? C24 C23 1.385(11) . ? C24 H24 0.9500 . ? C22 C17 1.367(12) . ? C22 C21 1.378(13) . ? C22 H22 0.9500 . ? C17 C18 1.407(12) . ? C23 C28 1.380(11) . ? C18 C19 1.432(13) . ? C18 H18 0.9500 . ? C12 C13 1.398(12) . ? C12 H12 0.9500 . ? C30 H30 1.0000 . ? C28 C27 1.343(14) . ? C28 H28 0.9500 . ? C9 C10 1.501(12) . ? C2 C3 1.344(15) . ? C2 C1 1.353(12) . ? C2 H2 0.9500 . ? C3 C4 1.354(17) . ? C3 H3 0.9500 . ? C6 C1 1.335(12) . ? C6 C5 1.423(14) . ? C6 H6 0.9500 . ? C13 C14 1.358(15) . ? C13 H13 0.9500 . ? C26 C27 1.387(17) . ? C26 C25 1.407(14) . ? C26 H26 0.9500 . ? C20 C21 1.351(17) . ? C20 C19 1.411(18) . ? C20 H20 0.9500 . ? C5 C4 1.376(18) . ? C5 H5 0.9500 . ? C4 H4 0.9500 . ? C15 C14 1.386(15) . ? C15 H15 0.9500 . ? C27 H27 0.9500 . ? C19 H19 0.9500 . ? C14 H14 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C21 H21 0.9500 . ? C25 H25 0.9500 . ? C29 H29 1.0000 . ? 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 N2 Pd N2 180.000(3) . 2_767 ? N2 Pd Cl1 88.58(19) . . ? N2 Pd Cl1 91.42(19) 2_767 . ? N2 Pd Cl1 91.42(19) . 2_767 ? N2 Pd Cl1 88.58(19) 2_767 2_767 ? Cl1 Pd Cl1 179.997(2) . 2_767 ? C8 P C11 108.0(4) . . ? C8 P C17 111.1(4) . . ? C11 P C17 109.9(4) . . ? C8 P C23 114.3(4) . . ? C11 P C23 108.2(3) . . ? C17 P C23 105.1(4) . . ? C7 N1 N2 111.9(6) . . ? C7 N1 C1 128.1(7) . . ? N2 N1 C1 119.7(6) . . ? C9 N2 N1 105.5(6) . . ? C9 N2 Pd 123.2(5) . . ? N1 N2 Pd 120.9(4) . . ? C12 C11 C16 119.8(7) . . ? C12 C11 P 117.8(6) . . ? C16 C11 P 122.2(6) . . ? C9 C8 C7 106.3(7) . . ? C9 C8 P 125.4(6) . . ? C7 C8 P 127.7(6) . . ? O C7 N1 123.8(8) . . ? O C7 C8 130.8(8) . . ? N1 C7 C8 105.3(6) . . ? C15 C16 C11 118.4(9) . . ? C15 C16 H16 120.8 . . ? C11 C16 H16 120.8 . . ? C25 C24 C23 119.7(8) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C17 C22 C21 121.0(9) . . ? C17 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C17 C18 123.0(8) . . ? C22 C17 P 119.8(6) . . ? C18 C17 P 117.1(7) . . ? C28 C23 C24 120.8(8) . . ? C28 C23 P 120.6(6) . . ? C24 C23 P 118.2(6) . . ? C17 C18 C19 114.4(10) . . ? C17 C18 H18 122.8 . . ? C19 C18 H18 122.8 . . ? C11 C12 C13 120.4(9) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? Cl7 C30 Cl6 114.4(6) . . ? Cl7 C30 Cl5 107.1(7) . . ? Cl6 C30 Cl5 106.4(6) . . ? Cl7 C30 H30 109.6 . . ? Cl6 C30 H30 109.6 . . ? Cl5 C30 H30 109.6 . . ? C27 C28 C23 119.0(9) . . ? C27 C28 H28 120.5 . . ? C23 C28 H28 120.5 . . ? N2 C9 C8 110.7(7) . . ? N2 C9 C10 118.1(7) . . ? C8 C9 C10 131.2(8) . . ? C3 C2 C1 122.8(11) . . ? C3 C2 H2 118.6 . . ? C1 C2 H2 118.6 . . ? C2 C3 C4 117.8(11) . . ? C2 C3 H3 121.1 . . ? C4 C3 H3 121.1 . . ? C1 C6 C5 120.4(10) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C14 C13 C12 120.4(9) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C27 C26 C25 118.2(9) . . ? C27 C26 H26 120.9 . . ? C25 C26 H26 120.9 . . ? C6 C1 C2 119.9(9) . . ? C6 C1 N1 120.7(7) . . ? C2 C1 N1 119.4(8) . . ? C21 C20 C19 120.7(9) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C4 C5 C6 116.2(11) . . ? C4 C5 H5 121.9 . . ? C6 C5 H5 121.9 . . ? C3 C4 C5 122.9(11) . . ? C3 C4 H4 118.5 . . ? C5 C4 H4 118.5 . . ? C14 C15 C16 121.5(10) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C28 C27 C26 122.3(10) . . ? C28 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? C20 C19 C18 121.2(10) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C13 C14 C15 119.4(9) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C20 C21 C22 119.5(11) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C24 C25 C26 119.5(9) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? Cl4 C29 Cl3 113.8(8) . . ? Cl4 C29 Cl2 111.8(7) . . ? Cl3 C29 Cl2 109.4(7) . . ? Cl4 C29 H29 107.1 . . ? Cl3 C29 H29 107.1 . . ? Cl2 C29 H29 107.1 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 N1 N2 C9 4.5(8) . . . . ? C1 N1 N2 C9 178.8(6) . . . . ? C7 N1 N2 Pd 150.5(5) . . . . ? C1 N1 N2 Pd -35.3(8) . . . . ? N2 Pd N2 C9 37(100) 2_767 . . . ? Cl1 Pd N2 C9 76.6(6) . . . . ? Cl1 Pd N2 C9 -103.4(6) 2_767 . . . ? N2 Pd N2 N1 -102(100) 2_767 . . . ? Cl1 Pd N2 N1 -63.3(5) . . . . ? Cl1 Pd N2 N1 116.7(5) 2_767 . . . ? C8 P C11 C12 50.9(7) . . . . ? C17 P C11 C12 172.3(7) . . . . ? C23 P C11 C12 -73.3(7) . . . . ? C8 P C11 C16 -124.0(7) . . . . ? C17 P C11 C16 -2.6(8) . . . . ? C23 P C11 C16 111.7(7) . . . . ? C11 P C8 C9 39.2(8) . . . . ? C17 P C8 C9 -81.5(7) . . . . ? C23 P C8 C9 159.7(6) . . . . ? C11 P C8 C7 -150.6(6) . . . . ? C17 P C8 C7 88.7(7) . . . . ? C23 P C8 C7 -30.1(8) . . . . ? N2 N1 C7 O 177.5(6) . . . . ? C1 N1 C7 O 3.9(12) . . . . ? N2 N1 C7 C8 -1.8(8) . . . . ? C1 N1 C7 C8 -175.4(7) . . . . ? C9 C8 C7 O 179.2(8) . . . . ? P C8 C7 O 7.5(12) . . . . ? C9 C8 C7 N1 -1.6(8) . . . . ? P C8 C7 N1 -173.3(5) . . . . ? C12 C11 C16 C15 -0.7(13) . . . . ? P C11 C16 C15 174.2(7) . . . . ? C21 C22 C17 C18 -2.5(15) . . . . ? C21 C22 C17 P 175.1(8) . . . . ? C8 P C17 C22 -171.5(7) . . . . ? C11 P C17 C22 69.0(8) . . . . ? C23 P C17 C22 -47.4(8) . . . . ? C8 P C17 C18 6.2(8) . . . . ? C11 P C17 C18 -113.3(7) . . . . ? C23 P C17 C18 130.4(7) . . . . ? C25 C24 C23 C28 4.1(13) . . . . ? C25 C24 C23 P 177.5(7) . . . . ? C8 P C23 C28 -113.1(7) . . . . ? C11 P C23 C28 7.3(8) . . . . ? C17 P C23 C28 124.8(7) . . . . ? C8 P C23 C24 73.5(7) . . . . ? C11 P C23 C24 -166.1(7) . . . . ? C17 P C23 C24 -48.6(8) . . . . ? C22 C17 C18 C19 1.4(14) . . . . ? P C17 C18 C19 -176.2(7) . . . . ? C16 C11 C12 C13 -0.1(14) . . . . ? P C11 C12 C13 -175.2(8) . . . . ? C24 C23 C28 C27 0.4(14) . . . . ? P C23 C28 C27 -172.8(9) . . . . ? N1 N2 C9 C8 -5.5(8) . . . . ? Pd N2 C9 C8 -150.5(5) . . . . ? N1 N2 C9 C10 174.2(7) . . . . ? Pd N2 C9 C10 29.2(10) . . . . ? C7 C8 C9 N2 4.6(8) . . . . ? P C8 C9 N2 176.5(5) . . . . ? C7 C8 C9 C10 -175.1(9) . . . . ? P C8 C9 C10 -3.2(13) . . . . ? C1 C2 C3 C4 1(2) . . . . ? C11 C12 C13 C14 -0.2(16) . . . . ? C5 C6 C1 C2 0.9(16) . . . . ? C5 C6 C1 N1 179.0(9) . . . . ? C3 C2 C1 C6 -1.3(18) . . . . ? C3 C2 C1 N1 -179.4(10) . . . . ? C7 N1 C1 C6 130.1(9) . . . . ? N2 N1 C1 C6 -43.1(11) . . . . ? C7 N1 C1 C2 -51.7(12) . . . . ? N2 N1 C1 C2 135.1(9) . . . . ? C1 C6 C5 C4 -0.6(16) . . . . ? C2 C3 C4 C5 -1(2) . . . . ? C6 C5 C4 C3 0.8(19) . . . . ? C11 C16 C15 C14 1.9(16) . . . . ? C23 C28 C27 C26 -5.7(18) . . . . ? C25 C26 C27 C28 6.3(19) . . . . ? C21 C20 C19 C18 -2.1(19) . . . . ? C17 C18 C19 C20 0.8(16) . . . . ? C12 C13 C14 C15 1.4(17) . . . . ? C16 C15 C14 C13 -2.3(18) . . . . ? C19 C20 C21 C22 1.1(19) . . . . ? C17 C22 C21 C20 1.1(17) . . . . ? C23 C24 C25 C26 -3.4(14) . . . . ? C27 C26 C25 C24 -1.6(16) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.41 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.996 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.137