# Copyright The Royal Society of Chemistry, 1998 # Re cif file for structure in manuscript Dalton 7/07199J data_kcpd _audit_creation_date 98-01-16 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common ? #ActaC _chemical_formula_analytical ? #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural ? #ActaC _chemical_formula_sum C31.5_O1_H37_Pd1_P1_Cl1_B1_F4_N2 #ActaC _chemical_formula_weight 719.31 #ActaC _chemical_melting_point ? #ActaC _computing_data_collection ? #ActaC _computing_cell_refinement ? #ActaC _computing_data_reduction xtal #ActaC _computing_structure_solution xtal #ActaC _computing_structure_refinement xtal #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 18.788(4) #ActaC _cell_length_b 18.993(7) #ActaC _cell_length_c 18.700(7) #ActaC _cell_angle_alpha 90.00000 #ActaC _cell_angle_beta 90.00000 #ActaC _cell_angle_gamma 90.00000 #ActaC _cell_volume 6673(4) #ActaC _cell_formula_units_Z 8 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used ? #ActaC _cell_measurement_theta_min 12.0 #ActaC _cell_measurement_theta_max 18.5 #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting orthorhombic #ActaC _symmetry_space_group_name_H-M p_b_c_a #ActaC _symmetry_space_group_name_Hall -p_2ac_2ab #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z -x,-y,-z 1/2+x,+y,1/2-z 1/2-x,1/2+y,+z +x,1/2-y,1/2+z _exptl_crystal_description ? #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour ? #ActaC _exptl_crystal_size_max 0.41 #ActaC _exptl_crystal_size_mid 0.32 #ActaC _exptl_crystal_size_min 0.21 #ActaC _exptl_crystal_density_diffrn 1.432 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 2936 #ActaC _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu .73mm-1 #ActaC _exptl_absorpt_correction_type Gaussian #ActaC _exptl_absorpt_correction_T_min 0.82 #ActaC _exptl_absorpt_correction_T_max 0.86 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength ? #ActaC _diffrn_radiation_type xray_tube #ActaC _diffrn_radiation_source ? #ActaC _diffrn_radiation_monochromator ? #ActaC _diffrn_radiation_detector ? #ActaC _diffrn_measurement_device ? #ActaC _diffrn_measurement_method ? #ActaC _diffrn_standards_number ? #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time ? #ActaC _diffrn_standards_decay_% ? #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale 1 19.14 _diffrn_reflns_number ? #ActaC _diffrn_reflns_av_R_equivalents ? #ActaC _diffrn_reflns_av_sigmaI/netI ? #ActaC _diffrn_reflns_limit_h_min ? #ActaC _diffrn_reflns_limit_h_max ? #ActaC _diffrn_reflns_limit_k_min ? #ActaC _diffrn_reflns_limit_k_max ? #ActaC _diffrn_reflns_limit_l_min ? #ActaC _diffrn_reflns_limit_l_max ? #ActaC _diffrn_reflns_theta_min 0.0 #ActaC _diffrn_reflns_theta_max 25.0 #ActaC _diffrn_reflns_reduction_process ? #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 252 .002 .002 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 8 .008 .006 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 296 0 0 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Pd ? 0 8 -1.177 1.007 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 P ? 0 8 .09 .095 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 Cl ? 0 8 .132 .159 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 B ? 0 8 0 .001 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 F ? 0 32 .014 .01 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 N ? 0 16 .004 .003 Int_Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Pd .72125(2) .43465(2) .45129(2) .0454(2) Uani ? ? P1 .78061(8) .53298(7) .42596(7) .0468(8) Uani ? ? C111 .7257(3) .6112(3) .4118(3) .047(3) Uani ? ? C112 .6541(3) .6037(3) .3964(3) .056(4) Uani ? ? C113 .6128(3) .6621(4) .3835(3) .067(4) Uani ? ? C114 .6416(4) .7275(3) .3861(3) .068(5) Uani ? ? C115 .7123(4) .7361(3) .4029(3) .071(5) Uani ? ? C116 .7541(3) .6781(3) .4160(3) .061(4) Uani ? ? C121 .8372(3) .5577(3) .5002(3) .047(3) Uani ? ? C122 .8057(3) .5712(3) .5657(3) .060(4) Uani ? ? C123 .8466(4) .5877(3) .6255(3) .072(5) Uani ? ? C124 .9195(4) .5897(3) .6197(4) .080(5) Uani ? ? C125 .9509(3) .5762(3) .5560(5) .081(5) Uani ? ? C126 .9111(3) .5605(3) .4950(3) .064(4) Uani ? ? C131 .8408(3) .5244(3) .3508(3) .054(4) Uani ? ? C132 .8639(3) .4572(3) .3338(4) .073(5) Uani ? ? C133 .9125(4) .4472(4) .2803(5) .097(6) Uani ? ? C134 .9397(5) .5028(6) .2443(5) .117(8) Uani ? ? C135 .9170(5) .5695(5) .2586(5) .127(8) Uani ? ? C136 .8662(4) .5807(4) .3131(4) .088(6) Uani ? ? N1 .6631(2) .3443(2) .4835(2) .048(3) Uani ? ? C2 .6793(3) .3220(3) .5507(3) .048(3) Uani ? ? C21 .7473(3) .3527(3) .5772(3) .045(3) Uani ? ? O21 .75955(19) .41514(18) .55913(19) .053(2) Uani ? ? N21 .7929(2) .3165(2) .6175(2) .047(3) Uani ? ? C211 .7885(3) .2400(3) .6309(3) .058(4) Uani ? ? C212 .7792(4) .2244(3) .7095(3) .083(5) Uani ? ? C213 .8513(3) .2019(3) .5990(4) .077(5) Uani ? ? C214 .8563(3) .3530(3) .6479(3) .060(4) Uani ? ? C215 .9067(3) .3789(3) .5912(4) .078(5) Uani ? ? C216 .8344(4) .4102(3) .7000(4) .088(5) Uani ? ? C3 .6323(3) .2828(3) .5897(3) .054(4) Uani ? ? C4 .5691(3) .2615(3) .5594(4) .068(4) Uani ? ? C5 .5555(3) .2789(3) .4906(4) .074(5) Uani ? ? C6 .6031(3) .3207(3) .4540(3) .064(4) Uani ? ? C0 .6842(3) .4348(3) .3492(3) .061(4) Uani ? ? B .4660(5) .7255(5) .7259(5) .079(6) Uani ? ? F1 .3973(2) .7315(3) .7417(3) .153(5) Uani ? ? F2 .4811(3) .7695(3) .6722(3) .148(5) Uani ? ? F3 .5062(3) .7353(3) .7819(3) .178(5) Uani ? ? F4 .4767(3) .6597(3) .6993(3) .134(4) Uani ? ? Cl1 .5776(6) .4927(6) .5524(5) .247(11) Uani ? ? Cl2 .4797(9) .4704(9) .4584(7) .342(18) Uani ? ? C1 .5311(9) .4612(9) .5499(9) .094(13) Uani ? ? H112 .63194 .55695 .39578 .06900 Uiso ? ? H113 .56199 .65700 .37182 .08100 Uiso ? ? H114 .61113 .76831 .37469 .08900 Uiso ? ? H115 .73271 .78390 .40610 .09200 Uiso ? ? H116 .80468 .68356 .42824 .07700 Uiso ? ? H122 .75385 .56886 .56951 .07600 Uiso ? ? H123 .82383 .59731 .67178 .09200 Uiso ? ? H124 .94967 .60001 .66048 .10000 Uiso ? ? H125 1.00296 .57638 .55330 .09600 Uiso ? ? H126 .93482 .55008 .44887 .07900 Uiso ? ? H132 .84596 .41572 .36135 .09400 Uiso ? ? H133 .92816 .40017 .26620 .12500 Uiso ? ? H134 .97617 .49777 .20678 .14100 Uiso ? ? H135 .93802 .61033 .23288 .14700 Uiso ? ? H136 .84861 .62988 .32291 .11000 Uiso ? ? H211 .74645 .22014 .60812 .07600 Uiso ? ? H212a .73793 .24695 .72784 .11700 Uiso ? ? H212b .82003 .24234 .73526 .11700 Uiso ? ? H212c .77610 .17512 .71902 .11700 Uiso ? ? H213a .89495 .21863 .62075 .10900 Uiso ? ? H213b .85472 .20971 .54888 .10900 Uiso ? ? H213c .84932 .15188 .60720 .10900 Uiso ? ? H214 .88574 .31984 .67574 .07400 Uiso ? ? H215a .88182 .41165 .56087 .11000 Uiso ? ? H215b .92209 .34034 .56147 .11000 Uiso ? ? H215c .94779 .40172 .60944 .11000 Uiso ? ? H216a .80629 .39108 .73965 .12100 Uiso ? ? H216b .80529 .44504 .67738 .12100 Uiso ? ? H216c .87420 .43414 .72179 .12100 Uiso ? ? H3 .64301 .26938 .63994 .06900 Uiso ? ? H4 .53427 .23272 .58548 .08500 Uiso ? ? H5 .51191 .26191 .46640 .09000 Uiso ? ? H6 .59317 .33357 .40401 .08100 Uiso ? ? H0a .63025 .43789 .35065 .07500 Uiso ? ? H0b .71447 .46299 .31331 .07500 Uiso ? ? H0c .70919 .38693 .33476 .07500 Uiso ? ? H1a .49876 .47118 .58768 .15000 Uiso ? ? H1b .54331 .41135 .55325 .15000 Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Pd .0501(2) .0418(2) .0443(2) -.0011(3) -.0072(2) .0031(2) P1 .0501(9) .0424(8) .0478(8) .0019(8) -.0028(8) .0017(7) C111 .052(4) .049(3) .041(3) -.000(3) -.002(3) .002(3) C112 .052(4) .053(4) .062(4) -.001(3) .001(3) -.005(3) C113 .055(4) .070(5) .074(5) .009(4) -.003(3) .002(4) C114 .081(5) .063(4) .061(4) .020(4) -.010(4) .011(4) C115 .091(5) .049(4) .072(5) .004(4) -.013(4) .005(3) C116 .059(4) .049(4) .075(4) -.000(3) -.010(4) .010(3) C121 .052(3) .036(3) .055(4) .004(3) -.010(3) .003(3) C122 .066(4) .052(4) .063(4) .004(3) -.006(3) -.002(3) C123 .098(6) .059(4) .061(4) .007(4) -.012(4) -.008(3) C124 .092(6) .060(5) .086(6) .001(4) -.038(5) -.004(4) C125 .056(4) .073(5) .113(6) .000(4) -.025(5) -.007(5) C126 .058(4) .059(4) .075(4) .004(4) -.008(3) -.003(4) C131 .051(4) .061(4) .050(4) .004(3) .001(3) .001(3) C132 .067(4) .079(5) .072(5) .013(4) .006(4) -.012(4) C133 .079(6) .114(7) .096(6) .014(5) .010(5) -.037(6) C134 .090(7) .166(10) .096(7) .015(7) .039(5) -.026(7) C135 .137(8) .138(8) .105(7) .009(7) .062(6) .028(7) C136 .096(6) .087(6) .082(5) .004(4) .027(4) .015(4) N1 .048(3) .045(3) .050(3) -.004(2) -.009(2) .004(2) C2 .044(3) .043(3) .057(4) .003(3) -.004(3) .001(3) C21 .050(3) .048(3) .038(3) -.002(3) -.000(3) .003(3) O21 .060(2) .046(2) .053(2) -.0056(18) -.016(2) .0076(19) N21 .043(3) .053(3) .044(3) -.007(2) -.008(2) .009(2) C211 .055(4) .049(3) .068(4) -.004(3) -.007(4) .008(3) C212 .089(5) .090(5) .068(5) -.015(5) -.005(4) .039(4) C213 .070(5) .071(4) .090(5) .009(4) -.010(4) .004(4) C214 .053(4) .063(4) .065(4) -.013(3) -.021(3) .019(4) C215 .053(4) .083(5) .097(5) -.015(4) -.011(4) .025(4) C216 .114(6) .079(5) .070(5) -.013(5) -.032(5) -.005(4) C3 .045(3) .062(4) .056(4) .003(3) -.002(3) .013(3) C4 .052(4) .067(4) .086(6) -.008(3) -.003(4) .020(4) C5 .055(4) .072(5) .096(6) -.020(4) -.022(4) .012(4) C6 .062(4) .062(4) .069(4) -.012(3) -.022(4) .004(4) C0 .069(4) .063(4) .050(4) -.005(4) -.012(3) .003(3) B .089(7) .064(5) .084(7) -.016(5) -.009(6) .010(5) F1 .081(3) .215(6) .162(5) -.018(4) .042(3) -.040(4) F2 .185(5) .127(4) .131(4) -.021(4) .049(4) .031(4) F3 .162(5) .245(7) .127(5) -.052(5) -.063(4) -.051(4) F4 .156(5) .119(4) .129(4) .041(4) -.065(4) -.008(3) Cl1 .323(14) .181(8) .236(10) .131(9) .165(10) .049(8) Cl2 .39(2) .39(2) .247(13) .108(16) .092(15) .056(13) C1 .048(9) .067(11) .17(2) -.016(8) .025(12) -.013(12) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details ? _refine_ls_structure_factor_coef ? #ActaC _refine_ls_matrix_type ? #ActaC _refine_ls_weighting_scheme ? #ActaC _refine_ls_hydrogen_treatment ? #ActaC _refine_ls_extinction_method ? #ActaC _refine_ls_extinction_coef ? #ActaC _refine_ls_extinction_expression ? _refine_ls_abs_structure_details ? #ActaC _refine_ls_abs_structure_Flack ? #ActaC _refine_ls_number_reflns ? #ActaC _refine_ls_number_parameters ? #ActaC _refine_ls_number_restraints ? #ActaC _refine_ls_number_constraints ? #ActaC _refine_ls_R_factor_all ? #ActaC _refine_ls_R_factor_obs ? #ActaC _refine_ls_wR_factor_all ? #ActaC _refine_ls_wR_factor_obs ? #ActaC _refine_ls_goodness_of_fit_all ? #ActaC _refine_ls_goodness_of_fit_obs ? #ActaC _refine_ls_shift/esd_max ? #ActaC _refine_ls_shift/esd_mean ? #ActaC _refine_diff_density_min ? #ActaC _refine_diff_density_max ? #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Pd P1 2.2262(15) . . ? Pd N1 2.122(4) . . ? Pd O21 2.173(4) . . ? Pd C0 2.032(6) . . ? P1 C111 1.828(6) . . ? P1 C121 1.810(6) . . ? P1 C131 1.812(6) . . ? C111 C112 1.383(8) . . ? C111 C116 1.380(8) . . ? C112 C113 1.376(9) . . ? C112 H112 .981(6) . . ? C113 C114 1.355(10) . . ? C113 H113 .983(6) . . ? C114 C115 1.374(10) . . ? C114 H114 .988(7) . . ? C115 C116 1.376(9) . . ? C115 H115 .988(6) . . ? C116 H116 .983(6) . . ? C121 C122 1.384(8) . . ? C121 C126 1.394(8) . . ? C122 C123 1.392(9) . . ? C122 H122 .978(6) . . ? C123 C124 1.375(12) . . ? C123 H123 .983(7) . . ? C124 C125 1.352(12) . . ? C124 H124 .970(8) . . ? C125 C126 1.395(10) . . ? C125 H125 .980(6) . . ? C126 H126 .991(6) . . ? C131 C132 1.385(9) . . ? C131 C136 1.366(9) . . ? C132 C133 1.368(11) . . ? C132 H132 1.000(7) . . ? C133 C134 1.353(13) . . ? C133 H133 .978(8) . . ? C134 C135 1.363(15) . . ? C134 H134 .985(9) . . ? C135 C136 1.412(12) . . ? C135 H135 .993(10) . . ? C136 H136 1.008(7) . . ? N1 C2 1.360(7) . . ? N1 C6 1.333(7) . . ? C2 C21 1.490(8) . . ? C2 C3 1.366(8) . . ? C21 O21 1.255(7) . . ? C21 N21 1.331(7) . . ? N21 C211 1.476(7) . . ? N21 C214 1.491(7) . . ? C211 C212 1.510(9) . . ? C211 C213 1.507(9) . . ? C211 H211 .972(6) . . ? C212 H212a .950(7) . . ? C212 H212b .968(7) . . ? C212 H212c .955(6) . . ? C213 H213a .970(7) . . ? C213 H213b .951(7) . . ? C213 H213c .962(6) . . ? C214 C215 1.503(9) . . ? C214 C216 1.517(9) . . ? C214 H214 .988(6) . . ? C215 H215a .963(7) . . ? C215 H215b .964(7) . . ? C215 H215c .948(6) . . ? C216 H216a .979(7) . . ? C216 H216b .957(7) . . ? C216 H216c .966(7) . . ? C3 C4 1.377(8) . . ? C3 H3 .994(6) . . ? C4 C5 1.352(10) . . ? C4 H4 .983(6) . . ? C5 C6 1.378(9) . . ? C5 H5 .989(7) . . ? C6 H6 .984(6) . . ? C0 H0a 1.016(6) . . ? C0 H0b 1.029(6) . . ? C0 H0c 1.058(6) . . ? B F1 1.329(11) . . ? B F2 1.336(11) . . ? B F3 1.305(11) . . ? B F4 1.360(10) . . ? Cl1 C1 1.06(2) . . ? Cl1 H1a 1.673(11) . . ? Cl1 H1b 1.675(11) . . ? Cl1 Cl2 1.30(2) . 5_666 ? Cl2 C1 1.97(2) . . ? Cl2 Cl2 2.06(2) . 5_666 ? Cl2 C1 1.32(2) . 5_666 ? Cl2 H1a 1.462(15) . 5_666 ? C1 H1a .951(17) . . ? C1 H1b .977(16) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC Pd C111 3.435(5) . . ? Pd C121 3.323(5) . . ? Pd C131 3.389(6) . . ? Pd C132 3.492(7) . . ? Pd C2 2.941(6) . . ? Pd C21 2.865(5) . . ? Pd N21 4.063(4) . . ? Pd C6 3.100(6) . . ? Pd Cl1 3.474(11) . . ? Pd H112 3.0477(8) . . ? Pd H115 3.1081(10) . 7_645 ? Pd H132 2.9065(7) . . ? Pd H0a 2.5434(7) . . ? Pd H0b 2.6388(10) . . ? Pd H0c 2.3709(8) . . ? P1 C112 2.785(6) . . ? P1 C116 2.807(6) . . ? P1 C122 2.752(6) . . ? P1 C126 2.821(6) . . ? P1 C132 2.736(7) . . ? P1 C136 2.804(7) . . ? P1 C0 2.969(6) . . ? C111 C113 2.391(8) . . ? C111 C114 2.757(9) . . ? C111 C115 2.391(8) . . ? C111 C121 2.854(8) . . ? C111 C131 2.949(8) . . ? C111 H112 2.063(6) . . ? C111 H116 2.046(6) . . ? C112 C114 2.370(9) . . ? C112 C115 2.744(8) . . ? C112 C116 2.379(8) . . ? C112 H113 2.057(6) . . ? C113 C115 2.367(9) . . ? C113 C116 2.741(9) . . ? C113 F3 3.379(9) . 8_564 ? C113 H112 2.042(7) . . ? C113 H114 2.024(7) . . ? C114 C116 2.379(9) . . ? C114 F3 3.282(9) . 8_564 ? C114 H113 2.025(7) . . ? C114 H115 2.054(7) . . ? C115 N1 3.460(8) . 7_655 ? C115 H114 2.064(7) . . ? C115 H116 2.058(7) . . ? C116 H115 2.058(6) . . ? C116 H136 2.649(6) . . ? C121 C123 2.418(8) . . ? C121 C124 2.785(10) . . ? C121 C125 2.403(9) . . ? C121 C131 2.865(8) . . ? C121 H122 2.044(5) . . ? C121 H126 2.075(5) . . ? C122 C124 2.390(10) . . ? C122 C125 2.735(9) . . ? C122 C126 2.389(8) . . ? C122 H123 2.073(6) . . ? C123 C125 2.360(10) . . ? C123 C126 2.772(9) . . ? C123 H122 2.064(8) . . ? C123 H124 2.057(8) . . ? C124 C126 2.400(10) . . ? C124 H123 2.050(8) . . ? C124 H125 2.015(8) . . ? C125 H124 2.005(9) . . ? C125 H126 2.086(9) . . ? C126 H125 2.062(6) . . ? C131 C133 2.388(10) . . ? C131 C134 2.754(11) . . ? C131 C135 2.399(11) . . ? C131 H126 2.593(6) . . ? C131 H132 2.077(6) . . ? C131 H136 2.074(6) . . ? C132 C134 2.363(11) . . ? C132 C135 2.744(12) . . ? C132 C136 2.378(10) . . ? C132 H133 2.057(7) . . ? C133 C135 2.360(13) . . ? C133 C136 2.749(11) . . ? C133 F4 3.279(10) . 2_664 ? C133 H132 2.053(8) . . ? C133 H134 2.060(8) . . ? C134 C136 2.397(12) . . ? C134 F4 3.564(12) . 2_664 ? C134 H133 2.004(11) . . ? C134 H135 2.053(11) . . ? C135 F2 3.531(11) . 3_566 ? C135 H134 2.008(10) . . ? C135 H136 2.101(9) . . ? C136 F2 3.581(9) . 3_566 ? C136 H135 2.094(7) . . ? N1 C21 2.367(7) . . ? N1 O21 2.663(6) . . ? N1 N21 3.536(6) . . ? N1 C3 2.376(7) . . ? N1 C4 2.758(8) . . ? N1 C5 2.377(8) . . ? N1 C0 3.070(7) . . ? N1 F4 4.312(7) . 5_666 ? N1 Cl1 3.492(11) . . ? N1 C1 3.554(17) . . ? N1 H115 2.690(4) . 7_645 ? N1 H116 3.279(4) . 7_645 ? N1 H3 3.275(4) . . ? N1 H5 3.259(4) . . ? N1 H6 1.995(4) . . ? N1 H0a 3.117(4) . . ? N1 H0c 3.023(4) . . ? N1 H1b 2.897(4) . . ? C2 O21 2.330(6) . . ? C2 N21 2.476(7) . . ? C2 C211 2.981(8) . . ? C2 C4 2.373(8) . . ? C2 C5 2.709(8) . . ? C2 C6 2.306(9) . . ? C2 H211 2.548(5) . . ? C2 H3 2.061(6) . . ? C21 C211 2.487(8) . . ? C21 C214 2.436(8) . . ? C21 C3 2.547(8) . . ? C21 H211 2.583(6) . . ? O21 N21 2.258(5) . . ? O21 C214 2.729(7) . . ? O21 C215 2.912(7) . . ? O21 C216 2.988(8) . . ? O21 H215a 2.298(4) . . ? O21 H216b 2.439(4) . . ? N21 C212 2.467(8) . . ? N21 C213 2.462(8) . . ? N21 C215 2.494(7) . . ? N21 C216 2.482(8) . . ? N21 C3 3.128(7) . . ? N21 H211 2.034(4) . . ? N21 H212a 2.659(4) . . ? N21 H212b 2.663(4) . . ? N21 H212c 3.303(4) . . ? N21 H213a 2.670(4) . . ? N21 H213b 2.665(4) . . ? N21 H213c 3.306(4) . . ? N21 H214 2.058(4) . . ? N21 H215a 2.680(4) . . ? N21 H215b 2.682(4) . . ? N21 H215c 3.334(4) . . ? N21 H216a 2.700(4) . . ? N21 H216b 2.697(4) . . ? N21 H216c 3.337(4) . . ? N21 H3 2.985(4) . . ? C211 C214 2.517(8) . . ? C211 H212a 2.051(6) . . ? C211 H212b 2.041(6) . . ? C211 H212c 2.071(6) . . ? C211 H213a 2.050(6) . . ? C211 H213b 2.057(6) . . ? C211 H213c 2.074(6) . . ? C211 H214 2.519(6) . . ? C212 C213 2.507(9) . . ? C212 F1 3.443(8) . 4_646 ? C212 H211 1.995(6) . . ? C213 F2 3.667(8) . 7_645 ? C213 H211 2.007(7) . . ? C214 F2 3.473(8) . 7_645 ? C214 H215a 2.029(6) . . ? C214 H215b 2.049(6) . . ? C214 H215c 2.080(6) . . ? C214 H216a 2.086(6) . . ? C214 H216b 2.068(6) . . ? C214 H216c 2.097(6) . . ? C215 C216 2.518(10) . . ? C215 F2 3.325(8) . 7_645 ? C215 H214 1.978(7) . . ? C216 H214 2.021(7) . . ? C3 C5 2.351(9) . . ? C3 C6 2.694(9) . . ? C3 F1 3.347(8) . 4_646 ? C3 F3 3.654(8) . 4_646 ? C3 H211 2.476(6) . . ? C3 H4 2.075(6) . . ? C4 C6 2.356(9) . . ? C4 F3 3.326(9) . 4_646 ? C4 H3 2.054(7) . . ? C4 H5 2.044(7) . . ? C5 F2 3.254(9) . 5_666 ? C5 H4 2.019(7) . . ? C5 H6 2.049(7) . . ? C6 B 3.711(12) . 5_666 ? C6 F2 3.319(8) . 5_666 ? C6 F4 3.257(8) . 5_666 ? C6 H5 2.058(6) . . ? C0 F4 3.631(8) . 5_666 ? C0 H112 2.666(6) . . ? B H124 3.208(10) . 6_456 ? B H133 3.197(10) . 2_665 ? B H135 3.255(9) . 3_466 ? B H213a 3.272(10) . 7_655 ? B H214 3.442(10) . 7_655 ? B H3 3.345(10) . 4_656 ? B H6 2.897(10) . 5_666 ? F1 F2 2.164(7) . . ? F1 F3 2.181(7) . . ? F1 F4 2.171(7) . . ? F1 H123 3.319(6) . 6_456 ? F1 H124 3.248(6) . 6_456 ? F1 H135 3.137(6) . 3_466 ? F1 H136 3.038(6) . 3_466 ? F1 H212a 2.621(5) . 4_656 ? F1 H3 2.449(5) . 4_656 ? F1 H6 2.996(6) . 5_666 ? F1 H0c 3.332(5) . 5_666 ? F2 F3 2.202(8) . . ? F2 F4 2.149(7) . . ? F2 H135 3.001(5) . 3_466 ? F2 H136 3.139(5) . 3_466 ? F2 H213a 2.700(5) . 7_655 ? F2 H214 2.679(5) . 7_655 ? F2 H215b 3.068(5) . 7_655 ? F2 H215c 3.077(5) . 7_655 ? F2 H5 2.664(5) . 5_666 ? F2 H6 2.795(5) . 5_666 ? F3 F4 2.180(8) . . ? F3 H113 2.848(6) . 8_565 ? F3 H114 2.627(6) . 8_565 ? F3 H124 2.982(6) . 6_456 ? F3 H133 2.868(6) . 2_665 ? F3 H135 3.212(6) . 3_466 ? F3 H214 3.262(6) . 7_655 ? F3 H3 3.227(6) . 4_656 ? F3 H4 2.595(6) . 4_656 ? F4 H124 2.901(5) . 6_456 ? F4 H133 2.460(5) . 2_665 ? F4 H134 3.121(5) . 2_665 ? F4 H213a 3.038(5) . 7_655 ? F4 H6 2.340(5) . 5_666 ? F4 H0a 2.889(5) . 5_666 ? Cl1 Cl2 2.579(18) . . ? Cl1 C1 2.93(2) . 5_666 ? Cl2 H1a 2.443(12) . . ? Cl2 H1b 2.415(15) . . ? Cl2 H1b 2.297(17) . 5_666 ? C1 C1 2.65(2) . 5_666 ? H112 H113 2.3535(6) . . ? H113 H114 2.3075(7) . . ? H114 H115 2.3771(5) . . ? H115 H116 2.3731(6) . . ? H116 H136 2.3665(6) . . ? H122 H123 2.3829(6) . . ? H123 H124 2.3743(5) . . ? H124 H125 2.2849(7) . . ? H125 H126 2.3879(6) . . ? H132 H133 2.3745(5) . . ? H133 H134 2.3419(6) . . ? H134 H135 2.3070(7) . . ? H134 H1a 2.3516(8) . 2_664 ? H211 H212a 2.3015(8) . . ? H211 H212c 2.3113(7) . . ? H211 H213b 2.3247(4) . . ? H211 H213c 2.3273(4) . . ? H211 H3 2.2373(4) . . ? H212a H212b 1.5512(3) . . ? H212a H212c 1.5501(4) . . ? H212b H212c 1.5503(4) . . ? H212b H214 2.2203(4) . . ? H213a H213b 1.5512(4) . . ? H213a H213c 1.5513(4) . . ? H213a H214 2.1869(6) . . ? H213b H213c 1.5512(4) . . ? H214 H215b 2.2769(8) . . ? H214 H215c 2.3054(5) . . ? H214 H216a 2.3425(4) . . ? H214 H216c 2.3455(7) . . ? H215a H215b 1.5514(4) . . ? H215a H215c 1.5481(3) . . ? H215b H215c 1.5482(4) . . ? H216a H216b 1.5513(4) . . ? H216a H216c 1.5519(3) . . ? H216b H216c 1.5520(3) . . ? H3 H4 2.3866(4) . . ? H4 H5 2.3329(8) . . ? H5 H6 2.3547(4) . . ? H6 H0a 2.3252(6) . . ? H0a H0b 1.7940(3) . . ? H0a H0c 1.7958(3) . . ? H0b H0c 1.5025(5) . . ? H1a H1b 1.5513(3) . . ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC P1 Pd N1 175.52(12) . . . ? P1 Pd O21 100.06(10) . . . ? P1 Pd C0 88.30(17) . . . ? N1 Pd O21 76.65(15) . . . ? N1 Pd C0 95.3(2) . . . ? O21 Pd C0 170.3(2) . . . ? Pd P1 C111 115.5(2) . . . ? Pd P1 C121 110.42(18) . . . ? Pd P1 C131 113.7(2) . . . ? C111 P1 C121 103.4(2) . . . ? C111 P1 C131 108.2(3) . . . ? C121 P1 C131 104.6(3) . . . ? P1 C111 C112 119.7(4) . . . ? P1 C111 C116 121.4(4) . . . ? C112 C111 C116 118.9(5) . . . ? C111 C112 C113 120.2(5) . . . ? C111 C112 H112 120.6(5) . . . ? C113 C112 H112 119.2(6) . . . ? C112 C113 C114 120.4(6) . . . ? C112 C113 H113 120.5(6) . . . ? C114 C113 H113 119.1(7) . . . ? C113 C114 C115 120.3(6) . . . ? C113 C114 H114 118.7(7) . . . ? C115 C114 H114 121.1(6) . . . ? C114 C115 C116 119.8(6) . . . ? C114 C115 H115 120.0(6) . . . ? C116 C115 H115 120.2(7) . . . ? C111 C116 C115 120.4(6) . . . ? C111 C116 H116 119.0(6) . . . ? C115 C116 H116 120.6(6) . . . ? P1 C121 C122 118.4(4) . . . ? P1 C121 C126 122.9(4) . . . ? C122 C121 C126 118.6(5) . . . ? C121 C122 C123 121.1(6) . . . ? C121 C122 H122 118.8(6) . . . ? C123 C122 H122 120.1(6) . . . ? C122 C123 C124 119.5(6) . . . ? C122 C123 H123 120.6(7) . . . ? C124 C123 H123 119.9(7) . . . ? C123 C124 C125 119.9(7) . . . ? C123 C124 H124 121.7(8) . . . ? C125 C124 H124 118.5(8) . . . ? C124 C125 C126 121.8(6) . . . ? C124 C125 H125 118.7(8) . . . ? C126 C125 H125 119.5(8) . . . ? C121 C126 C125 119.0(6) . . . ? C121 C126 H126 120.0(6) . . . ? C125 C126 H126 121.0(6) . . . ? P1 C131 C132 117.1(5) . . . ? P1 C131 C136 123.3(5) . . . ? C132 C131 C136 119.6(6) . . . ? C131 C132 C133 120.3(6) . . . ? C131 C132 H132 120.2(6) . . . ? C133 C132 H132 119.5(7) . . . ? C132 C133 C134 120.6(8) . . . ? C132 C133 H133 121.7(8) . . . ? C134 C133 H133 117.7(8) . . . ? C133 C134 C135 120.7(8) . . . ? C133 C134 H134 122.8(11) . . . ? C135 C134 H134 116.6(10) . . . ? C134 C135 C136 119.5(8) . . . ? C134 C135 H135 120.4(9) . . . ? C136 C135 H135 120.0(9) . . . ? C131 C136 C135 119.4(7) . . . ? C131 C136 H136 121.1(7) . . . ? C135 C136 H136 119.5(7) . . . ? Pd N1 C2 113.5(3) . . . ? Pd N1 C6 126.1(4) . . . ? C2 N1 C6 117.8(5) . . . ? N1 C2 C21 112.2(4) . . . ? N1 C2 C3 121.3(5) . . . ? C21 C2 C3 126.1(5) . . . ? C2 C21 O21 115.9(5) . . . ? C2 C21 N21 122.6(5) . . . ? O21 C21 N21 121.6(5) . . . ? Pd O21 C21 110.5(3) . . . ? C21 N21 C211 124.6(4) . . . ? C21 N21 C214 119.2(4) . . . ? C211 N21 C214 116.0(4) . . . ? N21 C211 C212 111.4(5) . . . ? N21 C211 C213 111.2(5) . . . ? N21 C211 H211 110.7(5) . . . ? C212 C211 C213 112.4(5) . . . ? C212 C211 H211 104.9(5) . . . ? C213 C211 H211 106.1(5) . . . ? C211 C212 H212a 110.9(6) . . . ? C211 C212 H212b 109.0(6) . . . ? C211 C212 H212c 112.4(6) . . . ? H212a C212 H212b 108.0(6) . . . ? H212a C212 H212c 108.9(6) . . . ? H212b C212 H212c 107.5(6) . . . ? C211 C213 H213a 109.8(6) . . . ? C211 C213 H213b 111.5(6) . . . ? C211 C213 H213c 112.4(6) . . . ? H213a C213 H213b 107.7(6) . . . ? H213a C213 H213c 106.8(6) . . . ? H213b C213 H213c 108.3(6) . . . ? N21 C214 C215 112.8(5) . . . ? N21 C214 C216 111.2(5) . . . ? N21 C214 H214 110.5(5) . . . ? C215 C214 C216 113.0(5) . . . ? C215 C214 H214 103.2(5) . . . ? C216 C214 H214 105.7(5) . . . ? C214 C215 H215a 108.7(5) . . . ? C214 C215 H215b 110.3(6) . . . ? C214 C215 H215c 114.1(6) . . . ? H215a C215 H215b 107.2(7) . . . ? H215a C215 H215c 108.2(6) . . . ? H215b C215 H215c 108.1(6) . . . ? C214 C216 H216a 111.5(6) . . . ? C214 C216 H216b 111.4(6) . . . ? C214 C216 H216c 113.4(6) . . . ? H216a C216 H216b 106.5(7) . . . ? H216a C216 H216c 105.9(6) . . . ? H216b C216 H216c 107.7(6) . . . ? C2 C3 C4 119.8(6) . . . ? C2 C3 H3 121.0(5) . . . ? C4 C3 H3 119.3(6) . . . ? C3 C4 C5 118.9(6) . . . ? C3 C4 H4 122.2(7) . . . ? C5 C4 H4 118.8(6) . . . ? C4 C5 C6 119.3(6) . . . ? C4 C5 H5 120.8(6) . . . ? C6 C5 H5 119.9(7) . . . ? N1 C6 C5 122.5(6) . . . ? N1 C6 H6 118.0(6) . . . ? C5 C6 H6 119.4(6) . . . ? Pd C0 H0a 108.4(4) . . . ? Pd C0 H0b 115.1(4) . . . ? Pd C0 H0c 95.0(4) . . . ? H0a C0 H0b 122.6(6) . . . ? H0a C0 H0c 119.9(6) . . . ? H0b C0 H0c 92.1(4) . . . ? F1 B F2 108.6(8) . . . ? F1 B F3 111.8(8) . . . ? F1 B F4 107.7(7) . . . ? F2 B F3 113.0(8) . . . ? F2 B F4 105.7(7) . . . ? F3 B F4 109.8(8) . . . ? C1 Cl1 H1a 31.7(9) . . . ? C1 Cl1 H1b 33.1(9) . . . ? C1 Cl1 Cl2 67.3(13) . . 5_666 ? H1a Cl1 H1b 55.2(3) . . . ? H1a Cl1 Cl2 57.3(8) . . 5_666 ? H1b Cl1 Cl2 100.3(10) . . 5_666 ? C1 Cl2 Cl1 126.0(11) . . 5_666 ? C1 Cl2 Cl2 38.2(7) . . 5_666 ? C1 Cl2 C1 105.3(12) . . 5_666 ? C1 Cl2 H1a 116.3(11) . . 5_666 ? Cl1 Cl2 Cl2 97.5(11) 5_666 . 5_666 ? Cl1 Cl2 C1 47.7(10) 5_666 . 5_666 ? Cl1 Cl2 H1a 74.3(9) 5_666 . 5_666 ? Cl2 Cl2 C1 67.1(10) 5_666 . 5_666 ? Cl2 Cl2 H1a 85.9(9) 5_666 . 5_666 ? C1 Cl2 H1a 39.5(8) 5_666 . 5_666 ? Cl1 C1 Cl2 113.1(14) . . . ? Cl1 C1 H1a 112.4(17) . . . ? Cl1 C1 H1b 110.5(16) . . . ? Cl1 C1 Cl2 65.0(13) . . 5_666 ? Cl2 C1 H1a 108.4(13) . . . ? Cl2 C1 H1b 104.9(13) . . . ? Cl2 C1 Cl2 74.7(11) . . 5_666 ? H1a C1 H1b 107.2(16) . . . ? H1a C1 Cl2 78.1(13) . . 5_666 ? H1b C1 Cl2 174.3(18) . . 5_666 ? Cl1 H1a C1 35.9(10) . . . ? Cl1 H1a Cl2 48.4(8) . . 5_666 ? C1 H1a Cl2 62.3(12) . . 5_666 ? Cl1 H1b C1 36.4(10) . . . ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min ? _reflns_limit_h_max ? _reflns_limit_k_min ? _reflns_limit_k_max ? _reflns_limit_l_min ? _reflns_limit_l_max ? _reflns_number_total ? #ActaC _reflns_number_observed ? #ActaC _reflns_observed_criterion refl_observed_if_F____>_***__sigma(F___) _reflns_d_resolution_high ? _reflns_d_resolution_low ? loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 4.4322 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_observed_status _refln_scale_group_code ? ? ? ? ? ? ? ? _publ_requested_journal ? #ActaC _publ_requested_coeditor_name ? #ActaC _publ_contact_author #ActaC ; ? name ? institute ? department ? address ? city ? country ; _publ_contact_letter #ActaC ; ? letter to co-editor ; _publ_contact_author_phone ? #ActaC _publ_contact_author_fax ? #ActaC _publ_contact_author_email ? #ActaC loop_ _publ_author_name #ActaC _publ_author_address #ActaC '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title #ActaC ; ? ; _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; ? ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; #============================================================================== # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ?