# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5-eu _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common "[{{Eu(DMSO)}2(HBr3L')(H3Br2L'')}2({mu-}OH)2 ] 18 DMSO" _chemical_melting_point ? _chemical_formula_moiety 'C82 H70 Br10 Eu4 N24 O16 S4, 12(C2 H6 O S)' _chemical_formula_sum 'C106 H142 Br10 Eu4 N24 O28 S16' _chemical_formula_weight 4120.34 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.4400(5) _cell_length_b 15.7422(6) _cell_length_c 18.2586(6) _cell_angle_alpha 74.988(3) _cell_angle_beta 86.298(3) _cell_angle_gamma 75.568(3) _cell_volume 3882.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7486 _cell_measurement_theta_min 2.9033 _cell_measurement_theta_max 28.9071 _exptl_crystal_description plate _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.3415 _exptl_crystal_size_mid 0.1546 _exptl_crystal_size_min 0.0265 _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2028 _exptl_absorpt_coefficient_mu 4.451 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4954 _exptl_absorpt_correction_T_max 0.8900 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '736 images at 1.0 deg in \w and 45 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43697 _diffrn_reflns_av_R_equivalents 0.0803 _diffrn_reflns_av_sigmaI/netI 0.1996 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13662 _reflns_number_gt 6869 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.32.24 Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.32.24 Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.32.24 Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0363P)^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 13662 _refine_ls_number_parameters 797 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1031 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1024 _refine_ls_wR_factor_gt 0.0960 _refine_ls_goodness_of_fit_ref 0.810 _refine_ls_restrained_S_all 0.816 _refine_ls_shift/su_max 0.001 _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 Eu1 Eu 0.38476(3) 0.56209(3) 0.45045(3) 0.01175(13) Uani 1 1 d . . . Eu2 Eu 0.54831(3) 0.31673(3) 0.41378(3) 0.01392(13) Uani 1 1 d . . . O7 O 0.4873(4) 0.4195(4) 0.4883(3) 0.0220(16) Uani 1 1 d . . . H7 H 0.4520 0.3972 0.5224 0.033 Uiso 1 1 calc R . . C1 C 0.5258(6) 0.6163(6) 0.3079(5) 0.017(2) Uani 1 1 d . . . N11 N 0.4771(5) 0.7015(5) 0.3002(5) 0.026(2) Uani 1 1 d . . . N12 N 0.4039(5) 0.7027(5) 0.3543(5) 0.026(2) Uani 1 1 d . . . C11 C 0.3438(7) 0.7816(7) 0.3455(6) 0.028(3) Uani 1 1 d . . . H11 H 0.3514 0.8280 0.3020 0.034 Uiso 1 1 calc R . . C12 C 0.2662(6) 0.8039(6) 0.3970(6) 0.025(2) Uani 1 1 d . . . C13 C 0.2615(7) 0.7586(6) 0.4751(6) 0.025(3) Uani 1 1 d . . . C14 C 0.1873(7) 0.7891(6) 0.5193(6) 0.029(3) Uani 1 1 d . . . H14 H 0.1871 0.7599 0.5718 0.034 Uiso 1 1 calc R . . C15 C 0.1133(7) 0.8610(6) 0.4895(7) 0.035(3) Uani 1 1 d . . . H15 H 0.0601 0.8791 0.5202 0.043 Uiso 1 1 calc R . . C16 C 0.1166(7) 0.9071(6) 0.4140(6) 0.028(3) Uani 1 1 d . . . C17 C 0.1901(6) 0.8807(6) 0.3693(6) 0.031(3) Uani 1 1 d . . . H17 H 0.1912 0.9143 0.3180 0.037 Uiso 1 1 calc R . . O1 O 0.3357(4) 0.6853(4) 0.5060(4) 0.0294(17) Uani 1 1 d . . . Br1 Br 0.01340(8) 1.00646(7) 0.37119(7) 0.0458(3) Uani 1 1 d . . . N31 N 0.5063(5) 0.5456(5) 0.3562(5) 0.026(2) Uani 1 1 d . . . N32 N 0.5733(5) 0.4684(5) 0.3442(4) 0.021(2) Uani 1 1 d . . . C31 C 0.6315(7) 0.4954(6) 0.2893(6) 0.026(3) Uani 1 1 d . . . C32 C 0.7125(6) 0.4336(6) 0.2632(5) 0.023(2) Uani 1 1 d . . . C33 C 0.7114(7) 0.3388(7) 0.2786(6) 0.030(3) Uani 1 1 d . . . C34 C 0.7868(7) 0.2806(7) 0.2497(6) 0.038(3) Uani 1 1 d . . . H34 H 0.7855 0.2191 0.2560 0.046 Uiso 1 1 calc R . . C35 C 0.8627(8) 0.3119(7) 0.2124(6) 0.039(3) Uani 1 1 d . . . H35 H 0.9143 0.2712 0.1950 0.047 Uiso 1 1 calc R . . C36 C 0.8643(7) 0.4036(7) 0.2000(6) 0.037(3) Uani 1 1 d . . . C37 C 0.7896(6) 0.4637(6) 0.2242(5) 0.025(2) Uani 1 1 d . . . H37 H 0.7906 0.5258 0.2144 0.030 Uiso 1 1 calc R . . O3 O 0.6423(5) 0.3066(4) 0.3155(4) 0.0338(18) Uani 1 1 d . . . Br3 Br 0.96849(8) 0.44302(8) 0.14599(7) 0.0463(3) Uani 1 1 d . . . N21 N 0.6046(5) 0.5871(5) 0.2663(5) 0.025(2) Uani 1 1 d . . . N22 N 0.6493(6) 0.6348(5) 0.2056(5) 0.030(2) Uani 1 1 d . . . C21 C 0.6214(7) 0.7215(7) 0.1869(6) 0.033(3) Uani 1 1 d . . . H21 H 0.5702 0.7519 0.2133 0.039 Uiso 1 1 calc R . . C22 C 0.6699(7) 0.7733(7) 0.1241(6) 0.032(3) Uani 1 1 d . . . C23 C 0.6430(9) 0.8691(7) 0.1063(7) 0.044(3) Uani 1 1 d . . . C24 C 0.6938(9) 0.9166(8) 0.0462(7) 0.060(4) Uani 1 1 d . . . H24 H 0.6781 0.9809 0.0331 0.072 Uiso 1 1 calc R . . C25 C 0.7644(9) 0.8709(8) 0.0074(7) 0.054(4) Uani 1 1 d . . . H25 H 0.7958 0.9038 -0.0335 0.064 Uiso 1 1 calc R . . C26 C 0.7909(7) 0.7766(8) 0.0271(6) 0.041(3) Uani 1 1 d . . . C27 C 0.7438(7) 0.7274(7) 0.0841(6) 0.036(3) Uani 1 1 d . . . H27 H 0.7610 0.6630 0.0962 0.043 Uiso 1 1 calc R . . O2 O 0.5699(5) 0.9093(5) 0.1445(5) 0.056(2) Uani 1 1 d . . . H2 H 0.5602 0.9659 0.1283 0.084 Uiso 1 1 calc R . . Br2 Br 0.88800(9) 0.71396(9) -0.02657(7) 0.0590(4) Uani 1 1 d . . . C4 C 0.3490(7) 0.3657(7) 0.3169(5) 0.026(3) Uani 1 1 d . . . N41 N 0.3846(5) 0.2890(5) 0.2983(5) 0.036(2) Uani 1 1 d . . . H41N H 0.3546 0.2690 0.2683 0.043 Uiso 1 1 calc R . . N42 N 0.4727(5) 0.2424(5) 0.3294(5) 0.029(2) Uani 1 1 d . . . C41 C 0.5134(7) 0.1713(7) 0.3056(6) 0.032(3) Uani 1 1 d . . . H41 H 0.4822 0.1586 0.2669 0.039 Uiso 1 1 calc R . . C42 C 0.6053(7) 0.1085(7) 0.3350(6) 0.031(3) Uani 1 1 d . . . C43 C 0.6498(7) 0.1073(6) 0.4035(6) 0.028(3) Uani 1 1 d . . . C44 C 0.7333(6) 0.0402(6) 0.4269(6) 0.033(3) Uani 1 1 d . . . H44 H 0.7652 0.0391 0.4711 0.039 Uiso 1 1 calc R . . C45 C 0.7708(7) -0.0245(7) 0.3876(6) 0.033(3) Uani 1 1 d . . . H45 H 0.8274 -0.0700 0.4046 0.039 Uiso 1 1 calc R . . C46 C 0.7248(7) -0.0217(7) 0.3241(7) 0.038(3) Uani 1 1 d . . . C47 C 0.6432(7) 0.0424(6) 0.2957(6) 0.030(3) Uani 1 1 d . . . H47 H 0.6137 0.0417 0.2509 0.037 Uiso 1 1 calc R . . Br41 Br 0.77306(9) -0.11523(8) 0.27126(8) 0.0561(4) Uani 1 1 d . . . O41 O 0.6124(4) 0.1666(4) 0.4450(4) 0.0336(18) Uani 1 1 d . . . N61 N 0.3947(5) 0.4019(5) 0.3565(4) 0.024(2) Uani 1 1 d . . . N62 N 0.3315(5) 0.4805(5) 0.3673(4) 0.025(2) Uani 1 1 d . . . C61 C 0.2492(7) 0.4900(6) 0.3345(5) 0.023(2) Uani 1 1 d . . . C62 C 0.1679(6) 0.5683(6) 0.3253(6) 0.027(3) Uani 1 1 d . . . C63 C 0.1642(7) 0.6270(6) 0.3749(6) 0.025(3) Uani 1 1 d . . . C64 C 0.0853(7) 0.7010(6) 0.3671(6) 0.030(3) Uani 1 1 d . . . H64 H 0.0793 0.7396 0.4003 0.036 Uiso 1 1 calc R . . C65 C 0.0161(7) 0.7199(7) 0.3133(6) 0.038(3) Uani 1 1 d . . . H65 H -0.0358 0.7718 0.3087 0.045 Uiso 1 1 calc R . . C66 C 0.0222(7) 0.6630(7) 0.2656(6) 0.032(3) Uani 1 1 d . . . C67 C 0.0958(7) 0.5880(6) 0.2730(6) 0.030(3) Uani 1 1 d . . . H67 H 0.0976 0.5482 0.2414 0.036 Uiso 1 1 calc R . . Br6 Br -0.07044(8) 0.69374(8) 0.18803(7) 0.0471(3) Uani 1 1 d . . . O6 O 0.2307(4) 0.6126(4) 0.4247(4) 0.0282(17) Uani 1 1 d . . . N52 N 0.1837(7) 0.3920(6) 0.2715(6) 0.044(3) Uani 1 1 d D . . H52A H 0.187(7) 0.344(5) 0.313(4) 0.053 Uiso 1 1 d D . . H52B H 0.197(7) 0.420(6) 0.224(3) 0.053 Uiso 1 1 d D . . N51 N 0.2581(5) 0.4183(5) 0.3017(5) 0.031(2) Uani 1 1 d . . . S91 S 0.21508(19) 0.45542(19) 0.54898(17) 0.0397(8) Uani 1 1 d . . . O91 O 0.3108(4) 0.4740(4) 0.5532(4) 0.0340(18) Uani 1 1 d . . . C911 C 0.1326(7) 0.5433(7) 0.5794(6) 0.054(4) Uani 1 1 d . . . H91A H 0.1257 0.6001 0.5400 0.081 Uiso 1 1 calc R . . H91B H 0.1560 0.5504 0.6262 0.081 Uiso 1 1 calc R . . H91C H 0.0704 0.5280 0.5890 0.081 Uiso 1 1 calc R . . C912 C 0.2111(8) 0.3663(7) 0.6281(6) 0.051(3) Uani 1 1 d . . . H91D H 0.2543 0.3105 0.6204 0.076 Uiso 1 1 calc R . . H91E H 0.1457 0.3582 0.6352 0.076 Uiso 1 1 calc R . . H91F H 0.2310 0.3801 0.6731 0.076 Uiso 1 1 calc R . . S92 S 0.3999(2) 0.18207(19) 0.54764(18) 0.0425(8) Uani 1 1 d . . . O92 O 0.4328(4) 0.2652(4) 0.5039(4) 0.040(2) Uani 1 1 d . . . C922 C 0.4970(7) 0.1194(7) 0.6095(6) 0.051(3) Uani 1 1 d . . . H92A H 0.5010 0.1514 0.6483 0.076 Uiso 1 1 calc R . . H92B H 0.5567 0.1132 0.5804 0.076 Uiso 1 1 calc R . . H92C H 0.4870 0.0592 0.6340 0.076 Uiso 1 1 calc R . . C921 C 0.4101(8) 0.1090(6) 0.4858(6) 0.047(3) Uani 1 1 d . . . H92D H 0.3598 0.1347 0.4472 0.071 Uiso 1 1 calc R . . H92E H 0.4033 0.0492 0.5152 0.071 Uiso 1 1 calc R . . H92F H 0.4729 0.1029 0.4611 0.071 Uiso 1 1 calc R . . S81 S 0.1227(2) 0.2068(2) 0.4303(2) 0.0575(9) Uani 1 1 d . . . O81 O 0.2105(5) 0.2061(6) 0.3787(5) 0.065(3) Uani 1 1 d . . . C811 C 0.1212(9) 0.2910(9) 0.4774(8) 0.081(4) Uiso 1 1 d . . . H81A H 0.1734 0.2699 0.5144 0.121 Uiso 1 1 calc R . . H81B H 0.0600 0.3041 0.5037 0.121 Uiso 1 1 calc R . . H81C H 0.1294 0.3462 0.4405 0.121 Uiso 1 1 calc R . . C812 C 0.0215(8) 0.2679(8) 0.3707(7) 0.063(4) Uiso 1 1 d . . . H81D H 0.0099 0.2308 0.3382 0.094 Uiso 1 1 calc R . . H81E H 0.0341 0.3244 0.3390 0.094 Uiso 1 1 calc R . . H81F H -0.0350 0.2818 0.4022 0.094 Uiso 1 1 calc R . . S82 S 0.2797(2) 0.1461(2) 0.18225(19) 0.0522(9) Uani 1 1 d . . . O82 O 0.3104(6) 0.2261(5) 0.1953(5) 0.061(2) Uani 1 1 d . . . C821 C 0.1659(9) 0.1504(8) 0.2255(7) 0.076(4) Uiso 1 1 d . . . H82A H 0.1189 0.2021 0.1958 0.114 Uiso 1 1 calc R . . H82B H 0.1688 0.1573 0.2771 0.114 Uiso 1 1 calc R . . H82C H 0.1469 0.0943 0.2275 0.114 Uiso 1 1 calc R . . C822 C 0.3414(9) 0.0490(8) 0.2508(7) 0.074(4) Uiso 1 1 d . . . H82D H 0.4089 0.0333 0.2365 0.110 Uiso 1 1 calc R . . H82E H 0.3130 -0.0020 0.2529 0.110 Uiso 1 1 calc R . . H82F H 0.3362 0.0623 0.3006 0.110 Uiso 1 1 calc R . . S83 S 0.5592(2) 0.1568(2) 0.0669(2) 0.0622(10) Uani 1 1 d . . . O83 O 0.5327(6) 0.0854(5) 0.1302(5) 0.060(2) Uani 1 1 d . . . C831 C 0.4495(9) 0.2436(9) 0.0465(8) 0.084(5) Uiso 1 1 d . . . H83A H 0.4040 0.2221 0.0226 0.126 Uiso 1 1 calc R . . H83B H 0.4627 0.2984 0.0121 0.126 Uiso 1 1 calc R . . H83C H 0.4221 0.2575 0.0938 0.126 Uiso 1 1 calc R . . C832 C 0.6209(9) 0.2162(9) 0.1075(8) 0.085(5) Uiso 1 1 d . . . H83D H 0.6848 0.1783 0.1231 0.127 Uiso 1 1 calc R . . H83E H 0.5857 0.2315 0.1519 0.127 Uiso 1 1 calc R . . H83F H 0.6267 0.2719 0.0702 0.127 Uiso 1 1 calc R . . S84 S 0.4773(3) 0.5530(3) 0.1156(2) 0.0725(11) Uani 1 1 d . . . O84 O 0.4248(7) 0.6015(6) 0.0417(5) 0.087(3) Uani 1 1 d . . . C841 C 0.3960(9) 0.5737(8) 0.1897(7) 0.067(4) Uiso 1 1 d . . . H84A H 0.3830 0.6379 0.1898 0.100 Uiso 1 1 calc R . . H84B H 0.4239 0.5362 0.2385 0.100 Uiso 1 1 calc R . . H84C H 0.3361 0.5587 0.1818 0.100 Uiso 1 1 calc R . . C842 C 0.4853(9) 0.4348(8) 0.1294(8) 0.083(5) Uiso 1 1 d . . . H84D H 0.5293 0.4117 0.0919 0.124 Uiso 1 1 calc R . . H84E H 0.4219 0.4256 0.1232 0.124 Uiso 1 1 calc R . . H84F H 0.5092 0.4022 0.1806 0.124 Uiso 1 1 calc R . . S85 S 0.1769(2) 0.5196(2) 0.0486(2) 0.0635(10) Uani 1 1 d . . . O85 O 0.2220(6) 0.4916(6) 0.1261(5) 0.073(3) Uani 1 1 d . . . C851 C 0.1727(9) 0.6342(8) 0.0139(8) 0.079(4) Uiso 1 1 d . . . H85A H 0.1223 0.6695 0.0401 0.119 Uiso 1 1 calc R . . H85B H 0.1590 0.6524 -0.0406 0.119 Uiso 1 1 calc R . . H85C H 0.2345 0.6453 0.0225 0.119 Uiso 1 1 calc R . . C852 C 0.2720(9) 0.4817(9) -0.0092(8) 0.084(5) Uiso 1 1 d . . . H85D H 0.2868 0.4155 0.0018 0.126 Uiso 1 1 calc R . . H85E H 0.3284 0.5009 0.0010 0.126 Uiso 1 1 calc R . . H85F H 0.2538 0.5077 -0.0626 0.126 Uiso 1 1 calc R . . S86 S 0.2412(7) 0.8899(6) 0.1225(5) 0.107(4) Uiso 0.527(8) 1 d PD A 1 O86 O 0.2110(13) 0.9579(11) 0.1715(10) 0.098(7) Uiso 0.527(8) 1 d PD A 1 C861 C 0.211(3) 0.7885(15) 0.172(2) 0.135(7) Uiso 0.527(8) 1 d PD A 1 H86A H 0.2247 0.7768 0.2259 0.203 Uiso 0.527(8) 1 calc PR A 1 H86B H 0.2492 0.7383 0.1522 0.203 Uiso 0.527(8) 1 calc PR A 1 H86C H 0.1431 0.7940 0.1649 0.203 Uiso 0.527(8) 1 calc PR A 1 C862 C 0.205(3) 0.890(2) 0.0330(12) 0.135(7) Uiso 0.527(8) 1 d PD A 1 H86D H 0.2200 0.9414 -0.0050 0.203 Uiso 0.527(8) 1 calc PR A 1 H86E H 0.1354 0.8958 0.0334 0.203 Uiso 0.527(8) 1 calc PR A 1 H86F H 0.2379 0.8333 0.0204 0.203 Uiso 0.527(8) 1 calc PR A 1 S86' S 0.2751(6) 0.8115(5) 0.0889(5) 0.072(3) Uiso 0.473(8) 1 d PD A 2 O86' O 0.3504(14) 0.8540(13) 0.1196(11) 0.093(7) Uiso 0.473(8) 1 d PD A 2 C863 C 0.194(3) 0.780(3) 0.1603(19) 0.135(7) Uiso 0.473(8) 1 d PD A 2 H86G H 0.2284 0.7461 0.2073 0.203 Uiso 0.473(8) 1 calc PR A 2 H86H H 0.1579 0.7427 0.1446 0.203 Uiso 0.473(8) 1 calc PR A 2 H86I H 0.1489 0.8350 0.1689 0.203 Uiso 0.473(8) 1 calc PR A 2 C864 C 0.207(3) 0.860(2) 0.0055(15) 0.135(7) Uiso 0.473(8) 1 d PD A 2 H86J H 0.2490 0.8799 -0.0366 0.203 Uiso 0.473(8) 1 calc PR A 2 H86K H 0.1570 0.9120 0.0123 0.203 Uiso 0.473(8) 1 calc PR A 2 H86L H 0.1782 0.8147 -0.0058 0.203 Uiso 0.473(8) 1 calc PR A 2 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 Eu1 0.0091(2) 0.0100(3) 0.0162(3) -0.0044(2) 0.0002(2) -0.0013(2) Eu2 0.0122(3) 0.0114(3) 0.0189(3) -0.0051(2) 0.0006(2) -0.0029(2) O7 0.023(4) 0.018(3) 0.021(4) 0.003(3) 0.006(3) -0.006(3) C1 0.009(5) 0.022(6) 0.021(6) -0.008(5) 0.012(4) -0.005(4) N11 0.018(4) 0.027(5) 0.035(6) -0.014(4) 0.013(4) -0.004(4) N12 0.027(5) 0.014(4) 0.031(6) 0.000(4) 0.000(4) -0.002(4) C11 0.036(6) 0.029(6) 0.017(6) -0.007(5) 0.007(5) -0.004(5) C12 0.019(5) 0.024(6) 0.033(7) -0.014(5) 0.005(5) 0.000(5) C13 0.027(6) 0.012(5) 0.038(8) -0.005(5) -0.003(6) -0.010(5) C14 0.024(6) 0.027(6) 0.039(8) -0.013(6) -0.002(6) -0.010(5) C15 0.021(6) 0.027(6) 0.056(9) -0.012(6) 0.011(6) -0.003(5) C16 0.028(6) 0.018(6) 0.039(8) -0.014(6) 0.004(5) -0.001(5) C17 0.023(6) 0.032(6) 0.031(7) -0.006(5) 0.003(5) 0.001(5) O1 0.025(4) 0.023(4) 0.040(5) -0.009(4) 0.008(3) -0.008(3) Br1 0.0299(6) 0.0394(7) 0.0621(9) -0.0149(7) -0.0021(6) 0.0055(5) N31 0.019(4) 0.021(5) 0.039(6) -0.012(5) 0.003(4) -0.001(4) N32 0.019(4) 0.020(4) 0.019(5) -0.008(4) -0.001(4) 0.010(4) C31 0.021(5) 0.021(6) 0.032(7) -0.002(5) 0.010(5) -0.008(5) C32 0.022(5) 0.024(6) 0.019(6) -0.003(5) -0.003(5) 0.000(5) C33 0.028(6) 0.026(6) 0.032(7) -0.001(6) -0.002(5) -0.007(5) C34 0.037(7) 0.022(6) 0.055(9) -0.016(6) 0.012(6) 0.000(5) C35 0.038(7) 0.038(7) 0.036(8) -0.013(6) -0.001(6) 0.008(6) C36 0.028(6) 0.036(7) 0.049(8) -0.013(6) -0.001(6) -0.009(5) C37 0.023(5) 0.025(6) 0.025(7) -0.002(5) -0.005(5) -0.004(5) O3 0.040(4) 0.025(4) 0.042(5) -0.011(4) 0.010(4) -0.017(3) Br3 0.0310(6) 0.0508(7) 0.0616(9) -0.0233(7) 0.0170(6) -0.0128(6) N21 0.031(5) 0.016(5) 0.027(5) -0.003(4) 0.003(4) -0.008(4) N22 0.040(5) 0.021(5) 0.028(6) -0.002(4) 0.005(4) -0.010(4) C21 0.029(6) 0.037(7) 0.033(7) -0.010(6) 0.010(5) -0.009(5) C22 0.038(7) 0.037(7) 0.021(7) -0.006(6) 0.014(5) -0.014(5) C23 0.064(9) 0.026(7) 0.039(8) -0.001(6) 0.006(7) -0.016(6) C24 0.078(10) 0.040(8) 0.060(10) -0.014(8) -0.002(8) -0.009(7) C25 0.067(9) 0.039(8) 0.050(9) -0.013(7) 0.024(7) -0.009(7) C26 0.038(7) 0.048(8) 0.042(8) -0.020(7) 0.003(6) -0.010(6) C27 0.029(6) 0.038(7) 0.043(8) -0.011(6) 0.010(6) -0.013(5) O2 0.063(6) 0.034(5) 0.072(7) -0.019(5) 0.029(5) -0.014(4) Br2 0.0510(8) 0.0641(9) 0.0512(9) -0.0091(8) 0.0173(7) -0.0046(7) C4 0.024(6) 0.040(7) 0.015(6) -0.005(5) 0.000(5) -0.015(5) N41 0.026(5) 0.023(5) 0.060(7) -0.028(5) -0.018(5) 0.013(4) N42 0.025(5) 0.028(5) 0.032(6) -0.012(5) -0.002(4) -0.001(4) C41 0.025(6) 0.032(6) 0.038(8) -0.006(6) -0.012(5) -0.004(5) C42 0.025(6) 0.030(6) 0.041(8) -0.019(6) 0.001(5) -0.004(5) C43 0.026(6) 0.019(6) 0.036(7) 0.005(5) -0.004(5) -0.011(5) C44 0.024(6) 0.023(6) 0.053(8) 0.000(6) -0.004(6) -0.017(5) C45 0.017(5) 0.028(6) 0.055(8) -0.020(6) 0.002(6) 0.001(5) C46 0.029(6) 0.034(7) 0.052(9) -0.023(6) 0.015(6) -0.003(5) C47 0.030(6) 0.029(6) 0.036(7) -0.018(6) -0.003(5) -0.004(5) Br41 0.0440(8) 0.0496(8) 0.0723(11) -0.0305(8) 0.0008(7) 0.0085(6) O41 0.030(4) 0.039(4) 0.038(5) -0.013(4) 0.001(4) -0.014(3) N61 0.024(5) 0.030(5) 0.021(5) -0.017(4) 0.003(4) -0.004(4) N62 0.024(5) 0.025(5) 0.027(5) -0.003(4) -0.008(4) -0.009(4) C61 0.033(6) 0.017(5) 0.020(6) -0.002(5) 0.001(5) -0.008(5) C62 0.023(6) 0.018(5) 0.038(7) -0.004(5) -0.004(5) 0.000(5) C63 0.018(6) 0.021(6) 0.031(7) -0.001(5) 0.000(5) -0.005(5) C64 0.036(6) 0.024(6) 0.029(7) -0.012(5) -0.006(5) 0.003(5) C65 0.025(6) 0.047(7) 0.044(8) -0.022(6) -0.006(6) -0.003(5) C66 0.023(6) 0.032(6) 0.042(8) -0.016(6) -0.004(5) -0.003(5) C67 0.034(6) 0.029(6) 0.028(7) -0.007(5) -0.002(5) -0.010(5) Br6 0.0381(7) 0.0454(7) 0.0564(9) -0.0202(7) -0.0206(6) 0.0055(6) O6 0.025(4) 0.027(4) 0.034(5) -0.014(4) -0.002(3) -0.004(3) N52 0.034(5) 0.045(7) 0.057(8) -0.015(6) -0.017(6) -0.011(5) N51 0.024(5) 0.027(5) 0.038(6) -0.016(5) -0.001(4) 0.008(4) S91 0.0299(16) 0.0506(19) 0.043(2) -0.0129(16) 0.0033(14) -0.0181(14) O91 0.022(4) 0.040(4) 0.040(5) -0.005(4) -0.003(3) -0.012(3) C911 0.019(6) 0.081(9) 0.056(9) -0.022(8) 0.016(6) -0.002(6) C912 0.044(7) 0.070(9) 0.041(8) -0.002(7) 0.009(6) -0.032(6) S92 0.0370(17) 0.0356(17) 0.054(2) -0.0048(16) 0.0062(16) -0.0160(14) O92 0.035(4) 0.028(4) 0.058(6) -0.008(4) 0.018(4) -0.017(3) C922 0.042(7) 0.050(7) 0.058(9) 0.001(7) -0.011(6) -0.019(6) C921 0.059(8) 0.027(6) 0.051(8) -0.007(6) 0.015(7) -0.010(6) S81 0.050(2) 0.067(2) 0.057(2) -0.015(2) -0.0024(18) -0.0163(18) O81 0.039(5) 0.095(7) 0.065(6) -0.031(5) 0.006(5) -0.016(5) S82 0.055(2) 0.055(2) 0.054(2) -0.0182(18) -0.0041(18) -0.0221(17) O82 0.071(6) 0.050(5) 0.076(7) -0.028(5) -0.020(5) -0.019(4) S83 0.072(2) 0.051(2) 0.058(3) -0.005(2) -0.002(2) -0.0125(19) O83 0.084(6) 0.035(5) 0.059(6) 0.005(5) -0.007(5) -0.028(4) S84 0.082(3) 0.085(3) 0.051(3) 0.003(2) -0.001(2) -0.043(2) O84 0.108(8) 0.108(8) 0.039(6) 0.008(6) -0.017(6) -0.040(6) S85 0.064(2) 0.071(2) 0.060(3) -0.019(2) -0.002(2) -0.0233(19) O85 0.078(6) 0.097(7) 0.054(6) -0.017(5) -0.010(5) -0.038(5) _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 Eu1 O6 2.205(6) . ? Eu1 O7 2.335(6) 2_666 ? Eu1 O1 2.352(6) . ? Eu1 O91 2.391(7) . ? Eu1 N31 2.393(8) . ? Eu1 N62 2.490(8) . ? Eu1 N12 2.508(7) . ? Eu1 C1 3.269(9) . ? Eu1 S91 3.461(3) . ? Eu1 Eu1 3.7248(9) 2_666 ? Eu1 Eu2 3.7944(7) 2_666 ? Eu1 Eu2 4.1873(6) . ? Eu2 O3 2.194(7) . ? Eu2 O41 2.246(7) . ? Eu2 O1 2.284(6) 2_666 ? Eu2 O7 2.349(6) . ? Eu2 O92 2.404(6) . ? Eu2 N61 2.429(7) . ? Eu2 N32 2.498(8) . ? Eu2 N42 2.593(8) . ? Eu2 Eu1 3.7944(7) 2_666 ? O7 H7 0.8400 . ? C1 N31 1.308(11) . ? C1 N11 1.326(10) . ? C1 N21 1.374(10) . ? N11 N12 1.399(10) . ? N12 C11 1.303(10) . ? C11 C12 1.450(12) . ? C11 H11 0.9500 . ? C12 C17 1.421(12) . ? C12 C13 1.425(13) . ? C13 C14 1.365(13) . ? C13 O1 1.387(10) . ? C14 C15 1.369(12) . ? C14 H14 0.9500 . ? C15 C16 1.386(13) . ? C15 H15 0.9500 . ? C16 C17 1.345(12) . ? C16 Br1 1.905(9) . ? C17 H17 0.9500 . ? O1 Eu2 2.284(6) 2_666 ? N31 N32 1.409(9) . ? N32 C31 1.319(11) . ? C31 N21 1.356(11) . ? C31 C32 1.465(12) . ? C32 C37 1.399(12) . ? C32 C33 1.448(12) . ? C33 O3 1.302(11) . ? C33 C34 1.408(13) . ? C34 C35 1.381(13) . ? C34 H34 0.9500 . ? C35 C36 1.408(13) . ? C35 H35 0.9500 . ? C36 C37 1.378(12) . ? C36 Br3 1.892(10) . ? C37 H37 0.9500 . ? N21 N22 1.388(10) . ? N22 C21 1.282(11) . ? C21 C22 1.472(13) . ? C21 H21 0.9500 . ? C22 C27 1.408(13) . ? C22 C23 1.414(13) . ? C23 O2 1.343(12) . ? C23 C24 1.430(15) . ? C24 C25 1.366(14) . ? C24 H24 0.9500 . ? C25 C26 1.391(14) . ? C25 H25 0.9500 . ? C26 C27 1.378(13) . ? C26 Br2 1.880(11) . ? C27 H27 0.9500 . ? O2 H2 0.8400 . ? C4 N41 1.310(11) . ? C4 N61 1.321(11) . ? C4 N51 1.368(11) . ? N41 N42 1.376(9) . ? N41 H41N 0.8800 . ? N42 C41 1.295(11) . ? C41 C42 1.480(12) . ? C41 H41 0.9500 . ? C42 C47 1.397(12) . ? C42 C43 1.436(13) . ? C43 O41 1.341(11) . ? C43 C44 1.397(12) . ? C44 C45 1.377(13) . ? C44 H44 0.9500 . ? C45 C46 1.358(13) . ? C45 H45 0.9500 . ? C46 C47 1.375(12) . ? C46 Br41 1.929(10) . ? C47 H47 0.9500 . ? N61 N62 1.395(9) . ? N62 C61 1.324(11) . ? C61 N51 1.383(11) . ? C61 C62 1.457(12) . ? C62 C67 1.381(12) . ? C62 C63 1.442(13) . ? C63 O6 1.303(10) . ? C63 C64 1.396(12) . ? C64 C65 1.370(12) . ? C64 H64 0.9500 . ? C65 C66 1.387(13) . ? C65 H65 0.9500 . ? C66 C67 1.360(12) . ? C66 Br6 1.897(10) . ? C67 H67 0.9500 . ? N52 N51 1.431(11) . ? N52 H52A 0.91(2) . ? N52 H52B 0.90(2) . ? S91 O91 1.492(6) . ? S91 C912 1.743(10) . ? S91 C911 1.770(10) . ? C911 H91A 0.9800 . ? C911 H91B 0.9800 . ? C911 H91C 0.9800 . ? C912 H91D 0.9800 . ? C912 H91E 0.9800 . ? C912 H91F 0.9800 . ? S92 O92 1.515(7) . ? S92 C922 1.776(10) . ? S92 C921 1.785(10) . ? C922 H92A 0.9800 . ? C922 H92B 0.9800 . ? C922 H92C 0.9800 . ? C921 H92D 0.9800 . ? C921 H92E 0.9800 . ? C921 H92F 0.9800 . ? S81 O81 1.530(8) . ? S81 C811 1.753(13) . ? S81 C812 1.791(11) . ? C811 H81A 0.9800 . ? C811 H81B 0.9800 . ? C811 H81C 0.9800 . ? C812 H81D 0.9800 . ? C812 H81E 0.9800 . ? C812 H81F 0.9800 . ? S82 O82 1.512(8) . ? S82 C821 1.771(12) . ? S82 C822 1.780(12) . ? C821 H82A 0.9800 . ? C821 H82B 0.9800 . ? C821 H82C 0.9800 . ? C822 H82D 0.9800 . ? C822 H82E 0.9800 . ? C822 H82F 0.9800 . ? S83 O83 1.492(8) . ? S83 C832 1.754(13) . ? S83 C831 1.803(12) . ? C831 H83A 0.9800 . ? C831 H83B 0.9800 . ? C831 H83C 0.9800 . ? C832 H83D 0.9800 . ? C832 H83E 0.9800 . ? C832 H83F 0.9800 . ? S84 O84 1.513(8) . ? S84 C841 1.775(12) . ? S84 C842 1.787(13) . ? C841 H84A 0.9800 . ? C841 H84B 0.9800 . ? C841 H84C 0.9800 . ? C842 H84D 0.9800 . ? C842 H84E 0.9800 . ? C842 H84F 0.9800 . ? S85 O85 1.507(8) . ? S85 C851 1.737(12) . ? S85 C852 1.757(13) . ? C851 H85A 0.9800 . ? C851 H85B 0.9800 . ? C851 H85C 0.9800 . ? C852 H85D 0.9800 . ? C852 H85E 0.9800 . ? C852 H85F 0.9800 . ? S86 O86 1.534(16) . ? S86 C862 1.749(5) . ? S86 C861 1.759(5) . ? C861 H86A 0.9800 . ? C861 H86B 0.9800 . ? C861 H86C 0.9800 . ? C862 H86D 0.9800 . ? C862 H86E 0.9800 . ? C862 H86F 0.9800 . ? S86' O86' 1.607(17) . ? S86' C864 1.753(5) . ? S86' C863 1.756(5) . ? C863 H86G 0.9800 . ? C863 H86H 0.9800 . ? C863 H86I 0.9800 . ? C864 H86J 0.9800 . ? C864 H86K 0.9800 . ? C864 H86L 0.9800 . ? 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 O6 Eu1 O7 145.1(2) . 2_666 ? O6 Eu1 O1 75.8(2) . . ? O7 Eu1 O1 69.3(2) 2_666 . ? O6 Eu1 O91 76.1(2) . . ? O7 Eu1 O91 101.5(2) 2_666 . ? O1 Eu1 O91 88.8(2) . . ? O6 Eu1 N31 123.9(2) . . ? O7 Eu1 N31 80.1(2) 2_666 . ? O1 Eu1 N31 126.4(2) . . ? O91 Eu1 N31 141.2(2) . . ? O6 Eu1 N62 68.1(2) . . ? O7 Eu1 N62 146.8(2) 2_666 . ? O1 Eu1 N62 143.6(2) . . ? O91 Eu1 N62 87.1(2) . . ? N31 Eu1 N62 73.7(3) . . ? O6 Eu1 N12 85.7(2) . . ? O7 Eu1 N12 84.6(2) 2_666 . ? O1 Eu1 N12 71.6(2) . . ? O91 Eu1 N12 156.1(2) . . ? N31 Eu1 N12 62.4(3) . . ? N62 Eu1 N12 100.4(2) . . ? O6 Eu1 C1 114.8(2) . . ? O7 Eu1 C1 78.5(2) 2_666 . ? O1 Eu1 C1 108.4(2) . . ? O91 Eu1 C1 161.2(2) . . ? N31 Eu1 C1 20.0(2) . . ? N62 Eu1 C1 83.4(2) . . ? N12 Eu1 C1 42.5(2) . . ? O6 Eu1 S91 57.43(17) . . ? O7 Eu1 S91 121.86(15) 2_666 . ? O1 Eu1 S91 92.56(16) . . ? O91 Eu1 S91 20.83(15) . . ? N31 Eu1 S91 140.98(19) . . ? N62 Eu1 S91 72.25(19) . . ? N12 Eu1 S91 142.82(18) . . ? C1 Eu1 S91 155.60(17) . . ? O6 Eu1 Eu1 162.09(17) . 2_666 ? O7 Eu1 Eu1 36.72(13) 2_666 2_666 ? O1 Eu1 Eu1 102.04(15) . 2_666 ? O91 Eu1 Eu1 86.15(14) . 2_666 ? N31 Eu1 Eu1 72.04(18) . 2_666 ? N62 Eu1 Eu1 113.76(17) . 2_666 ? N12 Eu1 Eu1 110.71(17) . 2_666 ? C1 Eu1 Eu1 82.86(15) . 2_666 ? S91 Eu1 Eu1 105.36(5) . 2_666 ? O6 Eu1 Eu2 109.33(16) . 2_666 ? O7 Eu1 Eu2 36.01(14) 2_666 2_666 ? O1 Eu1 Eu2 34.49(15) . 2_666 ? O91 Eu1 Eu2 89.30(16) . 2_666 ? N31 Eu1 Eu2 110.22(18) . 2_666 ? N62 Eu1 Eu2 176.05(18) . 2_666 ? N12 Eu1 Eu2 82.20(18) . 2_666 ? C1 Eu1 Eu2 100.49(16) . 2_666 ? S91 Eu1 Eu2 103.88(5) . 2_666 ? Eu1 Eu1 Eu2 67.673(15) 2_666 2_666 ? O6 Eu1 Eu2 123.12(16) . . ? O7 Eu1 Eu2 91.14(13) 2_666 . ? O1 Eu1 Eu2 158.83(15) . . ? O91 Eu1 Eu2 87.21(15) . . ? N31 Eu1 Eu2 54.02(18) . . ? N62 Eu1 Eu2 56.94(17) . . ? N12 Eu1 Eu2 115.94(18) . . ? C1 Eu1 Eu2 74.01(16) . . ? S91 Eu1 Eu2 91.04(5) . . ? Eu1 Eu1 Eu2 56.955(13) 2_666 . ? Eu2 Eu1 Eu2 124.628(13) 2_666 . ? O3 Eu2 O41 80.8(2) . . ? O3 Eu2 O1 96.2(2) . 2_666 ? O41 Eu2 O1 82.0(2) . 2_666 ? O3 Eu2 O7 139.1(2) . . ? O41 Eu2 O7 131.8(2) . . ? O1 Eu2 O7 70.2(2) 2_666 . ? O3 Eu2 O92 151.9(2) . . ? O41 Eu2 O92 79.1(2) . . ? O1 Eu2 O92 100.3(2) 2_666 . ? O7 Eu2 O92 68.5(2) . . ? O3 Eu2 N61 103.2(2) . . ? O41 Eu2 N61 130.0(2) . . ? O1 Eu2 N61 144.5(2) 2_666 . ? O7 Eu2 N61 75.7(2) . . ? O92 Eu2 N61 75.6(2) . . ? O3 Eu2 N32 68.9(2) . . ? O41 Eu2 N32 145.5(2) . . ? O1 Eu2 N32 85.2(2) 2_666 . ? O7 Eu2 N32 71.6(2) . . ? O92 Eu2 N32 134.8(2) . . ? N61 Eu2 N32 74.7(2) . . ? O3 Eu2 N42 72.5(2) . . ? O41 Eu2 N42 71.1(2) . . ? O1 Eu2 N42 152.0(2) 2_666 . ? O7 Eu2 N42 134.6(2) . . ? O92 Eu2 N42 82.5(2) . . ? N61 Eu2 N42 63.4(2) . . ? N32 Eu2 N42 112.7(2) . . ? O3 Eu2 Eu1 116.51(17) . 2_666 ? O41 Eu2 Eu1 113.37(17) . 2_666 ? O1 Eu2 Eu1 35.67(15) 2_666 2_666 ? O7 Eu2 Eu1 35.76(14) . 2_666 ? O92 Eu2 Eu1 89.61(17) . 2_666 ? N61 Eu2 Eu1 108.92(18) . 2_666 ? N32 Eu2 Eu1 69.09(17) . 2_666 ? N42 Eu2 Eu1 170.08(18) . 2_666 ? O3 Eu2 Eu1 123.81(16) . . ? O41 Eu2 Eu1 155.15(18) . . ? O1 Eu2 Eu1 90.94(15) 2_666 . ? O7 Eu2 Eu1 26.08(13) . . ? O92 Eu2 Eu1 78.74(15) . . ? N61 Eu2 Eu1 53.57(18) . . ? N32 Eu2 Eu1 56.24(17) . . ? N42 Eu2 Eu1 116.78(17) . . ? Eu1 Eu2 Eu1 55.372(13) 2_666 . ? Eu2 O7 H7 109.5 . . ? N31 C1 N11 125.5(8) . . ? N31 C1 N21 108.5(8) . . ? N11 C1 N21 126.1(9) . . ? N31 C1 Eu1 38.7(4) . . ? N11 C1 Eu1 87.0(5) . . ? N21 C1 Eu1 146.8(6) . . ? C1 N11 N12 108.3(8) . . ? C11 N12 N11 113.4(8) . . ? C11 N12 Eu1 124.2(7) . . ? N11 N12 Eu1 122.2(5) . . ? N12 C11 C12 124.8(9) . . ? N12 C11 H11 117.6 . . ? C12 C11 H11 117.6 . . ? C17 C12 C13 116.2(9) . . ? C17 C12 C11 117.8(9) . . ? C13 C12 C11 125.9(9) . . ? C14 C13 O1 120.6(10) . . ? C14 C13 C12 120.6(9) . . ? O1 C13 C12 118.7(9) . . ? C13 C14 C15 121.3(11) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C16 119.3(10) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C17 C16 C15 120.9(9) . . ? C17 C16 Br1 119.2(8) . . ? C15 C16 Br1 119.9(8) . . ? C16 C17 C12 121.6(10) . . ? C16 C17 H17 119.2 . . ? C12 C17 H17 119.2 . . ? C13 O1 Eu2 126.6(5) . 2_666 ? C13 O1 Eu1 121.0(6) . . ? Eu2 O1 Eu1 109.8(2) 2_666 . ? C1 N31 N32 107.4(7) . . ? C1 N31 Eu1 121.3(6) . . ? N32 N31 Eu1 131.1(6) . . ? C31 N32 N31 108.1(8) . . ? C31 N32 Eu2 133.7(6) . . ? N31 N32 Eu2 117.6(6) . . ? N32 C31 N21 107.9(8) . . ? N32 C31 C32 123.5(8) . . ? N21 C31 C32 128.5(9) . . ? C37 C32 C33 119.9(9) . . ? C37 C32 C31 121.9(9) . . ? C33 C32 C31 118.2(9) . . ? O3 C33 C34 119.3(9) . . ? O3 C33 C32 122.7(9) . . ? C34 C33 C32 118.0(9) . . ? C35 C34 C33 120.7(10) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C36 120.5(10) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C37 C36 C35 120.6(10) . . ? C37 C36 Br3 121.0(8) . . ? C35 C36 Br3 118.4(8) . . ? C36 C37 C32 120.2(9) . . ? C36 C37 H37 119.9 . . ? C32 C37 H37 119.9 . . ? C33 O3 Eu2 141.4(7) . . ? C31 N21 C1 108.1(8) . . ? C31 N21 N22 121.1(8) . . ? C1 N21 N22 130.5(7) . . ? C21 N22 N21 118.3(8) . . ? N22 C21 C22 119.0(9) . . ? N22 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? C27 C22 C23 120.9(10) . . ? C27 C22 C21 120.0(9) . . ? C23 C22 C21 119.1(10) . . ? O2 C23 C22 118.5(10) . . ? O2 C23 C24 124.3(10) . . ? C22 C23 C24 117.2(11) . . ? C25 C24 C23 121.1(11) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 120.6(12) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C27 C26 C25 120.7(10) . . ? C27 C26 Br2 118.7(8) . . ? C25 C26 Br2 120.5(9) . . ? C26 C27 C22 119.4(10) . . ? C26 C27 H27 120.3 . . ? C22 C27 H27 120.3 . . ? C23 O2 H2 109.5 . . ? N41 C4 N61 124.7(9) . . ? N41 C4 N51 125.7(9) . . ? N61 C4 N51 109.5(9) . . ? C4 N41 N42 114.5(8) . . ? C4 N41 H41N 122.7 . . ? N42 N41 H41N 122.7 . . ? C41 N42 N41 115.4(8) . . ? C41 N42 Eu2 127.0(6) . . ? N41 N42 Eu2 117.1(6) . . ? N42 C41 C42 124.1(9) . . ? N42 C41 H41 117.9 . . ? C42 C41 H41 117.9 . . ? C47 C42 C43 120.4(9) . . ? C47 C42 C41 115.4(9) . . ? C43 C42 C41 123.9(9) . . ? O41 C43 C44 120.6(10) . . ? O41 C43 C42 122.0(8) . . ? C44 C43 C42 117.4(10) . . ? C45 C44 C43 122.0(10) . . ? C45 C44 H44 119.0 . . ? C43 C44 H44 119.0 . . ? C46 C45 C44 118.4(9) . . ? C46 C45 H45 120.8 . . ? C44 C45 H45 120.8 . . ? C45 C46 C47 124.2(10) . . ? C45 C46 Br41 118.8(8) . . ? C47 C46 Br41 117.0(9) . . ? C46 C47 C42 117.6(10) . . ? C46 C47 H47 121.2 . . ? C42 C47 H47 121.2 . . ? C43 O41 Eu2 132.6(6) . . ? C4 N61 N62 107.2(7) . . ? C4 N61 Eu2 120.0(6) . . ? N62 N61 Eu2 131.7(5) . . ? C61 N62 N61 108.5(7) . . ? C61 N62 Eu1 133.6(6) . . ? N61 N62 Eu1 117.5(5) . . ? N62 C61 N51 108.1(8) . . ? N62 C61 C62 125.9(9) . . ? N51 C61 C62 125.5(9) . . ? C67 C62 C63 119.5(8) . . ? C67 C62 C61 123.8(9) . . ? C63 C62 C61 116.7(9) . . ? O6 C63 C64 121.1(9) . . ? O6 C63 C62 122.3(8) . . ? C64 C63 C62 116.6(9) . . ? C65 C64 C63 122.4(10) . . ? C65 C64 H64 118.8 . . ? C63 C64 H64 118.8 . . ? C64 C65 C66 119.6(9) . . ? C64 C65 H65 120.2 . . ? C66 C65 H65 120.2 . . ? C67 C66 C65 120.1(9) . . ? C67 C66 Br6 120.8(8) . . ? C65 C66 Br6 119.0(7) . . ? C66 C67 C62 121.6(10) . . ? C66 C67 H67 119.2 . . ? C62 C67 H67 119.2 . . ? C63 O6 Eu1 145.6(6) . . ? N51 N52 H52A 90(7) . . ? N51 N52 H52B 92(7) . . ? H52A N52 H52B 156(9) . . ? C4 N51 C61 106.6(8) . . ? C4 N51 N52 124.5(8) . . ? C61 N51 N52 127.7(8) . . ? O91 S91 C912 104.6(5) . . ? O91 S91 C911 105.3(5) . . ? C912 S91 C911 98.8(5) . . ? O91 S91 Eu1 34.7(3) . . ? C912 S91 Eu1 137.7(4) . . ? C911 S91 Eu1 103.5(4) . . ? S91 O91 Eu1 124.4(4) . . ? S91 C911 H91A 109.5 . . ? S91 C911 H91B 109.5 . . ? H91A C911 H91B 109.5 . . ? S91 C911 H91C 109.5 . . ? H91A C911 H91C 109.5 . . ? H91B C911 H91C 109.5 . . ? S91 C912 H91D 109.5 . . ? S91 C912 H91E 109.5 . . ? H91D C912 H91E 109.5 . . ? S91 C912 H91F 109.5 . . ? H91D C912 H91F 109.5 . . ? H91E C912 H91F 109.5 . . ? O92 S92 C922 103.7(5) . . ? O92 S92 C921 107.4(5) . . ? C922 S92 C921 99.3(5) . . ? S92 O92 Eu2 144.0(4) . . ? S92 C922 H92A 109.5 . . ? S92 C922 H92B 109.5 . . ? H92A C922 H92B 109.5 . . ? S92 C922 H92C 109.5 . . ? H92A C922 H92C 109.5 . . ? H92B C922 H92C 109.5 . . ? S92 C921 H92D 109.5 . . ? S92 C921 H92E 109.5 . . ? H92D C921 H92E 109.5 . . ? S92 C921 H92F 109.5 . . ? H92D C921 H92F 109.5 . . ? H92E C921 H92F 109.5 . . ? O81 S81 C811 104.9(6) . . ? O81 S81 C812 106.1(5) . . ? C811 S81 C812 96.5(6) . . ? S81 C811 H81A 109.5 . . ? S81 C811 H81B 109.5 . . ? H81A C811 H81B 109.5 . . ? S81 C811 H81C 109.5 . . ? H81A C811 H81C 109.5 . . ? H81B C811 H81C 109.5 . . ? S81 C812 H81D 109.5 . . ? S81 C812 H81E 109.5 . . ? H81D C812 H81E 109.5 . . ? S81 C812 H81F 109.5 . . ? H81D C812 H81F 109.5 . . ? H81E C812 H81F 109.5 . . ? O82 S82 C821 105.2(5) . . ? O82 S82 C822 106.3(5) . . ? C821 S82 C822 95.8(6) . . ? S82 C821 H82A 109.5 . . ? S82 C821 H82B 109.5 . . ? H82A C821 H82B 109.5 . . ? S82 C821 H82C 109.5 . . ? H82A C821 H82C 109.5 . . ? H82B C821 H82C 109.5 . . ? S82 C822 H82D 109.5 . . ? S82 C822 H82E 109.5 . . ? H82D C822 H82E 109.5 . . ? S82 C822 H82F 109.5 . . ? H82D C822 H82F 109.5 . . ? H82E C822 H82F 109.5 . . ? O83 S83 C832 106.9(6) . . ? O83 S83 C831 103.7(6) . . ? C832 S83 C831 97.3(6) . . ? S83 C831 H83A 109.5 . . ? S83 C831 H83B 109.5 . . ? H83A C831 H83B 109.5 . . ? S83 C831 H83C 109.5 . . ? H83A C831 H83C 109.5 . . ? H83B C831 H83C 109.5 . . ? S83 C832 H83D 109.5 . . ? S83 C832 H83E 109.5 . . ? H83D C832 H83E 109.5 . . ? S83 C832 H83F 109.5 . . ? H83D C832 H83F 109.5 . . ? H83E C832 H83F 109.5 . . ? O84 S84 C841 106.9(6) . . ? O84 S84 C842 107.1(6) . . ? C841 S84 C842 98.9(6) . . ? S84 C841 H84A 109.5 . . ? S84 C841 H84B 109.5 . . ? H84A C841 H84B 109.5 . . ? S84 C841 H84C 109.5 . . ? H84A C841 H84C 109.5 . . ? H84B C841 H84C 109.5 . . ? S84 C842 H84D 109.5 . . ? S84 C842 H84E 109.5 . . ? H84D C842 H84E 109.5 . . ? S84 C842 H84F 109.5 . . ? H84D C842 H84F 109.5 . . ? H84E C842 H84F 109.5 . . ? O85 S85 C851 106.2(6) . . ? O85 S85 C852 103.1(6) . . ? C851 S85 C852 95.8(7) . . ? S85 C851 H85A 109.5 . . ? S85 C851 H85B 109.5 . . ? H85A C851 H85B 109.5 . . ? S85 C851 H85C 109.5 . . ? H85A C851 H85C 109.5 . . ? H85B C851 H85C 109.5 . . ? S85 C852 H85D 109.5 . . ? S85 C852 H85E 109.5 . . ? H85D C852 H85E 109.5 . . ? S85 C852 H85F 109.5 . . ? H85D C852 H85F 109.5 . . ? H85E C852 H85F 109.5 . . ? O86 S86 C862 132.3(13) . . ? O86 S86 C861 107.8(13) . . ? C862 S86 C861 96(2) . . ? S86 C861 H86A 109.5 . . ? S86 C861 H86B 109.5 . . ? H86A C861 H86B 109.5 . . ? S86 C861 H86C 109.5 . . ? H86A C861 H86C 109.5 . . ? H86B C861 H86C 109.5 . . ? S86 C862 H86D 109.5 . . ? S86 C862 H86E 109.5 . . ? H86D C862 H86E 109.5 . . ? S86 C862 H86F 109.5 . . ? H86D C862 H86F 109.5 . . ? H86E C862 H86F 109.5 . . ? O86' S86' C864 126.1(15) . . ? O86' S86' C863 110.8(14) . . ? C864 S86' C863 106(2) . . ? S86' C863 H86G 109.5 . . ? S86' C863 H86H 109.5 . . ? H86G C863 H86H 109.5 . . ? S86' C863 H86I 109.5 . . ? H86G C863 H86I 109.5 . . ? H86H C863 H86I 109.5 . . ? S86' C864 H86J 109.5 . . ? S86' C864 H86K 109.5 . . ? H86J C864 H86K 109.5 . . ? S86' C864 H86L 109.5 . . ? H86J C864 H86L 109.5 . . ? H86K C864 H86L 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.320 _refine_diff_density_min -1.077 _refine_diff_density_rms 0.160 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 226 73 ' ' 2 0.014 0.536 0.458 7 1 ' ' 3 0.984 0.460 0.547 6 1 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 942794' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6 # begin Validation Reply Form _vrf_CHEMW03_6 ; PROBLEM: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.90 <> 1.10 RESPONSE: Our structure model contains disordered DMSO molecules which could not be refined satisfactorily. After application of SQUEEZE routine, the molecular weight differs from the calculated one. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common " [ [{{Gd(DMSO)}2(HBr3L')(H3Br2L'')}2({mu-}OH)2 ]~18 DMSO " _chemical_melting_point ? _chemical_formula_moiety 'C41 H35 Br5 Gd2 N12 O8 S2' _chemical_formula_sum 'C110 H142 Br10 Gd4 N24 O30 S18' _chemical_formula_weight 4285.66 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.5406(5) _cell_length_b 15.8933(6) _cell_length_c 18.2622(7) _cell_angle_alpha 73.997(3) _cell_angle_beta 85.829(3) _cell_angle_gamma 74.383(3) _cell_volume 3907.0(2) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6117 _cell_measurement_theta_min 2.7352 _cell_measurement_theta_max 28.3617 _exptl_crystal_description plate _exptl_crystal_colour dark-orange _exptl_crystal_size_max 0.095 _exptl_crystal_size_mid 0.038 _exptl_crystal_size_min 0.014 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 4.545 _exptl_absorpt_correction_T_min 0.79147 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '974 images at 1.0 deg in \w and 45 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51426 _diffrn_reflns_av_R_equivalents 0.0968 _diffrn_reflns_av_sigmaI/netI 0.2638 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13743 _reflns_number_gt 5872 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.32.24 Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.32.24 Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.32.24 Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0228P)^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 13743 _refine_ls_number_parameters 640 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.0961 _refine_ls_wR_factor_gt 0.0919 _refine_ls_goodness_of_fit_ref 0.805 _refine_ls_restrained_S_all 0.806 _refine_ls_shift/su_max 0.006 _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 Gd1 Gd 0.12024(4) 0.93655(4) 0.04813(3) 0.02141(16) Uani 1 1 d . . . Gd2 Gd 0.04864(4) 0.81370(4) -0.08556(3) 0.02176(17) Uani 1 1 d . . . C1 C -0.0228(8) 0.8825(7) 0.1947(6) 0.024(3) Uani 1 1 d . . . N11 N 0.0296(6) 0.7968(6) 0.2050(4) 0.025(2) Uani 1 1 d . . . N12 N 0.1020(6) 0.7940(5) 0.1496(5) 0.024(2) Uani 1 1 d . . . C11 C 0.1616(7) 0.7157(7) 0.1592(6) 0.026(3) Uani 1 1 d . . . H11 H 0.1538 0.6702 0.2037 0.031 Uiso 1 1 calc R . . C12 C 0.2396(8) 0.6899(7) 0.1090(6) 0.024(3) Uani 1 1 d . . . C13 C 0.2428(7) 0.7359(7) 0.0295(6) 0.024(3) Uani 1 1 d . . . C14 C 0.3167(8) 0.7011(7) -0.0145(6) 0.027(3) Uani 1 1 d . . . H14 H 0.3176 0.7284 -0.0677 0.033 Uiso 1 1 calc R . . C15 C 0.3899(8) 0.6262(7) 0.0192(7) 0.037(3) Uani 1 1 d . . . H15 H 0.4411 0.6047 -0.0120 0.044 Uiso 1 1 calc R . . C16 C 0.3916(8) 0.5815(7) 0.0957(6) 0.032(3) Uani 1 1 d . . . C17 C 0.3149(7) 0.6144(7) 0.1381(6) 0.029(3) Uani 1 1 d . . . H17 H 0.3132 0.5837 0.1906 0.035 Uiso 1 1 calc R . . O1 O 0.1683(5) 0.8077(4) -0.0026(4) 0.0247(18) Uani 1 1 d . . . Br1 Br 0.49135(8) 0.48431(8) 0.13819(7) 0.0431(4) Uani 1 1 d . . . N31 N -0.0054(6) 0.9531(6) 0.1464(5) 0.022(2) Uani 1 1 d . . . N32 N -0.0738(6) 1.0325(5) 0.1556(5) 0.023(2) Uani 1 1 d . . . C31 C -0.1324(7) 1.0061(7) 0.2109(5) 0.015(2) Uani 1 1 d . . . C32 C -0.2129(7) 1.0673(7) 0.2382(5) 0.016(2) Uani 1 1 d . . . C33 C -0.2099(7) 1.1600(7) 0.2226(5) 0.019(3) Uani 1 1 d . . . C34 C -0.2867(8) 1.2175(7) 0.2507(6) 0.033(3) Uani 1 1 d . . . H34 H -0.2862 1.2784 0.2456 0.040 Uiso 1 1 calc R . . C35 C -0.3626(8) 1.1864(7) 0.2853(6) 0.032(3) Uani 1 1 d . . . H35 H -0.4151 1.2283 0.3005 0.038 Uiso 1 1 calc R . . C36 C -0.3671(7) 1.0983(7) 0.2991(5) 0.024(3) Uani 1 1 d . . . C37 C -0.2908(7) 1.0398(7) 0.2742(5) 0.021(3) Uani 1 1 d . . . H37 H -0.2919 0.9784 0.2823 0.025 Uiso 1 1 calc R . . O3 O -0.1413(5) 1.1923(4) 0.1890(4) 0.0272(19) Uani 1 1 d . . . Br3 Br -0.46958(8) 1.05624(8) 0.35212(7) 0.0421(3) Uani 1 1 d . . . N21 N -0.1012(6) 0.9113(5) 0.2368(4) 0.018(2) Uani 1 1 d . . . N22 N -0.1449(6) 0.8648(6) 0.2977(5) 0.025(2) Uani 1 1 d . . . C21 C -0.1187(8) 0.7781(8) 0.3159(6) 0.035(3) Uani 1 1 d . . . H21 H -0.0689 0.7467 0.2890 0.042 Uiso 1 1 calc R . . C22 C -0.1682(7) 0.7282(7) 0.3799(6) 0.023(3) Uani 1 1 d U . . C23 C -0.1403(8) 0.6329(7) 0.3991(6) 0.035(3) Uani 1 1 d . . . C24 C -0.1887(9) 0.5852(8) 0.4550(6) 0.050(4) Uani 1 1 d . . . H24 H -0.1714 0.5209 0.4675 0.060 Uiso 1 1 calc R . . C25 C -0.2628(10) 0.6301(8) 0.4936(7) 0.057(4) Uani 1 1 d . . . H25 H -0.2954 0.5969 0.5333 0.068 Uiso 1 1 calc R . . C26 C -0.2892(8) 0.7257(8) 0.4734(6) 0.042(3) Uani 1 1 d . . . C27 C -0.2418(7) 0.7723(7) 0.4183(5) 0.029(3) Uani 1 1 d . . . H27 H -0.2593 0.8366 0.4057 0.034 Uiso 1 1 calc R . . O2 O -0.0658(6) 0.5905(5) 0.3612(4) 0.053(2) Uani 1 1 d . . . H2A H -0.0559 0.5341 0.3786 0.079 Uiso 1 1 calc R . . Br2 Br -0.38908(10) 0.78886(9) 0.52706(7) 0.0604(4) Uani 1 1 d . . . C4 C -0.1561(8) 0.8682(7) -0.1792(6) 0.023(3) Uani 1 1 d . . . N41 N -0.1206(6) 0.7908(5) -0.1998(5) 0.028(2) Uani 1 1 d . . . H41N H -0.1513 0.7732 -0.2302 0.033 Uiso 1 1 calc R . . N42 N -0.0306(6) 0.7401(6) -0.1687(5) 0.031(2) Uani 1 1 d . . . C41 C 0.0106(8) 0.6696(7) -0.1934(6) 0.027(3) Uani 1 1 d . . . H41 H -0.0210 0.6576 -0.2317 0.032 Uiso 1 1 calc R . . C42 C 0.1033(7) 0.6076(7) -0.1654(7) 0.026(3) Uani 1 1 d . . . C43 C 0.1483(8) 0.6056(7) -0.1007(6) 0.022(3) Uani 1 1 d . . . C44 C 0.2354(8) 0.5387(7) -0.0807(6) 0.034(3) Uani 1 1 d . . . H44 H 0.2702 0.5371 -0.0380 0.041 Uiso 1 1 calc R . . C45 C 0.2718(8) 0.4745(8) -0.1220(7) 0.040(3) Uani 1 1 d . . . H45 H 0.3296 0.4291 -0.1064 0.048 Uiso 1 1 calc R . . C46 C 0.2234(8) 0.4776(7) -0.1859(7) 0.040(3) Uani 1 1 d . . . C47 C 0.1372(7) 0.5418(7) -0.2060(6) 0.026(3) Uani 1 1 d . . . H47 H 0.1009 0.5415 -0.2471 0.031 Uiso 1 1 calc R . . O4 O 0.1151(5) 0.6596(4) -0.0570(4) 0.0263(18) Uani 1 1 d . . . Br4 Br 0.26779(9) 0.39064(9) -0.24043(8) 0.0563(4) Uani 1 1 d . . . N61 N -0.1099(6) 0.9022(6) -0.1431(4) 0.021(2) Uani 1 1 d . . . N62 N -0.1742(6) 0.9822(6) -0.1332(4) 0.023(2) Uani 1 1 d . . . C61 C -0.2553(7) 0.9928(7) -0.1653(5) 0.018(3) Uani 1 1 d . . . C62 C -0.3389(7) 1.0710(7) -0.1714(6) 0.026(3) Uani 1 1 d . . . C63 C -0.3437(7) 1.1299(7) -0.1252(6) 0.018(3) Uani 1 1 d . . . C64 C -0.4230(8) 1.2049(7) -0.1360(6) 0.029(3) Uani 1 1 d . . . H64 H -0.4312 1.2432 -0.1029 0.035 Uiso 1 1 calc R . . C65 C -0.4887(7) 1.2256(7) -0.1913(6) 0.030(3) Uani 1 1 d . . . H65 H -0.5403 1.2785 -0.1970 0.036 Uiso 1 1 calc R . . C66 C -0.4818(7) 1.1713(7) -0.2391(6) 0.030(3) Uani 1 1 d . . . C67 C -0.4084(8) 1.0945(7) -0.2271(6) 0.030(3) Uani 1 1 d . . . H67 H -0.4047 1.0549 -0.2584 0.036 Uiso 1 1 calc R . . O6 O -0.2795(5) 1.1142(4) -0.0737(4) 0.0253(18) Uani 1 1 d . . . Br6 Br -0.57240(9) 1.20072(8) -0.31701(7) 0.0476(4) Uani 1 1 d . . . N51 N -0.2463(6) 0.9197(6) -0.1945(5) 0.027(2) Uani 1 1 d . . . N52 N -0.3175(6) 0.8937(5) -0.2253(4) 0.036(2) Uani 1 1 d U . . H52A H -0.3041 0.8408 -0.2357 0.043 Uiso 1 1 calc R . . H52B H -0.3752 0.9304 -0.2341 0.043 Uiso 1 1 calc R . . O7 O 0.0136(5) 1.0826(4) 0.0099(4) 0.0258(18) Uani 1 1 d D . . H7 H 0.020(7) 1.127(4) -0.025(4) 0.031 Uiso 1 1 d D . . O91 O 0.1921(4) 1.0271(4) -0.0573(4) 0.0312(19) Uani 1 1 d . . . S91 S 0.2867(2) 1.0491(2) -0.05447(19) 0.0509(10) Uani 1 1 d . . . C911 C 0.2872(9) 1.1375(9) -0.1370(7) 0.077(5) Uani 1 1 d . . . H91A H 0.2738 1.1197 -0.1816 0.116 Uiso 1 1 calc R . . H91B H 0.3500 1.1503 -0.1429 0.116 Uiso 1 1 calc R . . H91C H 0.2382 1.1920 -0.1328 0.116 Uiso 1 1 calc R . . C912 C 0.3716(9) 0.9615(9) -0.0797(7) 0.081(5) Uani 1 1 d . . . H91D H 0.3761 0.9049 -0.0396 0.121 Uiso 1 1 calc R . . H91E H 0.4338 0.9756 -0.0860 0.121 Uiso 1 1 calc R . . H91F H 0.3528 0.9545 -0.1277 0.121 Uiso 1 1 calc R . . O92 O -0.0671(5) 0.7612(5) 0.0079(4) 0.042(2) Uani 1 1 d . . . S92 S -0.0986(2) 0.6789(2) 0.05265(19) 0.0499(10) Uani 1 1 d . . . C921 C -0.0886(8) 0.6080(8) -0.0060(6) 0.056(4) Uani 1 1 d . . . H92A H -0.1339 0.6376 -0.0483 0.084 Uiso 1 1 calc R . . H92B H -0.1028 0.5512 0.0233 0.084 Uiso 1 1 calc R . . H92C H -0.0235 0.5949 -0.0260 0.084 Uiso 1 1 calc R . . C922 C 0.0017(8) 0.6194(7) 0.1074(7) 0.057(4) Uani 1 1 d . . . H92D H 0.0577 0.6373 0.0816 0.086 Uiso 1 1 calc R . . H92E H 0.0106 0.5543 0.1147 0.086 Uiso 1 1 calc R . . H92F H -0.0061 0.6329 0.1571 0.086 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 Gd1 0.0169(4) 0.0243(4) 0.0247(4) -0.0089(3) 0.0014(3) -0.0059(3) Gd2 0.0197(4) 0.0221(4) 0.0252(4) -0.0075(3) -0.0002(3) -0.0069(3) C1 0.022(7) 0.012(7) 0.041(8) -0.009(6) 0.008(6) -0.008(6) N11 0.019(6) 0.033(6) 0.022(5) -0.011(5) 0.006(4) -0.005(5) N12 0.018(5) 0.020(5) 0.034(6) -0.012(5) 0.006(5) -0.002(4) C11 0.021(7) 0.024(7) 0.022(7) -0.004(6) 0.005(5) 0.006(6) C12 0.032(7) 0.031(7) 0.012(6) -0.004(6) -0.003(6) -0.011(6) C13 0.004(6) 0.030(7) 0.035(8) -0.002(6) -0.003(6) -0.003(5) C14 0.016(7) 0.040(8) 0.038(8) -0.022(7) 0.010(6) -0.020(6) C15 0.024(8) 0.026(7) 0.064(10) -0.025(7) 0.014(7) -0.002(6) C16 0.046(8) 0.043(8) 0.016(7) -0.016(6) 0.007(6) -0.019(7) C17 0.031(7) 0.021(7) 0.034(7) -0.016(6) 0.004(6) 0.003(6) O1 0.022(5) 0.030(5) 0.026(5) -0.009(4) 0.005(4) -0.014(4) Br1 0.0273(8) 0.0435(8) 0.0479(9) -0.0126(7) 0.0012(6) 0.0086(6) N31 0.016(5) 0.033(6) 0.024(6) -0.008(5) 0.000(4) -0.018(5) N32 0.022(6) 0.023(6) 0.026(6) -0.012(5) -0.010(5) -0.001(5) C31 0.017(6) 0.015(6) 0.011(6) 0.006(5) -0.003(5) -0.009(5) C32 0.019(6) 0.019(6) 0.005(6) 0.003(5) -0.004(5) -0.003(5) C33 0.016(7) 0.029(7) 0.014(6) -0.007(6) -0.007(5) -0.003(6) C34 0.037(8) 0.031(8) 0.028(7) -0.009(6) 0.014(6) -0.006(7) C35 0.027(7) 0.022(7) 0.035(8) -0.006(6) -0.002(6) 0.011(6) C36 0.036(7) 0.022(7) 0.018(6) -0.009(6) 0.000(5) -0.012(6) C37 0.026(7) 0.036(7) 0.008(6) -0.009(5) 0.005(5) -0.015(6) O3 0.027(5) 0.023(4) 0.034(5) -0.009(4) 0.006(4) -0.011(4) Br3 0.0246(7) 0.0485(8) 0.0570(9) -0.0231(7) 0.0155(6) -0.0106(6) N21 0.019(5) 0.016(5) 0.019(5) -0.001(4) 0.006(4) -0.008(4) N22 0.022(6) 0.023(6) 0.028(6) -0.004(5) 0.004(4) -0.009(5) C21 0.034(8) 0.038(8) 0.038(8) -0.011(7) 0.008(6) -0.017(7) C22 0.025(5) 0.023(4) 0.020(4) 0.001(4) 0.007(4) -0.011(4) C23 0.036(8) 0.026(8) 0.040(8) 0.000(7) 0.010(6) -0.016(6) C24 0.072(11) 0.034(8) 0.043(9) -0.007(7) 0.026(8) -0.023(8) C25 0.082(12) 0.037(9) 0.046(9) -0.001(7) 0.028(8) -0.025(8) C26 0.045(9) 0.053(9) 0.031(8) -0.013(7) 0.014(7) -0.019(7) C27 0.030(7) 0.040(8) 0.017(7) -0.013(6) 0.012(6) -0.010(6) O2 0.056(6) 0.034(5) 0.068(6) -0.025(5) 0.036(5) -0.009(5) Br2 0.0482(10) 0.0648(10) 0.0533(10) -0.0092(8) 0.0222(8) -0.0026(8) C4 0.030(8) 0.013(7) 0.025(7) -0.011(6) 0.010(6) 0.002(6) N41 0.015(5) 0.032(6) 0.043(6) -0.021(5) -0.009(5) -0.002(5) N42 0.027(6) 0.028(6) 0.036(6) 0.000(5) -0.002(5) -0.015(5) C41 0.035(8) 0.025(7) 0.034(8) -0.024(6) -0.001(6) -0.014(6) C42 0.018(7) 0.013(6) 0.054(9) -0.016(6) 0.004(6) -0.006(5) C43 0.023(7) 0.018(7) 0.032(7) -0.009(6) 0.009(6) -0.015(6) C44 0.037(8) 0.022(7) 0.042(8) -0.004(7) -0.023(7) -0.005(6) C45 0.015(7) 0.041(8) 0.053(9) 0.002(7) -0.010(6) -0.002(6) C46 0.031(8) 0.036(8) 0.050(9) -0.014(7) -0.008(7) -0.002(6) C47 0.026(7) 0.025(7) 0.024(7) 0.006(6) -0.011(6) -0.013(6) O4 0.027(5) 0.029(5) 0.027(5) -0.010(4) 0.003(4) -0.011(4) Br4 0.0393(9) 0.0586(10) 0.0698(11) -0.0373(9) -0.0058(8) 0.0118(7) N61 0.026(6) 0.024(6) 0.021(6) -0.015(5) 0.000(4) -0.008(5) N62 0.015(5) 0.034(6) 0.025(6) -0.015(5) -0.001(4) -0.009(5) C61 0.019(7) 0.021(7) 0.018(6) -0.010(6) 0.009(5) -0.009(5) C62 0.018(7) 0.031(7) 0.022(7) -0.006(6) 0.002(6) 0.001(6) C63 0.010(6) 0.019(7) 0.026(7) -0.007(6) 0.004(5) -0.003(5) C64 0.024(7) 0.040(8) 0.033(8) -0.020(7) 0.010(6) -0.016(6) C65 0.006(6) 0.035(7) 0.058(9) -0.030(7) -0.009(6) -0.002(5) C66 0.018(7) 0.040(8) 0.033(7) -0.020(7) -0.012(6) 0.004(6) C67 0.043(8) 0.030(7) 0.027(7) -0.021(6) 0.005(6) -0.014(6) O6 0.023(5) 0.035(5) 0.019(4) -0.014(4) -0.006(4) 0.000(4) Br6 0.0370(8) 0.0500(9) 0.0537(9) -0.0255(8) -0.0209(7) 0.0095(7) N51 0.023(6) 0.027(6) 0.033(6) -0.009(5) -0.012(5) -0.006(5) N52 0.028(4) 0.035(4) 0.052(4) -0.023(4) -0.015(3) -0.007(3) O7 0.017(4) 0.031(5) 0.026(5) 0.003(4) 0.003(4) -0.012(4) O91 0.012(4) 0.045(5) 0.039(5) -0.015(4) 0.001(4) -0.009(4) S91 0.038(2) 0.073(3) 0.050(2) -0.015(2) 0.0088(18) -0.031(2) C911 0.059(11) 0.119(13) 0.061(10) -0.017(10) 0.012(8) -0.046(10) C912 0.045(10) 0.131(13) 0.056(10) 0.004(9) 0.017(8) -0.041(10) O92 0.048(6) 0.039(5) 0.055(6) -0.025(5) 0.027(4) -0.032(4) S92 0.048(2) 0.051(2) 0.056(2) -0.012(2) 0.0138(19) -0.026(2) C921 0.056(10) 0.066(9) 0.067(10) -0.037(8) 0.017(8) -0.037(8) C922 0.042(9) 0.041(8) 0.085(11) -0.005(8) -0.024(8) -0.011(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 Gd1 O6 2.274(7) 2_575 ? Gd1 O7 2.367(7) . ? Gd1 O1 2.392(6) . ? Gd1 O7 2.409(7) 2_575 ? Gd1 O91 2.421(7) . ? Gd1 N31 2.480(8) . ? Gd1 N62 2.554(7) 2_575 ? Gd1 N12 2.564(8) . ? Gd1 Gd1 3.8115(11) 2_575 ? Gd1 Gd2 3.8666(7) . ? Gd2 O3 2.247(7) 2_575 ? Gd2 O4 2.301(6) . ? Gd2 O1 2.355(6) . ? Gd2 O7 2.391(7) 2_575 ? Gd2 O92 2.448(7) . ? Gd2 N61 2.488(8) . ? Gd2 N32 2.537(8) 2_575 ? Gd2 N42 2.638(8) . ? C1 N31 1.295(11) . ? C1 N11 1.339(11) . ? C1 N21 1.375(11) . ? N11 N12 1.407(10) . ? N12 C11 1.285(10) . ? C11 C12 1.451(13) . ? C12 C17 1.395(13) . ? C12 C13 1.437(13) . ? C13 O1 1.371(11) . ? C13 C14 1.380(13) . ? C14 C15 1.393(14) . ? C15 C16 1.381(13) . ? C16 C17 1.379(12) . ? C16 Br1 1.841(11) . ? N31 N32 1.424(10) . ? N32 C31 1.325(11) . ? N32 Gd2 2.537(8) 2_575 ? C31 N21 1.403(11) . ? C31 C32 1.461(12) . ? C32 C37 1.381(12) . ? C32 C33 1.434(12) . ? C33 O3 1.284(11) . ? C33 C34 1.403(13) . ? C34 C35 1.371(13) . ? C35 C36 1.371(12) . ? C36 C37 1.380(12) . ? C36 Br3 1.891(10) . ? O3 Gd2 2.247(7) 2_575 ? N21 N22 1.372(10) . ? N22 C21 1.279(11) . ? C21 C22 1.480(13) . ? C22 C27 1.374(12) . ? C22 C23 1.406(13) . ? C23 C24 1.367(13) . ? C23 O2 1.365(11) . ? C24 C25 1.385(14) . ? C25 C26 1.410(14) . ? C26 C27 1.341(13) . ? C26 Br2 1.905(11) . ? C4 N61 1.279(11) . ? C4 N41 1.344(11) . ? C4 N51 1.348(12) . ? N41 N42 1.404(10) . ? N42 C41 1.303(11) . ? C41 C42 1.469(13) . ? C42 C43 1.380(13) . ? C42 C47 1.408(12) . ? C43 O4 1.307(10) . ? C43 C44 1.413(13) . ? C44 C45 1.402(13) . ? C45 C46 1.389(13) . ? C46 C47 1.386(13) . ? C46 Br4 1.871(11) . ? N61 N62 1.409(10) . ? N62 C61 1.305(11) . ? N62 Gd1 2.554(7) 2_575 ? C61 N51 1.379(11) . ? C61 C62 1.471(13) . ? C62 C67 1.390(13) . ? C62 C63 1.409(12) . ? C63 O6 1.300(10) . ? C63 C64 1.397(13) . ? C64 C65 1.352(13) . ? C65 C66 1.368(12) . ? C66 C67 1.365(13) . ? C66 Br6 1.886(10) . ? O6 Gd1 2.274(7) 2_575 ? N51 N52 1.415(10) . ? O7 Gd2 2.391(7) 2_575 ? O7 Gd1 2.409(7) 2_575 ? O91 S91 1.514(6) . ? S91 C912 1.738(13) . ? S91 C911 1.757(12) . ? O92 S92 1.506(7) . ? S92 C922 1.723(10) . ? S92 C921 1.730(10) . ? 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 O6 Gd1 O7 133.7(2) 2_575 . ? O6 Gd1 O1 77.1(2) 2_575 . ? O7 Gd1 O1 135.3(2) . . ? O6 Gd1 O7 146.6(2) 2_575 2_575 ? O7 Gd1 O7 74.1(3) . 2_575 ? O1 Gd1 O7 69.6(2) . 2_575 ? O6 Gd1 O91 75.7(2) 2_575 . ? O7 Gd1 O91 72.0(2) . . ? O1 Gd1 O91 91.8(2) . . ? O7 Gd1 O91 103.3(2) 2_575 . ? O6 Gd1 N31 124.2(2) 2_575 . ? O7 Gd1 N31 70.8(3) . . ? O1 Gd1 N31 123.7(2) . . ? O7 Gd1 N31 78.0(2) 2_575 . ? O91 Gd1 N31 140.8(3) . . ? O6 Gd1 N62 67.3(2) 2_575 2_575 ? O7 Gd1 N62 78.8(3) . 2_575 ? O1 Gd1 N62 143.4(3) . 2_575 ? O7 Gd1 N62 145.9(3) 2_575 2_575 ? O91 Gd1 N62 87.3(2) . 2_575 ? N31 Gd1 N62 73.8(3) . 2_575 ? O6 Gd1 N12 86.8(2) 2_575 . ? O7 Gd1 N12 130.4(2) . . ? O1 Gd1 N12 70.0(2) . . ? O7 Gd1 N12 83.3(2) 2_575 . ? O91 Gd1 N12 157.4(2) . . ? N31 Gd1 N12 61.4(3) . . ? N62 Gd1 N12 99.3(2) 2_575 . ? O6 Gd1 Gd1 163.02(17) 2_575 2_575 ? O7 Gd1 Gd1 37.44(16) . 2_575 ? O1 Gd1 Gd1 102.77(16) . 2_575 ? O7 Gd1 Gd1 36.67(16) 2_575 2_575 ? O91 Gd1 Gd1 87.31(15) . 2_575 ? N31 Gd1 Gd1 70.40(19) . 2_575 ? N62 Gd1 Gd1 113.72(19) 2_575 2_575 ? N12 Gd1 Gd1 109.23(18) . 2_575 ? O6 Gd1 Gd2 110.81(15) 2_575 . ? O7 Gd1 Gd2 102.03(17) . . ? O1 Gd1 Gd2 35.15(16) . . ? O7 Gd1 Gd2 36.18(16) 2_575 . ? O91 Gd1 Gd2 90.75(15) . . ? N31 Gd1 Gd2 108.62(17) . . ? N62 Gd1 Gd2 177.53(18) 2_575 . ? N12 Gd1 Gd2 81.96(17) . . ? Gd1 Gd1 Gd2 67.621(17) 2_575 . ? O3 Gd2 O4 80.9(2) 2_575 . ? O3 Gd2 O1 97.2(2) 2_575 . ? O4 Gd2 O1 82.9(2) . . ? O3 Gd2 O7 138.1(2) 2_575 2_575 ? O4 Gd2 O7 133.6(2) . 2_575 ? O1 Gd2 O7 70.5(2) . 2_575 ? O3 Gd2 O92 152.5(2) 2_575 . ? O4 Gd2 O92 79.9(2) . . ? O1 Gd2 O92 99.7(2) . . ? O7 Gd2 O92 68.6(2) 2_575 . ? O3 Gd2 N61 102.2(2) 2_575 . ? O4 Gd2 N61 128.8(2) . . ? O1 Gd2 N61 144.8(2) . . ? O7 Gd2 N61 75.5(2) 2_575 . ? O92 Gd2 N61 75.4(3) . . ? O3 Gd2 N32 68.0(2) 2_575 2_575 ? O4 Gd2 N32 144.7(2) . 2_575 ? O1 Gd2 N32 84.9(2) . 2_575 ? O7 Gd2 N32 71.1(2) 2_575 2_575 ? O92 Gd2 N32 134.9(2) . 2_575 ? N61 Gd2 N32 75.8(3) . 2_575 ? O3 Gd2 N42 73.4(2) 2_575 . ? O4 Gd2 N42 69.6(3) . . ? O1 Gd2 N42 151.9(3) . . ? O7 Gd2 N42 133.7(3) 2_575 . ? O92 Gd2 N42 81.5(2) . . ? N61 Gd2 N42 62.9(3) . . ? N32 Gd2 N42 114.3(2) 2_575 . ? O3 Gd2 Gd1 115.18(16) 2_575 . ? O4 Gd2 Gd1 115.52(16) . . ? O1 Gd2 Gd1 35.78(16) . . ? O7 Gd2 Gd1 36.49(16) 2_575 . ? O92 Gd2 Gd1 90.88(15) . . ? N61 Gd2 Gd1 109.06(18) . . ? N32 Gd2 Gd1 67.00(17) 2_575 . ? N42 Gd2 Gd1 170.1(2) . . ? N31 C1 N11 126.1(10) . . ? N31 C1 N21 108.1(9) . . ? N11 C1 N21 125.7(10) . . ? C1 N11 N12 109.0(8) . . ? C11 N12 N11 113.5(8) . . ? C11 N12 Gd1 124.0(7) . . ? N11 N12 Gd1 122.2(6) . . ? N12 C11 C12 126.5(10) . . ? C17 C12 C13 117.5(10) . . ? C17 C12 C11 118.7(10) . . ? C13 C12 C11 123.8(10) . . ? O1 C13 C14 121.1(10) . . ? O1 C13 C12 119.6(9) . . ? C14 C13 C12 118.9(10) . . ? C13 C14 C15 120.0(11) . . ? C16 C15 C14 123.1(11) . . ? C17 C16 C15 116.1(11) . . ? C17 C16 Br1 122.3(8) . . ? C15 C16 Br1 121.6(8) . . ? C16 C17 C12 124.2(11) . . ? C13 O1 Gd2 128.7(6) . . ? C13 O1 Gd1 120.4(6) . . ? Gd2 O1 Gd1 109.1(3) . . ? C1 N31 N32 109.5(8) . . ? C1 N31 Gd1 120.7(7) . . ? N32 N31 Gd1 129.5(6) . . ? C31 N32 N31 107.3(8) . . ? C31 N32 Gd2 133.1(7) . 2_575 ? N31 N32 Gd2 118.8(6) . 2_575 ? N32 C31 N21 107.1(9) . . ? N32 C31 C32 124.5(9) . . ? N21 C31 C32 128.4(9) . . ? C37 C32 C33 120.6(9) . . ? C37 C32 C31 122.6(9) . . ? C33 C32 C31 116.7(9) . . ? O3 C33 C34 118.7(10) . . ? O3 C33 C32 125.3(9) . . ? C34 C33 C32 115.9(10) . . ? C35 C34 C33 120.6(10) . . ? C36 C35 C34 123.8(10) . . ? C35 C36 C37 116.6(10) . . ? C35 C36 Br3 122.6(8) . . ? C37 C36 Br3 120.8(8) . . ? C36 C37 C32 122.3(10) . . ? C33 O3 Gd2 138.7(6) . 2_575 ? N22 N21 C1 131.3(9) . . ? N22 N21 C31 120.5(8) . . ? C1 N21 C31 108.1(8) . . ? C21 N22 N21 118.3(9) . . ? N22 C21 C22 118.1(10) . . ? C27 C22 C23 120.1(10) . . ? C27 C22 C21 121.8(10) . . ? C23 C22 C21 118.1(10) . . ? C24 C23 O2 121.7(10) . . ? C24 C23 C22 119.2(11) . . ? O2 C23 C22 119.0(10) . . ? C23 C24 C25 120.4(11) . . ? C24 C25 C26 119.2(11) . . ? C27 C26 C25 120.2(11) . . ? C27 C26 Br2 119.8(9) . . ? C25 C26 Br2 120.0(9) . . ? C26 C27 C22 120.8(11) . . ? N61 C4 N41 125.0(11) . . ? N61 C4 N51 111.6(9) . . ? N41 C4 N51 123.4(10) . . ? C4 N41 N42 114.6(8) . . ? C41 N42 N41 116.4(9) . . ? C41 N42 Gd2 126.7(7) . . ? N41 N42 Gd2 116.1(6) . . ? N42 C41 C42 123.5(10) . . ? C43 C42 C47 122.2(10) . . ? C43 C42 C41 124.5(10) . . ? C47 C42 C41 112.8(10) . . ? O4 C43 C42 124.6(10) . . ? O4 C43 C44 118.8(10) . . ? C42 C43 C44 116.6(10) . . ? C45 C44 C43 121.8(10) . . ? C46 C45 C44 119.9(11) . . ? C47 C46 C45 119.3(10) . . ? C47 C46 Br4 119.5(9) . . ? C45 C46 Br4 121.0(9) . . ? C46 C47 C42 119.9(10) . . ? C43 O4 Gd2 131.4(6) . . ? C4 N61 N62 105.9(8) . . ? C4 N61 Gd2 120.7(7) . . ? N62 N61 Gd2 132.2(6) . . ? C61 N62 N61 108.8(8) . . ? C61 N62 Gd1 133.6(7) . 2_575 ? N61 N62 Gd1 117.2(6) . 2_575 ? N62 C61 N51 107.5(9) . . ? N62 C61 C62 125.4(9) . . ? N51 C61 C62 127.0(9) . . ? C67 C62 C63 118.4(10) . . ? C67 C62 C61 122.0(10) . . ? C63 C62 C61 119.2(9) . . ? O6 C63 C64 121.7(9) . . ? O6 C63 C62 121.9(9) . . ? C64 C63 C62 116.3(9) . . ? C65 C64 C63 123.2(10) . . ? C64 C65 C66 120.7(10) . . ? C67 C66 C65 117.6(9) . . ? C67 C66 Br6 121.5(8) . . ? C65 C66 Br6 120.9(8) . . ? C66 C67 C62 123.5(9) . . ? C63 O6 Gd1 144.1(6) . 2_575 ? C4 N51 C61 106.2(8) . . ? C4 N51 N52 124.2(9) . . ? C61 N51 N52 129.1(9) . . ? Gd1 O7 Gd2 127.8(3) . 2_575 ? Gd1 O7 Gd1 105.9(3) . 2_575 ? Gd2 O7 Gd1 107.3(3) 2_575 2_575 ? S91 O91 Gd1 125.3(4) . . ? O91 S91 C912 105.0(5) . . ? O91 S91 C911 104.6(5) . . ? C912 S91 C911 99.9(6) . . ? S92 O92 Gd2 144.2(4) . . ? O92 S92 C922 100.4(5) . . ? O92 S92 C921 107.8(5) . . ? C922 S92 C921 97.9(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.179 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.135 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.010 -0.027 0.500 1688 669 ' ' _platon_squeeze_details ? _database_code_depnum_ccdc_archive 'CCDC 942795' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[(PdPh3)H3Br3L]' _chemical_melting_point ? _chemical_formula_moiety 'C40 H30 Br3 N6 O3 P Pd' _chemical_formula_sum 'C40 H30 Br3 N6 O3 P Pd' _chemical_formula_weight 1019.80 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' Br Br -0.2901 2.4595 '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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3937(5) _cell_length_b 13.1258(5) _cell_length_c 15.9585(6) _cell_angle_alpha 107.383(3) _cell_angle_beta 104.036(4) _cell_angle_gamma 99.477(3) _cell_volume 2135.92(15) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 9118 _cell_measurement_theta_min 2.5377 _cell_measurement_theta_max 28.6614 _exptl_crystal_description rhomboidal _exptl_crystal_colour red _exptl_crystal_size_max 0.373 _exptl_crystal_size_mid 0.143 _exptl_crystal_size_min 0.085 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 3.321 _exptl_absorpt_correction_T_min 0.4585 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '960 images at 1.0 deg in \w and 30 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37056 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.1151 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 28.77 _reflns_number_total 9951 _reflns_number_gt 5502 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.32.24 Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.32.24 Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.32.24 Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0415P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9951 _refine_ls_number_parameters 492 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0844 _refine_ls_goodness_of_fit_ref 0.847 _refine_ls_restrained_S_all 0.847 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.002 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 Pd11 Pd 0.31103(3) 0.15163(3) 0.35976(2) 0.01854(9) Uani 1 1 d . . . P11 P 0.16282(10) 0.23210(8) 0.40960(7) 0.0182(2) Uani 1 1 d . . . C1 C 0.3090(4) 0.0245(3) 0.1841(3) 0.0269(10) Uani 1 1 d . . . N21 N 0.2725(4) -0.0272(3) 0.0892(2) 0.0355(10) Uani 1 1 d . . . H21N H 0.2009 -0.0251 0.0542 0.043 Uiso 1 1 calc R . . N22 N 0.3497(4) -0.0817(3) 0.0509(2) 0.0320(9) Uani 1 1 d . B . C21 C 0.3096(5) -0.1392(4) -0.0358(3) 0.0356(12) Uani 1 1 d . . . H21 H 0.2262 -0.1539 -0.0743 0.043 Uiso 1 1 calc R A 1 C22 C 0.420(3) -0.183(3) -0.071(2) 0.028(2) Uani 0.250(17) 1 d PG B 1 C23 C 0.526(3) -0.198(2) -0.0158(17) 0.044(2) Uani 0.250(17) 1 d PG B 1 C24 C 0.596(2) -0.263(2) -0.0563(17) 0.055(3) Uani 0.250(17) 1 d PG B 1 H24 H 0.6683 -0.2735 -0.0188 0.065 Uiso 0.250(17) 1 calc PR B 1 C25 C 0.559(3) -0.314(2) -0.1517(17) 0.048(3) Uani 0.250(17) 1 d PG B 1 H25 H 0.6069 -0.3593 -0.1794 0.057 Uiso 0.250(17) 1 calc PR B 1 C26 C 0.453(3) -0.300(2) -0.2066(16) 0.0369(19) Uani 0.250(17) 1 d PG B 1 C27 C 0.383(2) -0.234(2) -0.166(2) 0.0263(19) Uani 0.250(17) 1 d PG B 1 H27 H 0.3108 -0.2241 -0.2036 0.032 Uiso 0.250(17) 1 calc PR B 1 O2 O 0.549(7) -0.113(8) 0.070(5) 0.073(4) Uani 0.250(17) 1 d P B 1 H2 H 0.4822 -0.0935 0.0718 0.110 Uiso 0.250(17) 1 calc PR B 1 Br2 Br 0.4073(10) -0.3637(8) -0.3304(6) 0.0448(6) Uani 0.250(17) 1 d P B 1 C22' C 0.3892(7) -0.1947(8) -0.0795(7) 0.028(2) Uani 0.750(17) 1 d PG B 2 C23' C 0.5136(8) -0.1770(7) -0.0294(5) 0.044(2) Uani 0.750(17) 1 d PG B 2 C24' C 0.5959(5) -0.2180(8) -0.0739(5) 0.055(3) Uani 0.750(17) 1 d PG B 2 H24' H 0.6808 -0.2060 -0.0396 0.065 Uiso 0.750(17) 1 calc PR B 2 C25' C 0.5538(7) -0.2767(7) -0.1684(5) 0.048(3) Uani 0.750(17) 1 d PG B 2 H25' H 0.6100 -0.3048 -0.1987 0.057 Uiso 0.750(17) 1 calc PR B 2 C26' C 0.4294(8) -0.2944(6) -0.2185(5) 0.0369(19) Uani 0.750(17) 1 d PG B 2 C27' C 0.3471(6) -0.2534(8) -0.1741(7) 0.0263(19) Uani 0.750(17) 1 d PG B 2 H27' H 0.2621 -0.2655 -0.2083 0.032 Uiso 0.750(17) 1 calc PR B 2 O2' O 0.5661(18) -0.129(2) 0.0637(17) 0.073(4) Uani 0.750(17) 1 d P B 2 H2' H 0.5178 -0.1528 0.0899 0.110 Uiso 0.750(17) 1 calc PR B 2 Br2' Br 0.3784(5) -0.3665(2) -0.3489(3) 0.0448(6) Uani 0.750(17) 1 d P B 2 N11 N 0.4023(3) 0.0000(3) 0.2332(2) 0.0219(8) Uani 1 1 d . . . N12 N 0.4310(3) 0.0655(2) 0.3247(2) 0.0187(8) Uani 1 1 d . . . C11 C 0.5246(4) 0.0521(3) 0.3835(3) 0.0190(9) Uani 1 1 d . . . H11 H 0.5677 0.0003 0.3588 0.023 Uiso 1 1 calc R . . C12 C 0.5675(4) 0.1084(3) 0.4814(3) 0.0173(9) Uani 1 1 d . . . C13 C 0.5020(4) 0.1755(3) 0.5306(3) 0.0187(9) Uani 1 1 d . . . C14 C 0.5510(4) 0.2206(3) 0.6283(3) 0.0221(10) Uani 1 1 d . . . H14 H 0.5070 0.2632 0.6623 0.027 Uiso 1 1 calc R . . C15 C 0.6601(4) 0.2043(3) 0.6751(3) 0.0251(10) Uani 1 1 d . . . H15 H 0.6917 0.2362 0.7406 0.030 Uiso 1 1 calc R . . C16 C 0.7242(4) 0.1409(3) 0.6259(3) 0.0223(10) Uani 1 1 d . . . C17 C 0.6781(4) 0.0930(3) 0.5312(3) 0.0217(9) Uani 1 1 d . . . H17 H 0.7223 0.0485 0.4989 0.026 Uiso 1 1 calc R . . O1 O 0.3975(2) 0.1979(2) 0.49402(17) 0.0241(7) Uani 1 1 d . . . Br1 Br 0.87743(4) 0.12148(4) 0.69054(3) 0.03132(13) Uani 1 1 d . . . N31 N 0.2460(3) 0.0966(3) 0.2202(2) 0.0219(8) Uani 1 1 d . . . N32 N 0.1735(3) 0.1314(3) 0.1571(2) 0.0232(8) Uani 1 1 d . D . C31 C 0.1497(4) 0.2254(3) 0.1882(3) 0.0237(10) Uani 1 1 d . . . H31 H 0.1839 0.2661 0.2526 0.028 Uiso 1 1 calc R C 1 C32 C 0.0746(5) 0.2731(4) 0.1319(4) 0.0257(14) Uani 0.917(2) 1 d PG D 1 C33 C 0.0135(6) 0.2168(3) 0.0382(4) 0.0299(16) Uani 0.917(2) 1 d PG D 1 C34 C -0.0543(6) 0.2679(4) -0.0140(3) 0.0375(18) Uani 0.917(2) 1 d PG D 1 H34 H -0.0960 0.2294 -0.0781 0.045 Uiso 0.917(2) 1 calc PR D 1 C35 C -0.0609(5) 0.3752(4) 0.0274(3) 0.0438(19) Uani 0.917(2) 1 d PG D 1 H35 H -0.1072 0.4101 -0.0083 0.053 Uiso 0.917(2) 1 calc PR D 1 C36 C 0.0002(4) 0.4316(3) 0.1211(3) 0.0333(14) Uani 0.917(2) 1 d PG D 1 C37 C 0.0679(4) 0.3805(4) 0.1734(3) 0.0268(13) Uani 0.917(2) 1 d PG D 1 H37 H 0.1097 0.4190 0.2374 0.032 Uiso 0.917(2) 1 calc PR D 1 O3 O 0.0211(6) 0.1132(5) -0.0048(3) 0.0423(15) Uani 0.917(2) 1 d P D 1 H3 H 0.0640 0.0915 0.0339 0.063 Uiso 0.917(2) 1 calc PR D 1 Br3 Br -0.00477(11) 0.57872(7) 0.18026(4) 0.0473(3) Uani 0.917(2) 1 d P D 1 C32' C 0.061(5) 0.269(4) 0.122(4) 0.013(7) Uiso 0.083(2) 1 d PG D 2 C33' C 0.032(6) 0.231(4) 0.026(4) 0.013(7) Uiso 0.083(2) 1 d PG D 2 C34' C -0.036(6) 0.283(4) -0.025(3) 0.013(7) Uiso 0.083(2) 1 d PG D 2 H34' H -0.0555 0.2565 -0.0902 0.016 Uiso 0.083(2) 1 calc PR D 2 C35' C -0.075(5) 0.373(4) 0.020(3) 0.013(7) Uiso 0.083(2) 1 d PG D 2 H35' H -0.1215 0.4085 -0.0155 0.016 Uiso 0.083(2) 1 calc PR D 2 C36' C -0.046(4) 0.411(4) 0.115(3) 0.013(7) Uiso 0.083(2) 1 d PG D 2 C37' C 0.022(4) 0.359(4) 0.166(3) 0.013(7) Uiso 0.083(2) 1 d PG D 2 H37' H 0.0415 0.3857 0.2317 0.016 Uiso 0.083(2) 1 calc PR D 2 Br3' Br -0.0836(12) 0.5362(7) 0.1638(5) 0.0473(3) Uani 0.083(2) 1 d P D 2 O3' O 0.002(6) 0.102(6) -0.027(4) 0.013(7) Uiso 0.083(2) 1 d P D 2 H3' H 0.0435 0.0732 0.0067 0.020 Uiso 0.083(2) 1 calc PR D 2 C70 C 0.1826(4) 0.3758(3) 0.4165(3) 0.0190(9) Uani 1 1 d . . . C75 C 0.3017(4) 0.4339(3) 0.4243(3) 0.0240(10) Uani 1 1 d . . . H75 H 0.3682 0.3987 0.4273 0.029 Uiso 1 1 calc R . . C74 C 0.3235(4) 0.5422(3) 0.4278(3) 0.0282(11) Uani 1 1 d . . . H74 H 0.4045 0.5813 0.4332 0.034 Uiso 1 1 calc R . . C73 C 0.2249(5) 0.5935(3) 0.4235(3) 0.0294(11) Uani 1 1 d . . . H73 H 0.2393 0.6678 0.4257 0.035 Uiso 1 1 calc R . . C72 C 0.1086(4) 0.5381(3) 0.4160(3) 0.0255(10) Uani 1 1 d . . . H72 H 0.0425 0.5738 0.4127 0.031 Uiso 1 1 calc R . . C71 C 0.0860(4) 0.4300(3) 0.4132(3) 0.0241(10) Uani 1 1 d . . . H71 H 0.0049 0.3924 0.4090 0.029 Uiso 1 1 calc R . . C60 C -0.0005(4) 0.1608(3) 0.3471(3) 0.0199(9) Uani 1 1 d . . . C65 C -0.0927(4) 0.1897(3) 0.3876(3) 0.0254(10) Uani 1 1 d . . . H65 H -0.0682 0.2434 0.4480 0.030 Uiso 1 1 calc R . . C64 C -0.2179(4) 0.1415(3) 0.3413(3) 0.0283(11) Uani 1 1 d . . . H64 H -0.2798 0.1638 0.3680 0.034 Uiso 1 1 calc R . . C63 C -0.2516(4) 0.0607(4) 0.2559(3) 0.0317(11) Uani 1 1 d . . . H63 H -0.3379 0.0269 0.2235 0.038 Uiso 1 1 calc R . . C62 C -0.1632(4) 0.0273(3) 0.2158(3) 0.0249(10) Uani 1 1 d . . . H62 H -0.1882 -0.0302 0.1572 0.030 Uiso 1 1 calc R . . C61 C -0.0379(4) 0.0787(3) 0.2619(3) 0.0228(10) Uani 1 1 d . . . H61 H 0.0232 0.0569 0.2342 0.027 Uiso 1 1 calc R . . C50 C 0.1762(4) 0.2354(3) 0.5263(3) 0.0203(9) Uani 1 1 d . . . C55 C 0.1438(4) 0.1356(3) 0.5392(3) 0.0259(10) Uani 1 1 d . . . H55 H 0.1073 0.0692 0.4872 0.031 Uiso 1 1 calc R . . C54 C 0.1642(4) 0.1322(4) 0.6271(3) 0.0325(11) Uani 1 1 d . . . H54 H 0.1440 0.0634 0.6352 0.039 Uiso 1 1 calc R . . C53 C 0.2135(4) 0.2279(4) 0.7028(3) 0.0377(12) Uani 1 1 d . . . H53 H 0.2275 0.2259 0.7634 0.045 Uiso 1 1 calc R . . C52 C 0.2424(5) 0.3273(4) 0.6895(3) 0.0404(13) Uani 1 1 d . . . H52 H 0.2756 0.3938 0.7417 0.048 Uiso 1 1 calc R . . C51 C 0.2245(4) 0.3319(3) 0.6033(3) 0.0272(11) Uani 1 1 d . . . H51 H 0.2450 0.4011 0.5959 0.033 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 Pd11 0.02265(19) 0.01830(18) 0.01754(17) 0.00653(13) 0.00911(14) 0.00808(14) P11 0.0220(6) 0.0166(5) 0.0188(5) 0.0070(4) 0.0087(5) 0.0069(5) C1 0.042(3) 0.022(2) 0.021(2) 0.0089(19) 0.013(2) 0.013(2) N21 0.053(3) 0.039(2) 0.017(2) 0.0079(17) 0.0071(19) 0.030(2) N22 0.047(3) 0.026(2) 0.025(2) 0.0047(17) 0.0178(19) 0.0154(19) C21 0.060(3) 0.033(3) 0.020(2) 0.009(2) 0.013(2) 0.029(3) C22 0.032(5) 0.021(3) 0.026(4) 0.003(3) 0.014(4) -0.003(4) C23 0.029(4) 0.053(5) 0.031(4) -0.009(3) 0.010(3) 0.002(3) C24 0.026(3) 0.068(8) 0.048(5) -0.006(4) 0.011(3) 0.005(4) C25 0.041(4) 0.049(6) 0.046(5) -0.002(4) 0.030(4) 0.002(4) C26 0.051(5) 0.024(3) 0.031(3) 0.001(2) 0.022(3) -0.001(3) C27 0.032(5) 0.011(4) 0.025(3) 0.001(3) 0.007(4) -0.007(4) O2 0.027(7) 0.106(10) 0.041(4) -0.036(5) 0.011(4) 0.011(4) Br2 0.0733(17) 0.0350(3) 0.0207(12) -0.0005(7) 0.0207(11) 0.0098(8) C22' 0.032(5) 0.021(3) 0.026(4) 0.003(3) 0.014(4) -0.003(4) C23' 0.029(4) 0.053(5) 0.031(4) -0.009(3) 0.010(3) 0.002(3) C24' 0.026(3) 0.068(8) 0.048(5) -0.006(4) 0.011(3) 0.005(4) C25' 0.041(4) 0.049(6) 0.046(5) -0.002(4) 0.030(4) 0.002(4) C26' 0.051(5) 0.024(3) 0.031(3) 0.001(2) 0.022(3) -0.001(3) C27' 0.032(5) 0.011(4) 0.025(3) 0.001(3) 0.007(4) -0.007(4) O2' 0.027(7) 0.106(10) 0.041(4) -0.036(5) 0.011(4) 0.011(4) Br2' 0.0733(17) 0.0350(3) 0.0207(12) -0.0005(7) 0.0207(11) 0.0098(8) N11 0.030(2) 0.0203(19) 0.0131(17) 0.0008(15) 0.0071(15) 0.0086(16) N12 0.0189(19) 0.0131(17) 0.0217(18) 0.0000(14) 0.0093(15) 0.0049(15) C11 0.020(2) 0.013(2) 0.029(2) 0.0079(18) 0.0160(19) 0.0047(18) C12 0.016(2) 0.010(2) 0.024(2) 0.0067(17) 0.0055(18) -0.0019(17) C13 0.019(2) 0.019(2) 0.021(2) 0.0097(18) 0.0115(18) 0.0033(18) C14 0.023(2) 0.022(2) 0.023(2) 0.0075(19) 0.0103(19) 0.0068(19) C15 0.032(3) 0.024(2) 0.019(2) 0.0087(18) 0.005(2) 0.006(2) C16 0.019(2) 0.014(2) 0.032(2) 0.0098(19) 0.0029(19) 0.0038(18) C17 0.023(2) 0.013(2) 0.031(2) 0.0095(18) 0.010(2) 0.0041(18) O1 0.0228(17) 0.0289(17) 0.0195(15) 0.0038(13) 0.0069(13) 0.0117(13) Br1 0.0270(3) 0.0281(3) 0.0345(3) 0.0088(2) 0.0019(2) 0.0113(2) N31 0.032(2) 0.0214(19) 0.0163(18) 0.0072(15) 0.0093(16) 0.0139(16) N32 0.031(2) 0.026(2) 0.0179(18) 0.0100(16) 0.0101(16) 0.0127(17) C31 0.032(3) 0.024(2) 0.019(2) 0.0099(19) 0.012(2) 0.010(2) C32 0.039(4) 0.022(3) 0.021(3) 0.011(2) 0.012(3) 0.014(2) C33 0.044(4) 0.018(3) 0.028(3) 0.011(2) 0.008(3) 0.009(3) C34 0.056(5) 0.030(3) 0.022(3) 0.011(2) 0.001(3) 0.010(3) C35 0.065(5) 0.040(3) 0.029(3) 0.019(3) 0.002(3) 0.029(3) C36 0.041(4) 0.031(3) 0.036(3) 0.016(3) 0.018(3) 0.017(3) C37 0.038(4) 0.027(3) 0.021(3) 0.010(2) 0.014(3) 0.012(3) O3 0.070(4) 0.024(3) 0.016(3) 0.000(2) -0.012(2) 0.019(2) Br3 0.0788(8) 0.0313(4) 0.0337(3) 0.0099(3) 0.0109(4) 0.0317(5) Br3' 0.0788(8) 0.0313(4) 0.0337(3) 0.0099(3) 0.0109(4) 0.0317(5) C70 0.026(2) 0.017(2) 0.018(2) 0.0067(17) 0.0093(18) 0.0086(19) C75 0.026(3) 0.021(2) 0.022(2) 0.0055(18) 0.0063(19) 0.004(2) C74 0.035(3) 0.022(2) 0.024(2) 0.0064(19) 0.010(2) -0.002(2) C73 0.051(3) 0.018(2) 0.022(2) 0.0090(19) 0.014(2) 0.008(2) C72 0.036(3) 0.021(2) 0.021(2) 0.0050(18) 0.012(2) 0.012(2) C71 0.028(3) 0.026(2) 0.024(2) 0.0096(19) 0.015(2) 0.009(2) C60 0.022(2) 0.019(2) 0.027(2) 0.0143(19) 0.0111(19) 0.0083(18) C65 0.032(3) 0.023(2) 0.028(2) 0.015(2) 0.013(2) 0.008(2) C64 0.027(3) 0.029(3) 0.034(3) 0.018(2) 0.014(2) 0.003(2) C63 0.025(3) 0.033(3) 0.037(3) 0.021(2) 0.002(2) 0.001(2) C62 0.029(3) 0.023(2) 0.021(2) 0.0112(19) 0.005(2) 0.002(2) C61 0.029(3) 0.022(2) 0.024(2) 0.0135(19) 0.010(2) 0.008(2) C50 0.019(2) 0.027(2) 0.020(2) 0.0121(19) 0.0082(18) 0.0095(19) C55 0.027(2) 0.027(2) 0.027(2) 0.010(2) 0.012(2) 0.009(2) C54 0.040(3) 0.034(3) 0.033(3) 0.020(2) 0.017(2) 0.008(2) C53 0.041(3) 0.052(3) 0.025(3) 0.019(2) 0.014(2) 0.010(3) C52 0.054(4) 0.036(3) 0.015(2) -0.004(2) 0.010(2) -0.004(3) C51 0.034(3) 0.025(2) 0.020(2) 0.0062(19) 0.012(2) -0.001(2) _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 Pd11 O1 1.983(3) . ? Pd11 N12 1.990(3) . ? Pd11 N31 2.023(3) . ? Pd11 P11 2.3101(11) . ? P11 C60 1.817(4) . ? P11 C50 1.819(4) . ? P11 C70 1.828(4) . ? C1 N11 1.307(5) . ? C1 N31 1.357(5) . ? C1 N21 1.384(5) . ? N21 N22 1.366(5) . ? N22 C21 1.285(5) . ? C21 C22' 1.435(8) . ? C21 C22 1.61(2) . ? C22 C23 1.3900 . ? C22 C27 1.3900 . ? C23 C24 1.3900 . ? C23 O2 1.41(6) . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C26 Br2 1.80(2) . ? C22' C23' 1.3900 . ? C22' C27' 1.3900 . ? C23' O2' 1.36(2) . ? C23' C24' 1.3900 . ? C24' C25' 1.3900 . ? C25' C26' 1.3900 . ? C26' C27' 1.3900 . ? C26' Br2' 1.902(7) . ? N11 N12 1.379(4) . ? N12 C11 1.313(5) . ? C11 C12 1.431(5) . ? C12 C17 1.397(5) . ? C12 C13 1.427(5) . ? C13 O1 1.314(5) . ? C13 C14 1.418(5) . ? C14 C15 1.371(5) . ? C15 C16 1.390(6) . ? C16 C17 1.377(5) . ? C16 Br1 1.899(4) . ? N31 N32 1.380(4) . ? N32 C31 1.286(5) . ? C31 C32 1.439(6) . ? C31 C32' 1.58(4) . ? C32 C33 1.3900 . ? C32 C37 1.3900 . ? C33 O3 1.356(7) . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C36 Br3 1.897(4) . ? C32' C33' 1.3900 . ? C32' C37' 1.3900 . ? C33' C34' 1.3900 . ? C33' O3' 1.59(8) . ? C34' C35' 1.3900 . ? C35' C36' 1.3900 . ? C36' C37' 1.3900 . ? C36' Br3' 1.76(4) . ? C70 C75 1.399(6) . ? C70 C71 1.405(5) . ? C75 C74 1.383(5) . ? C74 C73 1.399(6) . ? C73 C72 1.362(6) . ? C72 C71 1.384(5) . ? C60 C61 1.373(5) . ? C60 C65 1.407(6) . ? C65 C64 1.376(6) . ? C64 C63 1.370(6) . ? C63 C62 1.381(6) . ? C62 C61 1.383(6) . ? C50 C51 1.389(5) . ? C50 C55 1.391(5) . ? C55 C54 1.380(6) . ? C54 C53 1.373(6) . ? C53 C52 1.383(6) . ? C52 C51 1.362(6) . ? 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 O1 Pd11 N12 93.56(12) . . ? O1 Pd11 N31 171.33(13) . . ? N12 Pd11 N31 77.95(13) . . ? O1 Pd11 P11 83.15(8) . . ? N12 Pd11 P11 171.49(10) . . ? N31 Pd11 P11 105.51(10) . . ? C60 P11 C50 102.82(19) . . ? C60 P11 C70 107.25(18) . . ? C50 P11 C70 105.42(18) . . ? C60 P11 Pd11 117.11(14) . . ? C50 P11 Pd11 109.33(13) . . ? C70 P11 Pd11 113.77(14) . . ? N11 C1 N31 124.2(4) . . ? N11 C1 N21 117.4(4) . . ? N31 C1 N21 118.4(4) . . ? N22 N21 C1 118.7(4) . . ? C21 N22 N21 118.3(4) . . ? N22 C21 C22' 120.2(6) . . ? N22 C21 C22 110.9(14) . . ? C22' C21 C22 10.6(16) . . ? C23 C22 C27 120.0 . . ? C23 C22 C21 126(2) . . ? C27 C22 C21 112(2) . . ? C22 C23 C24 120.0 . . ? C22 C23 O2 102(4) . . ? C24 C23 O2 136(3) . . ? C25 C24 C23 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C27 120.0 . . ? C25 C26 Br2 120.0(18) . . ? C27 C26 Br2 120.0(18) . . ? C26 C27 C22 120.0 . . ? C23' C22' C27' 120.0 . . ? C23' C22' C21 119.4(6) . . ? C27' C22' C21 120.0(6) . . ? O2' C23' C24' 113.0(8) . . ? O2' C23' C22' 126.8(8) . . ? C24' C23' C22' 120.0 . . ? C23' C24' C25' 120.0 . . ? C24' C25' C26' 120.0 . . ? C27' C26' C25' 120.0 . . ? C27' C26' Br2' 121.2(5) . . ? C25' C26' Br2' 118.6(5) . . ? C26' C27' C22' 120.0 . . ? C1 N11 N12 108.8(3) . . ? C11 N12 N11 116.5(3) . . ? C11 N12 Pd11 124.8(3) . . ? N11 N12 Pd11 117.8(2) . . ? N12 C11 C12 125.9(4) . . ? C17 C12 C13 118.8(4) . . ? C17 C12 C11 117.3(4) . . ? C13 C12 C11 123.8(4) . . ? O1 C13 C14 116.0(4) . . ? O1 C13 C12 126.1(4) . . ? C14 C13 C12 117.9(4) . . ? C15 C14 C13 121.9(4) . . ? C14 C15 C16 119.4(4) . . ? C17 C16 C15 120.6(4) . . ? C17 C16 Br1 120.0(3) . . ? C15 C16 Br1 119.4(3) . . ? C16 C17 C12 121.4(4) . . ? C13 O1 Pd11 125.1(2) . . ? C1 N31 N32 114.4(3) . . ? C1 N31 Pd11 109.9(3) . . ? N32 N31 Pd11 134.1(3) . . ? C31 N32 N31 117.2(3) . . ? N32 C31 C32 124.3(4) . . ? N32 C31 C32' 121(2) . . ? C32 C31 C32' 4(2) . . ? C33 C32 C37 120.0 . . ? C33 C32 C31 122.1(4) . . ? C37 C32 C31 117.8(4) . . ? O3 C33 C32 121.4(4) . . ? O3 C33 C34 118.6(4) . . ? C32 C33 C34 120.0 . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C37 C36 C35 120.0 . . ? C37 C36 Br3 118.6(3) . . ? C35 C36 Br3 121.4(3) . . ? C36 C37 C32 120.0 . . ? C33' C32' C37' 120.0 . . ? C33' C32' C31 125(3) . . ? C37' C32' C31 115(3) . . ? C34' C33' C32' 120.0 . . ? C34' C33' O3' 112(4) . . ? C32' C33' O3' 118(4) . . ? C33' C34' C35' 120.0 . . ? C36' C35' C34' 120.0 . . ? C37' C36' C35' 120.0 . . ? C37' C36' Br3' 124(3) . . ? C35' C36' Br3' 115(3) . . ? C36' C37' C32' 120.0 . . ? C75 C70 C71 118.6(4) . . ? C75 C70 P11 117.3(3) . . ? C71 C70 P11 124.2(3) . . ? C74 C75 C70 120.7(4) . . ? C75 C74 C73 119.3(4) . . ? C72 C73 C74 120.7(4) . . ? C73 C72 C71 120.5(4) . . ? C72 C71 C70 120.2(4) . . ? C61 C60 C65 118.3(4) . . ? C61 C60 P11 122.6(3) . . ? C65 C60 P11 119.1(3) . . ? C64 C65 C60 121.2(4) . . ? C63 C64 C65 118.7(4) . . ? C64 C63 C62 121.6(4) . . ? C63 C62 C61 119.1(4) . . ? C60 C61 C62 121.0(4) . . ? C51 C50 C55 118.7(4) . . ? C51 C50 P11 123.0(3) . . ? C55 C50 P11 118.1(3) . . ? C54 C55 C50 120.5(4) . . ? C53 C54 C55 120.3(4) . . ? C54 C53 C52 119.0(4) . . ? C51 C52 C53 121.4(4) . . ? C52 C51 C50 120.0(4) . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.853 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.113 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 1.000 303 29 ' ' 2 0.156 0.542 0.716 10 -1 ' ' 3 0.844 0.458 0.284 10 -1 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 942796' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_8-[(pdpet3)h3br3l] _audit_creation_method SHELXL-97 _chemical_name_systematic ; (tris(5-Bromo-2-hydroxybenzylidene)triaminoguanidino)- triethylphosphine-palladium(ii) ; _chemical_name_common '[(PdPEt3)H3Br3L]' _chemical_melting_point ? _chemical_formula_moiety 'C28 H30 Br3 N6 O3 P Pd' _chemical_formula_sum 'C28 H30 Br3 N6 O3 P Pd' _chemical_formula_weight 875.65 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' Br Br -0.2901 2.4595 '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 9.6061(19) _cell_length_b 10.857(2) _cell_length_c 15.489(3) _cell_angle_alpha 101.61(3) _cell_angle_beta 94.92(3) _cell_angle_gamma 91.08(3) _cell_volume 1575.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 656 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 17.72 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 4.485 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7442 _exptl_absorpt_correction_T_max 0.8410 _exptl_absorpt_process_details 'SADABS Medium Absorber' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16679 _diffrn_reflns_av_R_equivalents 0.1448 _diffrn_reflns_av_sigmaI/netI 0.1641 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.10 _reflns_number_total 5625 _reflns_number_gt 3252 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0510P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5625 _refine_ls_number_parameters 394 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1348 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.1703 _refine_ls_wR_factor_gt 0.1471 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.006 _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 Pd1 Pd 0.55152(8) 0.04145(7) 0.32343(5) 0.0227(2) Uani 1 1 d . A . Br1 Br -0.03517(12) -0.26148(11) 0.49646(8) 0.0364(3) Uani 1 1 d . A . Br2 Br 0.79647(16) 0.92051(13) 0.87374(9) 0.0580(4) Uani 1 1 d . . . Br3 Br 0.87152(16) 0.26858(12) -0.08529(8) 0.0504(4) Uani 1 1 d . . . P1 P 0.6881(3) -0.0829(3) 0.22767(19) 0.0265(7) Uani 1 1 d . . . C50 C 0.7172(11) -0.2195(10) 0.2765(8) 0.034(3) Uani 1 1 d . A . H50B H 0.7714 -0.1918 0.3347 0.041 Uiso 1 1 calc R . . H50A H 0.6253 -0.2535 0.2872 0.041 Uiso 1 1 calc R . . C51 C 0.7942(13) -0.3266(11) 0.2219(9) 0.050(4) Uani 1 1 d . . . H51C H 0.7428 -0.3543 0.1635 0.075 Uiso 1 1 calc R A . H51A H 0.8004 -0.3972 0.2525 0.075 Uiso 1 1 calc R . . H51B H 0.8885 -0.2965 0.2148 0.075 Uiso 1 1 calc R . . C60 C 0.8606(11) -0.0335(9) 0.2076(7) 0.029(3) Uani 1 1 d . A . H60B H 0.9034 -0.1045 0.1696 0.035 Uiso 1 1 calc R . . H60A H 0.8524 0.0360 0.1749 0.035 Uiso 1 1 calc R . . C61 C 0.9558(10) 0.0102(10) 0.2915(8) 0.036(3) Uani 1 1 d . . . H61C H 0.9102 0.0750 0.3318 0.054 Uiso 1 1 calc R A . H61A H 1.0437 0.0451 0.2771 0.054 Uiso 1 1 calc R . . H61B H 0.9752 -0.0613 0.3199 0.054 Uiso 1 1 calc R . . C70 C 0.585(3) -0.151(2) 0.1185(14) 0.019(6) Uani 0.51(2) 1 d PD A 1 H70B H 0.6410 -0.2141 0.0823 0.023 Uiso 0.51(2) 1 calc PR A 1 H70A H 0.4980 -0.1936 0.1290 0.023 Uiso 0.51(2) 1 calc PR A 1 C71 C 0.549(3) -0.0417(19) 0.0684(12) 0.041(8) Uani 0.51(2) 1 d PD A 1 H71C H 0.5006 0.0234 0.1064 0.062 Uiso 0.51(2) 1 calc PR A 1 H71A H 0.4894 -0.0751 0.0139 0.062 Uiso 0.51(2) 1 calc PR A 1 H71B H 0.6361 -0.0052 0.0534 0.062 Uiso 0.51(2) 1 calc PR A 1 C70' C 0.627(3) -0.121(4) 0.115(2) 0.046(12) Uiso 0.49(2) 1 d PD A 2 H70C H 0.6107 -0.0433 0.0919 0.055 Uiso 0.49(2) 1 calc PR A 2 H70D H 0.6977 -0.1693 0.0805 0.055 Uiso 0.49(2) 1 calc PR A 2 C71' C 0.486(3) -0.203(3) 0.1024(19) 0.063(10) Uiso 0.49(2) 1 d PD A 2 H71F H 0.4988 -0.2727 0.1331 0.094 Uiso 0.49(2) 1 calc PR A 2 H71D H 0.4606 -0.2355 0.0393 0.094 Uiso 0.49(2) 1 calc PR A 2 H71E H 0.4118 -0.1499 0.1274 0.094 Uiso 0.49(2) 1 calc PR A 2 C1 C 0.6046(10) 0.2796(10) 0.4348(6) 0.023(2) Uani 1 1 d . A . N11 N 0.5039(8) 0.2394(8) 0.4739(5) 0.023(2) Uani 1 1 d . A . N12 N 0.4532(9) 0.1220(7) 0.4269(6) 0.025(2) Uani 1 1 d . . . C11 C 0.3543(10) 0.0665(9) 0.4581(7) 0.025(2) Uani 1 1 d . A . H11 H 0.3230 0.1106 0.5119 0.030 Uiso 1 1 calc R . . C12 C 0.2862(11) -0.0536(10) 0.4213(7) 0.029(3) Uani 1 1 d . . . C13 C 0.3282(11) -0.1351(10) 0.3436(7) 0.025(2) Uani 1 1 d . A . C14 C 0.2503(10) -0.2494(10) 0.3132(7) 0.026(2) Uani 1 1 d . . . H14 H 0.2714 -0.3030 0.2599 0.032 Uiso 1 1 calc R A . C15 C 0.1458(11) -0.2852(9) 0.3579(7) 0.026(2) Uani 1 1 d . A . H15 H 0.0974 -0.3641 0.3367 0.031 Uiso 1 1 calc R . . C16 C 0.1094(11) -0.2061(10) 0.4353(7) 0.029(3) Uani 1 1 d . . . C17 C 0.1772(11) -0.0940(10) 0.4644(7) 0.028(3) Uani 1 1 d . A . H16 H 0.1500 -0.0403 0.5161 0.034 Uiso 1 1 calc R . . O1 O 0.4311(7) -0.1142(7) 0.2985(5) 0.0310(18) Uani 1 1 d . . . N21 N 0.6634(8) 0.3952(7) 0.4706(5) 0.023(2) Uani 1 1 d . . . H21N H 0.7226 0.4318 0.4425 0.028 Uiso 1 1 calc R . . N22 N 0.6272(9) 0.4523(7) 0.5518(6) 0.024(2) Uani 1 1 d . . . C21 C 0.6858(10) 0.5585(9) 0.5909(6) 0.021(2) Uani 1 1 d . . . H21 H 0.7499 0.6004 0.5623 0.026 Uiso 1 1 calc R . . C22 C 0.6522(10) 0.6130(9) 0.6795(6) 0.020(2) Uani 1 1 d . . . C23 C 0.5576(10) 0.5541(9) 0.7241(7) 0.024(2) Uani 1 1 d . . . C24 C 0.5381(11) 0.6006(10) 0.8123(7) 0.032(3) Uani 1 1 d . . . H24 H 0.4784 0.5564 0.8424 0.038 Uiso 1 1 calc R . . C25 C 0.6067(11) 0.7122(10) 0.8561(7) 0.032(3) Uani 1 1 d . . . H25 H 0.5917 0.7463 0.9159 0.038 Uiso 1 1 calc R . . C26 C 0.6976(12) 0.7738(10) 0.8122(7) 0.034(3) Uani 1 1 d . . . C27 C 0.7174(10) 0.7242(9) 0.7243(7) 0.029(3) Uani 1 1 d . . . H27 H 0.7775 0.7683 0.6944 0.034 Uiso 1 1 calc R . . O2 O 0.4818(8) 0.4459(7) 0.6846(5) 0.0337(19) Uani 1 1 d . . . H2 H 0.5034 0.4221 0.6326 0.050 Uiso 1 1 calc R . . N31 N 0.6479(9) 0.2124(7) 0.3569(5) 0.024(2) Uani 1 1 d . . . N32 N 0.7433(8) 0.2755(8) 0.3197(6) 0.024(2) Uani 1 1 d . A . C31 C 0.7394(10) 0.2445(9) 0.2355(7) 0.023(2) Uani 1 1 d . . . H31 H 0.6702 0.1837 0.2052 0.028 Uiso 1 1 calc R A . C32 C 0.8346(11) 0.2970(9) 0.1838(7) 0.024(2) Uani 1 1 d . A . C33 C 0.9491(11) 0.3753(10) 0.2206(7) 0.028(3) Uani 1 1 d . . . C34 C 1.0382(13) 0.4211(10) 0.1698(8) 0.037(3) Uani 1 1 d . A . H34 H 1.1160 0.4744 0.1969 0.044 Uiso 1 1 calc R . . C35 C 1.0148(12) 0.3894(10) 0.0777(8) 0.036(3) Uani 1 1 d . . . H35 H 1.0770 0.4209 0.0421 0.043 Uiso 1 1 calc R A . C36 C 0.9015(13) 0.3125(10) 0.0384(7) 0.034(3) Uani 1 1 d . A . C37 C 0.8137(11) 0.2661(10) 0.0909(8) 0.032(3) Uani 1 1 d . . . H37 H 0.7368 0.2116 0.0636 0.039 Uiso 1 1 calc R A . O3 O 0.9774(7) 0.4106(7) 0.3103(5) 0.0311(18) Uani 1 1 d . A . H3 H 0.9053 0.3988 0.3351 0.047 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 0.0208(5) 0.0197(5) 0.0285(5) 0.0046(3) 0.0069(4) 0.0037(3) Br1 0.0290(7) 0.0366(7) 0.0466(8) 0.0120(6) 0.0138(6) -0.0017(5) Br2 0.0651(10) 0.0419(8) 0.0581(9) -0.0164(7) 0.0221(8) -0.0155(7) Br3 0.0850(11) 0.0328(7) 0.0375(8) 0.0070(6) 0.0281(7) 0.0073(7) P1 0.0277(16) 0.0224(16) 0.0302(17) 0.0045(12) 0.0091(13) 0.0060(12) C50 0.025(6) 0.026(6) 0.064(8) 0.029(6) 0.027(6) 0.009(5) C51 0.045(8) 0.027(7) 0.083(10) 0.015(7) 0.026(7) 0.017(6) C60 0.030(6) 0.011(5) 0.052(8) 0.015(5) 0.009(6) 0.004(5) C61 0.012(6) 0.036(7) 0.060(8) 0.016(6) -0.005(5) -0.001(5) C70 0.020(14) 0.012(12) 0.023(13) -0.001(9) -0.002(10) -0.013(11) C71 0.069(18) 0.042(15) 0.008(11) -0.002(10) -0.016(11) 0.037(13) C1 0.016(6) 0.033(7) 0.022(6) 0.009(5) -0.001(5) -0.002(5) N11 0.020(5) 0.023(5) 0.024(5) 0.003(4) 0.002(4) 0.002(4) N12 0.024(5) 0.015(5) 0.036(5) 0.007(4) -0.002(4) -0.006(4) C11 0.016(6) 0.023(6) 0.034(6) 0.005(5) 0.000(5) 0.007(5) C12 0.025(6) 0.027(6) 0.036(7) 0.011(5) 0.000(5) 0.004(5) C13 0.018(6) 0.024(6) 0.032(6) 0.008(5) -0.006(5) 0.007(5) C14 0.024(6) 0.024(6) 0.031(6) 0.005(5) 0.000(5) 0.007(5) C15 0.023(6) 0.018(6) 0.039(7) 0.012(5) 0.003(5) 0.002(5) C16 0.023(6) 0.022(6) 0.042(7) 0.009(5) 0.006(5) 0.005(5) C17 0.028(6) 0.029(7) 0.031(6) 0.009(5) 0.009(5) 0.008(5) O1 0.027(4) 0.032(4) 0.037(5) 0.005(3) 0.018(4) 0.005(3) N21 0.023(5) 0.020(5) 0.026(5) -0.001(4) 0.008(4) 0.001(4) N22 0.023(5) 0.015(5) 0.035(5) 0.004(4) 0.006(4) 0.007(4) C21 0.015(5) 0.025(6) 0.027(6) 0.010(5) 0.005(5) 0.012(4) C22 0.018(6) 0.020(6) 0.026(6) 0.009(4) 0.005(5) 0.003(4) C23 0.019(6) 0.017(6) 0.036(7) 0.003(5) 0.004(5) 0.005(4) C24 0.033(7) 0.030(7) 0.038(7) 0.013(5) 0.013(5) 0.008(5) C25 0.035(7) 0.033(7) 0.028(6) 0.002(5) 0.015(5) 0.009(5) C26 0.040(7) 0.024(6) 0.034(7) -0.004(5) 0.008(6) 0.011(5) C27 0.019(6) 0.021(6) 0.048(7) 0.012(5) 0.009(5) -0.005(5) O2 0.035(5) 0.031(5) 0.035(5) 0.003(4) 0.011(4) 0.002(4) N31 0.032(5) 0.015(5) 0.028(5) 0.008(4) 0.010(4) 0.003(4) N32 0.022(5) 0.021(5) 0.030(5) 0.005(4) 0.011(4) 0.012(4) C31 0.014(5) 0.024(6) 0.036(7) 0.012(5) 0.003(5) 0.010(4) C32 0.023(6) 0.017(6) 0.030(6) 0.001(5) 0.012(5) 0.010(5) C33 0.035(7) 0.020(6) 0.028(6) 0.005(5) 0.001(5) 0.011(5) C34 0.045(8) 0.016(6) 0.047(8) 0.001(5) 0.012(6) 0.006(5) C35 0.045(8) 0.021(6) 0.048(8) 0.016(5) 0.024(6) 0.012(6) C36 0.049(8) 0.018(6) 0.038(7) 0.008(5) 0.022(6) 0.012(6) C37 0.028(6) 0.017(6) 0.054(8) 0.008(5) 0.012(6) 0.004(5) O3 0.026(4) 0.027(4) 0.042(5) 0.005(4) 0.013(4) 0.007(3) _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 Pd1 O1 1.982(7) . ? Pd1 N12 1.988(9) . ? Pd1 N31 2.009(8) . ? Pd1 P1 2.311(3) . ? Br1 C16 1.900(11) . ? Br2 C26 1.878(11) . ? Br3 C36 1.874(11) . ? P1 C70' 1.76(3) . ? P1 C60 1.803(10) . ? P1 C50 1.811(10) . ? P1 C70 1.89(2) . ? C50 C51 1.535(14) . ? C50 H50B 0.9900 . ? C50 H50A 0.9900 . ? C51 H51C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C60 C61 1.510(14) . ? C60 H60B 0.9900 . ? C60 H60A 0.9900 . ? C61 H61C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C70 C71 1.57(2) . ? C70 H70B 0.9900 . ? C70 H70A 0.9900 . ? C71 H71C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C70' C71' 1.58(2) . ? C70' H70C 0.9900 . ? C70' H70D 0.9900 . ? C71' H71F 0.9800 . ? C71' H71D 0.9800 . ? C71' H71E 0.9800 . ? C1 N11 1.298(12) . ? C1 N21 1.357(12) . ? C1 N31 1.380(12) . ? N11 N12 1.391(11) . ? N12 C11 1.292(12) . ? C11 C12 1.435(14) . ? C11 H11 0.9500 . ? C12 C17 1.398(14) . ? C12 C13 1.437(14) . ? C13 O1 1.300(12) . ? C13 C14 1.411(14) . ? C14 C15 1.360(14) . ? C14 H14 0.9500 . ? C15 C16 1.403(14) . ? C15 H15 0.9500 . ? C16 C17 1.344(14) . ? C17 H16 0.9500 . ? N21 N22 1.362(11) . ? N21 H21N 0.8800 . ? N22 C21 1.284(12) . ? C21 C22 1.447(13) . ? C21 H21 0.9500 . ? C22 C27 1.375(13) . ? C22 C23 1.405(13) . ? C23 O2 1.373(11) . ? C23 C24 1.387(14) . ? C24 C25 1.387(15) . ? C24 H24 0.9500 . ? C25 C26 1.391(15) . ? C25 H25 0.9500 . ? C26 C27 1.390(14) . ? C27 H27 0.9500 . ? O2 H2 0.8400 . ? N31 N32 1.366(11) . ? N32 C31 1.277(12) . ? C31 C32 1.447(13) . ? C31 H31 0.9500 . ? C32 C33 1.384(14) . ? C32 C37 1.407(14) . ? C33 C34 1.362(15) . ? C33 O3 1.367(12) . ? C34 C35 1.395(15) . ? C34 H34 0.9500 . ? C35 C36 1.379(15) . ? C35 H35 0.9500 . ? C36 C37 1.376(14) . ? C37 H37 0.9500 . ? O3 H3 0.8400 . ? 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 O1 Pd1 N12 94.0(3) . . ? O1 Pd1 N31 171.1(3) . . ? N12 Pd1 N31 78.1(3) . . ? O1 Pd1 P1 82.0(2) . . ? N12 Pd1 P1 165.5(2) . . ? N31 Pd1 P1 106.6(2) . . ? C70' P1 C60 94.3(10) . . ? C70' P1 C50 113.3(13) . . ? C60 P1 C50 104.2(5) . . ? C70' P1 C70 16.0(12) . . ? C60 P1 C70 109.3(9) . . ? C50 P1 C70 102.9(8) . . ? C70' P1 Pd1 117.9(12) . . ? C60 P1 Pd1 122.9(4) . . ? C50 P1 Pd1 103.9(4) . . ? C70 P1 Pd1 111.4(8) . . ? C51 C50 P1 115.9(8) . . ? C51 C50 H50B 108.3 . . ? P1 C50 H50B 108.3 . . ? C51 C50 H50A 108.3 . . ? P1 C50 H50A 108.3 . . ? H50B C50 H50A 107.4 . . ? C50 C51 H51C 109.5 . . ? C50 C51 H51A 109.5 . . ? H51C C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51C C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C61 C60 P1 113.1(8) . . ? C61 C60 H60B 109.0 . . ? P1 C60 H60B 109.0 . . ? C61 C60 H60A 109.0 . . ? P1 C60 H60A 109.0 . . ? H60B C60 H60A 107.8 . . ? C60 C61 H61C 109.5 . . ? C60 C61 H61A 109.5 . . ? H61C C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61C C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C71 C70 P1 108.9(14) . . ? C71 C70 H70B 109.9 . . ? P1 C70 H70B 109.9 . . ? C71 C70 H70A 109.9 . . ? P1 C70 H70A 109.9 . . ? H70B C70 H70A 108.3 . . ? C71' C70' P1 110(2) . . ? C71' C70' H70C 109.7 . . ? P1 C70' H70C 109.7 . . ? C71' C70' H70D 109.7 . . ? P1 C70' H70D 109.7 . . ? H70C C70' H70D 108.2 . . ? C70' C71' H71F 109.5 . . ? C70' C71' H71D 109.5 . . ? H71F C71' H71D 109.5 . . ? C70' C71' H71E 109.5 . . ? H71F C71' H71E 109.5 . . ? H71D C71' H71E 109.5 . . ? N11 C1 N21 117.7(9) . . ? N11 C1 N31 122.6(9) . . ? N21 C1 N31 119.7(9) . . ? C1 N11 N12 110.0(8) . . ? C11 N12 N11 118.2(9) . . ? C11 N12 Pd1 123.7(7) . . ? N11 N12 Pd1 117.7(6) . . ? N12 C11 C12 128.0(10) . . ? N12 C11 H11 116.0 . . ? C12 C11 H11 116.0 . . ? C17 C12 C11 118.5(10) . . ? C17 C12 C13 118.9(10) . . ? C11 C12 C13 122.5(10) . . ? O1 C13 C14 116.8(9) . . ? O1 C13 C12 126.5(10) . . ? C14 C13 C12 116.8(10) . . ? C15 C14 C13 122.1(10) . . ? C15 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C14 C15 C16 120.2(10) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 119.6(10) . . ? C17 C16 Br1 121.8(8) . . ? C15 C16 Br1 118.6(8) . . ? C16 C17 C12 122.3(10) . . ? C16 C17 H16 118.8 . . ? C12 C17 H16 118.8 . . ? C13 O1 Pd1 125.0(6) . . ? C1 N21 N22 117.4(8) . . ? C1 N21 H21N 121.3 . . ? N22 N21 H21N 121.3 . . ? C21 N22 N21 119.9(8) . . ? N22 C21 C22 118.8(9) . . ? N22 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C27 C22 C23 117.6(9) . . ? C27 C22 C21 120.0(9) . . ? C23 C22 C21 122.4(9) . . ? O2 C23 C24 115.8(9) . . ? O2 C23 C22 122.7(9) . . ? C24 C23 C22 121.5(10) . . ? C23 C24 C25 119.4(10) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C24 C25 C26 119.7(10) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C27 C26 C25 119.8(10) . . ? C27 C26 Br2 120.8(9) . . ? C25 C26 Br2 119.4(8) . . ? C22 C27 C26 121.7(10) . . ? C22 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? C23 O2 H2 109.5 . . ? N32 N31 C1 114.4(8) . . ? N32 N31 Pd1 134.6(6) . . ? C1 N31 Pd1 111.0(6) . . ? C31 N32 N31 114.8(9) . . ? N32 C31 C32 123.5(10) . . ? N32 C31 H31 118.3 . . ? C32 C31 H31 118.3 . . ? C33 C32 C37 117.0(10) . . ? C33 C32 C31 123.7(10) . . ? C37 C32 C31 119.3(10) . . ? C34 C33 O3 116.8(10) . . ? C34 C33 C32 122.1(10) . . ? O3 C33 C32 121.1(10) . . ? C33 C34 C35 119.8(11) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C36 C35 C34 120.0(11) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C37 C36 C35 119.2(11) . . ? C37 C36 Br3 120.8(9) . . ? C35 C36 Br3 119.9(8) . . ? C36 C37 C32 121.8(11) . . ? C36 C37 H37 119.1 . . ? C32 C37 H37 119.1 . . ? C33 O3 H3 109.5 . . ? 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 O1 Pd1 P1 C70' 71.2(12) . . . . ? N12 Pd1 P1 C70' 146.0(15) . . . . ? N31 Pd1 P1 C70' -106.7(12) . . . . ? O1 Pd1 P1 C60 -172.5(5) . . . . ? N12 Pd1 P1 C60 -97.6(10) . . . . ? N31 Pd1 P1 C60 9.6(5) . . . . ? O1 Pd1 P1 C50 -55.1(5) . . . . ? N12 Pd1 P1 C50 19.8(11) . . . . ? N31 Pd1 P1 C50 127.0(5) . . . . ? O1 Pd1 P1 C70 55.0(7) . . . . ? N12 Pd1 P1 C70 129.9(12) . . . . ? N31 Pd1 P1 C70 -122.9(8) . . . . ? C70' P1 C50 C51 45.1(14) . . . . ? C60 P1 C50 C51 -56.1(10) . . . . ? C70 P1 C50 C51 58.0(12) . . . . ? Pd1 P1 C50 C51 174.2(8) . . . . ? C70' P1 C60 C61 -180.0(15) . . . . ? C50 P1 C60 C61 -64.6(9) . . . . ? C70 P1 C60 C61 -174.1(9) . . . . ? Pd1 P1 C60 C61 52.6(8) . . . . ? C70' P1 C70 C71 -49(6) . . . . ? C60 P1 C70 C71 -70.7(18) . . . . ? C50 P1 C70 C71 179.1(15) . . . . ? Pd1 P1 C70 C71 68.3(17) . . . . ? C60 P1 C70' C71' 166(2) . . . . ? C50 P1 C70' C71' 58(3) . . . . ? C70 P1 C70' C71' 6(5) . . . . ? Pd1 P1 C70' C71' -63(3) . . . . ? N21 C1 N11 N12 178.1(8) . . . . ? N31 C1 N11 N12 1.4(13) . . . . ? C1 N11 N12 C11 178.3(9) . . . . ? C1 N11 N12 Pd1 5.0(10) . . . . ? O1 Pd1 N12 C11 4.5(9) . . . . ? N31 Pd1 N12 C11 -179.6(9) . . . . ? P1 Pd1 N12 C11 -68.9(14) . . . . ? O1 Pd1 N12 N11 177.4(7) . . . . ? N31 Pd1 N12 N11 -6.7(7) . . . . ? P1 Pd1 N12 N11 104.0(10) . . . . ? N11 N12 C11 C12 179.9(9) . . . . ? Pd1 N12 C11 C12 -7.3(15) . . . . ? N12 C11 C12 C17 -177.5(10) . . . . ? N12 C11 C12 C13 4.2(17) . . . . ? C17 C12 C13 O1 -176.7(9) . . . . ? C11 C12 C13 O1 1.6(17) . . . . ? C17 C12 C13 C14 3.2(15) . . . . ? C11 C12 C13 C14 -178.6(10) . . . . ? O1 C13 C14 C15 175.9(9) . . . . ? C12 C13 C14 C15 -4.0(15) . . . . ? C13 C14 C15 C16 2.1(16) . . . . ? C14 C15 C16 C17 0.8(16) . . . . ? C14 C15 C16 Br1 -179.0(8) . . . . ? C15 C16 C17 C12 -1.5(16) . . . . ? Br1 C16 C17 C12 178.3(8) . . . . ? C11 C12 C17 C16 -178.8(10) . . . . ? C13 C12 C17 C16 -0.5(16) . . . . ? C14 C13 O1 Pd1 177.2(7) . . . . ? C12 C13 O1 Pd1 -3.0(15) . . . . ? N12 Pd1 O1 C13 0.3(8) . . . . ? N31 Pd1 O1 C13 -27(3) . . . . ? P1 Pd1 O1 C13 166.2(8) . . . . ? N11 C1 N21 N22 9.6(13) . . . . ? N31 C1 N21 N22 -173.6(9) . . . . ? C1 N21 N22 C21 176.0(9) . . . . ? N21 N22 C21 C22 -176.0(8) . . . . ? N22 C21 C22 C27 177.5(9) . . . . ? N22 C21 C22 C23 -0.2(15) . . . . ? C27 C22 C23 O2 177.0(9) . . . . ? C21 C22 C23 O2 -5.2(15) . . . . ? C27 C22 C23 C24 -4.9(15) . . . . ? C21 C22 C23 C24 172.9(10) . . . . ? O2 C23 C24 C25 -177.6(9) . . . . ? C22 C23 C24 C25 4.2(16) . . . . ? C23 C24 C25 C26 -2.2(17) . . . . ? C24 C25 C26 C27 1.0(17) . . . . ? C24 C25 C26 Br2 -177.1(8) . . . . ? C23 C22 C27 C26 3.7(16) . . . . ? C21 C22 C27 C26 -174.1(10) . . . . ? C25 C26 C27 C22 -1.9(17) . . . . ? Br2 C26 C27 C22 176.2(8) . . . . ? N11 C1 N31 N32 172.6(9) . . . . ? N21 C1 N31 N32 -4.0(13) . . . . ? N11 C1 N31 Pd1 -6.7(12) . . . . ? N21 C1 N31 Pd1 176.6(7) . . . . ? O1 Pd1 N31 N32 -144.6(18) . . . . ? N12 Pd1 N31 N32 -172.4(10) . . . . ? P1 Pd1 N31 N32 21.8(10) . . . . ? O1 Pd1 N31 C1 34(2) . . . . ? N12 Pd1 N31 C1 6.7(7) . . . . ? P1 Pd1 N31 C1 -159.1(6) . . . . ? C1 N31 N32 C31 -150.6(9) . . . . ? Pd1 N31 N32 C31 28.4(13) . . . . ? N31 N32 C31 C32 -177.8(9) . . . . ? N32 C31 C32 C33 7.5(15) . . . . ? N32 C31 C32 C37 -173.9(9) . . . . ? C37 C32 C33 C34 0.1(15) . . . . ? C31 C32 C33 C34 178.7(10) . . . . ? C37 C32 C33 O3 179.8(9) . . . . ? C31 C32 C33 O3 -1.6(15) . . . . ? O3 C33 C34 C35 -179.6(9) . . . . ? C32 C33 C34 C35 0.2(16) . . . . ? C33 C34 C35 C36 0.3(16) . . . . ? C34 C35 C36 C37 -1.0(16) . . . . ? C34 C35 C36 Br3 -179.3(8) . . . . ? C35 C36 C37 C32 1.3(16) . . . . ? Br3 C36 C37 C32 179.6(8) . . . . ? C33 C32 C37 C36 -0.9(15) . . . . ? C31 C32 C37 C36 -179.5(10) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.816 _refine_diff_density_min -1.678 _refine_diff_density_rms 0.193 _database_code_depnum_ccdc_archive 'CCDC 942797' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_9-[(pdpet3)h3l] _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(2-hydroxy-benzylidene)triaminoguanidino-triethylphosphine-palladium(ii)' ; _chemical_name_common '[(PdPEt3)H3L]' _chemical_melting_point ? _chemical_formula_moiety 'C28 H33 N6 O3 P Pd, C4H10 O' _chemical_formula_sum 'C32 H43 N6 O4 P Pd' _chemical_formula_weight 713.09 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.531(6) _cell_length_b 17.175(4) _cell_length_c 18.170(4) _cell_angle_alpha 90.00 _cell_angle_beta 123.949(3) _cell_angle_gamma 90.00 _cell_volume 6609(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6642 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 23.15 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2960 _exptl_absorpt_coefficient_mu 0.655 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8227 _exptl_absorpt_correction_T_max 0.8693 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34220 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.10 _reflns_number_total 5884 _reflns_number_gt 4693 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0639P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5884 _refine_ls_number_parameters 404 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1323 _refine_ls_wR_factor_gt 0.1253 _refine_ls_goodness_of_fit_ref 1.281 _refine_ls_restrained_S_all 1.281 _refine_ls_shift/su_max 0.055 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.762075(14) 0.048293(17) 0.58106(2) 0.02953(13) Uani 1 1 d . . . P1 P 0.73371(5) 0.14734(6) 0.63807(7) 0.0295(2) Uani 1 1 d . . . C1 C 0.70029(18) -0.0913(2) 0.4969(3) 0.0302(9) Uani 1 1 d . . . C60 C 0.78217(19) 0.1567(2) 0.7590(3) 0.0361(9) Uani 1 1 d . . . H60B H 0.7675 0.2022 0.7761 0.043 Uiso 1 1 calc R . . H60A H 0.7764 0.1098 0.7853 0.043 Uiso 1 1 calc R . . C61 C 0.8520(2) 0.1665(3) 0.7967(3) 0.0436(11) Uani 1 1 d . . . H61C H 0.8588 0.2164 0.7770 0.065 Uiso 1 1 calc R . . H61B H 0.8661 0.1239 0.7758 0.065 Uiso 1 1 calc R . . H61A H 0.8762 0.1655 0.8617 0.065 Uiso 1 1 calc R . . C50 C 0.7430(2) 0.2378(2) 0.5948(3) 0.0373(10) Uani 1 1 d . . . H50A H 0.7867 0.2400 0.6101 0.045 Uiso 1 1 calc R . . H50B H 0.7144 0.2363 0.5293 0.045 Uiso 1 1 calc R . . C51 C 0.7301(2) 0.3129(2) 0.6271(3) 0.0441(11) Uani 1 1 d . . . H51B H 0.7573 0.3149 0.6920 0.066 Uiso 1 1 calc R . . H51A H 0.6858 0.3142 0.6075 0.066 Uiso 1 1 calc R . . H51C H 0.7391 0.3577 0.6024 0.066 Uiso 1 1 calc R . . C70 C 0.65310(18) 0.1523(2) 0.6100(3) 0.0339(9) Uani 1 1 d . . . H70A H 0.6473 0.1108 0.6426 0.041 Uiso 1 1 calc R . . H70B H 0.6470 0.2030 0.6301 0.041 Uiso 1 1 calc R . . C71 C 0.6035(2) 0.1433(3) 0.5123(3) 0.0500(12) Uani 1 1 d . . . H71B H 0.6105 0.0945 0.4911 0.075 Uiso 1 1 calc R . . H71C H 0.6060 0.1872 0.4800 0.075 Uiso 1 1 calc R . . H71A H 0.5616 0.1422 0.5024 0.075 Uiso 1 1 calc R . . N31 N 0.70054(15) -0.03932(17) 0.5531(2) 0.0293(7) Uani 1 1 d . . . N32 N 0.66566(15) -0.06472(18) 0.5855(2) 0.0293(7) Uani 1 1 d . . . C31 C 0.67750(18) -0.0348(2) 0.6568(3) 0.0311(9) Uani 1 1 d . . . H31 H 0.7092 0.0041 0.6851 0.037 Uiso 1 1 calc R . . C32 C 0.64393(19) -0.0585(2) 0.6970(3) 0.0295(9) Uani 1 1 d . . . C33 C 0.65638(18) -0.0202(2) 0.7735(3) 0.0313(9) Uani 1 1 d . . . C34 C 0.6286(2) -0.0466(2) 0.8164(3) 0.0338(9) Uani 1 1 d . . . H34 H 0.6380 -0.0216 0.8691 0.041 Uiso 1 1 calc R . . C35 C 0.5874(2) -0.1087(2) 0.7831(3) 0.0375(10) Uani 1 1 d . . . H35 H 0.5689 -0.1265 0.8131 0.045 Uiso 1 1 calc R . . C36 C 0.5731(2) -0.1452(2) 0.7060(3) 0.0382(10) Uani 1 1 d . . . H36 H 0.5439 -0.1872 0.6823 0.046 Uiso 1 1 calc R . . C37 C 0.6009(2) -0.1206(2) 0.6636(3) 0.0381(10) Uani 1 1 d . . . H37 H 0.5908 -0.1461 0.6108 0.046 Uiso 1 1 calc R . . O3 O 0.69482(15) 0.04269(16) 0.80086(19) 0.0391(7) Uani 1 1 d . . . H3 H 0.7010 0.0595 0.8485 0.059 Uiso 1 1 calc R . . N21 N 0.65873(16) -0.15227(18) 0.4658(2) 0.0352(8) Uani 1 1 d . . . H21N H 0.6296 -0.1552 0.4774 0.042 Uiso 1 1 calc R . . N22 N 0.66316(15) -0.20797(18) 0.4169(2) 0.0326(8) Uani 1 1 d . . . C21 C 0.62628(19) -0.2666(2) 0.3934(3) 0.0339(9) Uani 1 1 d . . . H21 H 0.5980 -0.2701 0.4117 0.041 Uiso 1 1 calc R . . C22 C 0.62705(19) -0.3279(2) 0.3393(3) 0.0328(9) Uani 1 1 d . . . C23 C 0.6694(2) -0.3274(2) 0.3136(3) 0.0357(9) Uani 1 1 d . . . C24 C 0.6682(2) -0.3871(2) 0.2604(3) 0.0427(11) Uani 1 1 d . . . H24 H 0.6969 -0.3868 0.2427 0.051 Uiso 1 1 calc R . . C25 C 0.6244(3) -0.4472(2) 0.2335(3) 0.0484(12) Uani 1 1 d . . . H25 H 0.6232 -0.4878 0.1970 0.058 Uiso 1 1 calc R . . C26 C 0.5831(2) -0.4485(2) 0.2593(3) 0.0470(12) Uani 1 1 d . . . H26 H 0.5538 -0.4900 0.2413 0.056 Uiso 1 1 calc R . . C27 C 0.5843(2) -0.3897(2) 0.3108(3) 0.0388(10) Uani 1 1 d . . . H27 H 0.5552 -0.3908 0.3277 0.047 Uiso 1 1 calc R . . O2 O 0.71331(14) -0.27081(17) 0.3378(2) 0.0428(7) Uani 1 1 d . . . H2 H 0.7099 -0.2373 0.3686 0.064 Uiso 1 1 calc R . . N11 N 0.73787(15) -0.08542(19) 0.4687(2) 0.0301(7) Uani 1 1 d . . . N12 N 0.78105(15) -0.02525(18) 0.5144(2) 0.0275(7) Uani 1 1 d . . . C11 C 0.82566(19) -0.0184(2) 0.5013(3) 0.0323(9) Uani 1 1 d . . . H11 H 0.8263 -0.0545 0.4623 0.039 Uiso 1 1 calc R . . C12 C 0.87412(19) 0.0395(2) 0.5411(3) 0.0321(9) Uani 1 1 d . . . C13 C 0.87488(19) 0.1031(2) 0.5898(3) 0.0335(9) Uani 1 1 d . . . C14 C 0.9275(2) 0.1534(3) 0.6284(3) 0.0402(10) Uani 1 1 d . . . H14 H 0.9291 0.1968 0.6620 0.048 Uiso 1 1 calc R . . C15 C 0.9766(2) 0.1408(3) 0.6185(3) 0.0462(11) Uani 1 1 d . . . H15 H 1.0117 0.1752 0.6460 0.055 Uiso 1 1 calc R . . C16 C 0.9752(2) 0.0790(3) 0.5693(3) 0.0433(11) Uani 1 1 d . . . H16 H 1.0089 0.0709 0.5620 0.052 Uiso 1 1 calc R . . C17 C 0.9245(2) 0.0291(2) 0.5308(3) 0.0378(10) Uani 1 1 d . . . H17 H 0.9234 -0.0134 0.4964 0.045 Uiso 1 1 calc R . . O1 O 0.82992(13) 0.12172(16) 0.60242(19) 0.0373(7) Uani 1 1 d . . . OET O 0.51303(18) -0.17043(19) 0.4172(2) 0.0585(9) Uani 1 1 d . . . C90 C 0.5155(3) -0.0378(4) 0.3970(6) 0.131(4) Uani 1 1 d D . . H901 H 0.5606 -0.0370 0.4200 0.196 Uiso 1 1 calc R . . H902 H 0.5104 -0.0341 0.4465 0.196 Uiso 1 1 calc R . . H903 H 0.4944 0.0064 0.3568 0.196 Uiso 1 1 calc R . . C91 C 0.4877(4) -0.1099(4) 0.3492(5) 0.111(3) Uani 1 1 d D . . H911 H 0.4997 -0.1198 0.3067 0.134 Uiso 1 1 calc R . . H912 H 0.4411 -0.1078 0.3161 0.134 Uiso 1 1 calc R . . C92 C 0.4766(2) -0.2344(4) 0.3702(4) 0.0653(16) Uani 1 1 d . . . H921 H 0.4855 -0.2504 0.3259 0.078 Uiso 1 1 calc R . . H923 H 0.4312 -0.2210 0.3383 0.078 Uiso 1 1 calc R . . C93 C 0.4914(3) -0.2978(3) 0.4319(4) 0.0721(18) Uani 1 1 d . . . H931 H 0.4796 -0.2829 0.4729 0.108 Uiso 1 1 calc R . . H932 H 0.5368 -0.3088 0.4656 0.108 Uiso 1 1 calc R . . H933 H 0.4678 -0.3444 0.3989 0.108 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 0.0312(2) 0.02672(19) 0.0353(2) -0.00161(12) 0.02145(16) -0.00099(12) P1 0.0316(5) 0.0274(5) 0.0324(5) 0.0004(4) 0.0196(5) -0.0002(4) C1 0.027(2) 0.028(2) 0.031(2) 0.0022(16) 0.0144(18) 0.0028(16) C60 0.038(2) 0.036(2) 0.035(2) 0.0017(18) 0.021(2) 0.0023(18) C61 0.038(2) 0.037(2) 0.046(3) -0.006(2) 0.017(2) -0.0046(19) C50 0.044(2) 0.034(2) 0.045(2) 0.0042(19) 0.031(2) 0.0001(19) C51 0.053(3) 0.027(2) 0.054(3) -0.0015(19) 0.031(2) 0.000(2) C70 0.033(2) 0.031(2) 0.041(2) 0.0002(18) 0.0222(19) -0.0005(17) C71 0.038(3) 0.049(3) 0.051(3) 0.001(2) 0.018(2) 0.006(2) N31 0.0326(18) 0.0242(17) 0.0360(18) -0.0032(14) 0.0223(16) -0.0012(13) N32 0.0285(17) 0.0295(17) 0.0344(19) 0.0000(14) 0.0204(16) 0.0001(13) C31 0.028(2) 0.024(2) 0.039(2) 0.0019(17) 0.0171(19) -0.0006(16) C32 0.030(2) 0.026(2) 0.037(2) 0.0052(16) 0.0218(19) 0.0040(16) C33 0.028(2) 0.025(2) 0.036(2) 0.0030(17) 0.0151(18) -0.0021(16) C34 0.037(2) 0.034(2) 0.036(2) 0.0019(17) 0.024(2) 0.0012(18) C35 0.036(2) 0.036(2) 0.046(3) 0.0096(19) 0.026(2) 0.0024(19) C36 0.041(2) 0.026(2) 0.052(3) -0.0009(19) 0.029(2) -0.0047(18) C37 0.042(2) 0.028(2) 0.047(3) -0.0057(18) 0.027(2) -0.0007(18) O3 0.0453(18) 0.0425(17) 0.0356(16) -0.0050(13) 0.0264(15) -0.0123(14) N21 0.0345(19) 0.0323(19) 0.043(2) -0.0076(15) 0.0246(17) -0.0035(15) N22 0.0340(18) 0.0260(17) 0.0352(18) -0.0029(14) 0.0178(16) 0.0012(15) C21 0.033(2) 0.033(2) 0.034(2) 0.0020(17) 0.0179(19) -0.0001(18) C22 0.035(2) 0.026(2) 0.032(2) 0.0011(17) 0.0151(18) 0.0006(17) C23 0.038(2) 0.028(2) 0.038(2) 0.0030(18) 0.019(2) 0.0000(18) C24 0.050(3) 0.037(2) 0.045(3) 0.007(2) 0.030(2) 0.011(2) C25 0.066(3) 0.030(2) 0.041(3) -0.0036(19) 0.025(3) -0.001(2) C26 0.049(3) 0.035(2) 0.038(2) 0.0005(19) 0.012(2) -0.008(2) C27 0.040(2) 0.034(2) 0.036(2) 0.0017(18) 0.017(2) -0.0037(19) O2 0.0465(18) 0.0352(17) 0.059(2) -0.0065(14) 0.0367(17) -0.0061(14) N11 0.0295(17) 0.0299(17) 0.0321(18) 0.0003(14) 0.0181(16) 0.0009(14) N12 0.0280(17) 0.0236(16) 0.0305(17) 0.0013(13) 0.0161(15) 0.0020(13) C11 0.035(2) 0.028(2) 0.036(2) 0.0015(17) 0.0216(19) 0.0061(17) C12 0.030(2) 0.031(2) 0.037(2) 0.0081(17) 0.0207(19) 0.0038(17) C13 0.034(2) 0.033(2) 0.038(2) 0.0044(18) 0.023(2) -0.0003(18) C14 0.039(2) 0.037(2) 0.048(3) 0.0007(19) 0.027(2) -0.0052(19) C15 0.038(2) 0.040(3) 0.063(3) 0.003(2) 0.030(2) -0.005(2) C16 0.039(3) 0.042(3) 0.063(3) 0.008(2) 0.037(2) 0.002(2) C17 0.044(3) 0.032(2) 0.046(3) 0.0039(19) 0.030(2) 0.0037(19) O1 0.0393(16) 0.0314(15) 0.0494(18) -0.0069(13) 0.0298(15) -0.0066(13) OET 0.073(2) 0.0411(19) 0.078(2) 0.0207(18) 0.053(2) 0.0102(18) C90 0.050(4) 0.074(5) 0.189(10) 0.023(5) 0.018(5) 0.010(4) C91 0.082(5) 0.105(6) 0.124(7) 0.029(5) 0.043(5) 0.016(5) C92 0.041(3) 0.100(5) 0.061(3) -0.002(3) 0.033(3) 0.000(3) C93 0.106(5) 0.058(3) 0.089(4) -0.024(3) 0.077(4) -0.030(3) _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 Pd1 N12 1.988(3) . ? Pd1 O1 1.998(3) . ? Pd1 N31 2.025(3) . ? Pd1 P1 2.3085(11) . ? P1 C50 1.815(4) . ? P1 C70 1.825(4) . ? P1 C60 1.829(4) . ? C1 N11 1.320(5) . ? C1 N31 1.354(5) . ? C1 N21 1.368(5) . ? C60 C61 1.521(6) . ? C60 H60B 0.9900 . ? C60 H60A 0.9900 . ? C61 H61C 0.9800 . ? C61 H61B 0.9800 . ? C61 H61A 0.9800 . ? C50 C51 1.527(6) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51B 0.9800 . ? C51 H51A 0.9800 . ? C51 H51C 0.9800 . ? C70 C71 1.506(6) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C71 H71A 0.9800 . ? N31 N32 1.384(4) . ? N32 C31 1.264(5) . ? C31 C32 1.459(6) . ? C31 H31 0.9500 . ? C32 C37 1.404(6) . ? C32 C33 1.404(6) . ? C33 O3 1.354(5) . ? C33 C34 1.392(6) . ? C34 C35 1.377(6) . ? C34 H34 0.9500 . ? C35 C36 1.385(6) . ? C35 H35 0.9500 . ? C36 C37 1.374(6) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? O3 H3 0.8400 . ? N21 N22 1.353(4) . ? N21 H21N 0.8800 . ? N22 C21 1.279(5) . ? C21 C22 1.448(5) . ? C21 H21 0.9500 . ? C22 C27 1.398(6) . ? C22 C23 1.398(6) . ? C23 O2 1.358(5) . ? C23 C24 1.397(6) . ? C24 C25 1.395(6) . ? C24 H24 0.9500 . ? C25 C26 1.373(7) . ? C25 H25 0.9500 . ? C26 C27 1.366(6) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? O2 H2 0.8400 . ? N11 N12 1.397(4) . ? N12 C11 1.293(5) . ? C11 C12 1.429(6) . ? C11 H11 0.9500 . ? C12 C13 1.400(6) . ? C12 C17 1.412(6) . ? C13 O1 1.329(5) . ? C13 C14 1.410(6) . ? C14 C15 1.379(6) . ? C14 H14 0.9500 . ? C15 C16 1.377(6) . ? C15 H15 0.9500 . ? C16 C17 1.374(6) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? OET C92 1.384(6) . ? OET C91 1.461(8) . ? C90 C91 1.4489(11) . ? C90 H901 0.9800 . ? C90 H902 0.9800 . ? C90 H903 0.9800 . ? C91 H911 0.9900 . ? C91 H912 0.9900 . ? C92 C93 1.454(8) . ? C92 H921 0.9900 . ? C92 H923 0.9900 . ? C93 H931 0.9800 . ? C93 H932 0.9800 . ? C93 H933 0.9800 . ? 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 N12 Pd1 O1 92.27(12) . . ? N12 Pd1 N31 78.09(12) . . ? O1 Pd1 N31 170.09(12) . . ? N12 Pd1 P1 170.34(9) . . ? O1 Pd1 P1 84.43(8) . . ? N31 Pd1 P1 105.46(9) . . ? C50 P1 C70 103.82(19) . . ? C50 P1 C60 106.3(2) . . ? C70 P1 C60 103.46(19) . . ? C50 P1 Pd1 106.66(14) . . ? C70 P1 Pd1 119.74(14) . . ? C60 P1 Pd1 115.61(14) . . ? N11 C1 N31 122.9(3) . . ? N11 C1 N21 117.5(3) . . ? N31 C1 N21 119.5(3) . . ? C61 C60 P1 112.8(3) . . ? C61 C60 H60B 109.0 . . ? P1 C60 H60B 109.0 . . ? C61 C60 H60A 109.0 . . ? P1 C60 H60A 109.0 . . ? H60B C60 H60A 107.8 . . ? C60 C61 H61C 109.5 . . ? C60 C61 H61B 109.5 . . ? H61C C61 H61B 109.5 . . ? C60 C61 H61A 109.5 . . ? H61C C61 H61A 109.5 . . ? H61B C61 H61A 109.5 . . ? C51 C50 P1 116.7(3) . . ? C51 C50 H50A 108.1 . . ? P1 C50 H50A 108.1 . . ? C51 C50 H50B 108.1 . . ? P1 C50 H50B 108.1 . . ? H50A C50 H50B 107.3 . . ? C50 C51 H51B 109.5 . . ? C50 C51 H51A 109.5 . . ? H51B C51 H51A 109.5 . . ? C50 C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? C71 C70 P1 113.6(3) . . ? C71 C70 H70A 108.8 . . ? P1 C70 H70A 108.8 . . ? C71 C70 H70B 108.8 . . ? P1 C70 H70B 108.8 . . ? H70A C70 H70B 107.7 . . ? C70 C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C71 H71A 109.5 . . ? H71B C71 H71A 109.5 . . ? H71C C71 H71A 109.5 . . ? C1 N31 N32 112.3(3) . . ? C1 N31 Pd1 110.9(2) . . ? N32 N31 Pd1 136.1(2) . . ? C31 N32 N31 117.8(3) . . ? N32 C31 C32 121.9(4) . . ? N32 C31 H31 119.0 . . ? C32 C31 H31 119.0 . . ? C37 C32 C33 118.3(4) . . ? C37 C32 C31 122.1(4) . . ? C33 C32 C31 119.6(3) . . ? O3 C33 C34 123.1(4) . . ? O3 C33 C32 117.0(3) . . ? C34 C33 C32 119.9(4) . . ? C35 C34 C33 120.6(4) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 120.0(4) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C37 C36 C35 120.1(4) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C32 121.1(4) . . ? C36 C37 H37 119.5 . . ? C32 C37 H37 119.5 . . ? C33 O3 H3 109.5 . . ? N22 N21 C1 118.9(3) . . ? N22 N21 H21N 120.6 . . ? C1 N21 H21N 120.6 . . ? C21 N22 N21 117.4(3) . . ? N22 C21 C22 120.8(4) . . ? N22 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C27 C22 C23 118.1(4) . . ? C27 C22 C21 119.9(4) . . ? C23 C22 C21 121.9(4) . . ? O2 C23 C24 116.4(4) . . ? O2 C23 C22 123.3(4) . . ? C24 C23 C22 120.3(4) . . ? C25 C24 C23 119.2(4) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C26 C25 C24 120.8(4) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C27 C26 C25 119.7(4) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C22 121.9(4) . . ? C26 C27 H27 119.1 . . ? C22 C27 H27 119.1 . . ? C23 O2 H2 109.5 . . ? C1 N11 N12 109.2(3) . . ? C11 N12 N11 116.2(3) . . ? C11 N12 Pd1 126.4(3) . . ? N11 N12 Pd1 116.9(2) . . ? N12 C11 C12 125.0(4) . . ? N12 C11 H11 117.5 . . ? C12 C11 H11 117.5 . . ? C13 C12 C17 119.5(4) . . ? C13 C12 C11 124.4(4) . . ? C17 C12 C11 116.1(4) . . ? O1 C13 C12 126.0(4) . . ? O1 C13 C14 116.2(4) . . ? C12 C13 C14 117.8(4) . . ? C15 C14 C13 121.4(4) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C16 C15 C14 120.7(4) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C17 C16 C15 119.1(4) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C12 121.5(4) . . ? C16 C17 H17 119.3 . . ? C12 C17 H17 119.3 . . ? C13 O1 Pd1 123.6(2) . . ? C92 OET C91 102.5(4) . . ? C91 C90 H901 109.5 . . ? C91 C90 H902 109.5 . . ? H901 C90 H902 109.5 . . ? C91 C90 H903 109.5 . . ? H901 C90 H903 109.5 . . ? H902 C90 H903 109.5 . . ? C90 C91 OET 105.3(6) . . ? C90 C91 H911 110.7 . . ? OET C91 H911 110.7 . . ? C90 C91 H912 110.7 . . ? OET C91 H912 110.7 . . ? H911 C91 H912 108.8 . . ? OET C92 C93 108.9(5) . . ? OET C92 H921 109.9 . . ? C93 C92 H921 109.9 . . ? OET C92 H923 109.9 . . ? C93 C92 H923 109.9 . . ? H921 C92 H923 108.3 . . ? C92 C93 H931 109.5 . . ? C92 C93 H932 109.5 . . ? H931 C93 H932 109.5 . . ? C92 C93 H933 109.5 . . ? H931 C93 H933 109.5 . . ? H932 C93 H933 109.5 . . ? 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 N12 Pd1 P1 C50 -31.0(6) . . . . ? O1 Pd1 P1 C50 39.38(18) . . . . ? N31 Pd1 P1 C50 -141.39(18) . . . . ? N12 Pd1 P1 C70 86.3(6) . . . . ? O1 Pd1 P1 C70 156.65(18) . . . . ? N31 Pd1 P1 C70 -24.12(18) . . . . ? N12 Pd1 P1 C60 -148.9(6) . . . . ? O1 Pd1 P1 C60 -78.52(18) . . . . ? N31 Pd1 P1 C60 100.71(18) . . . . ? C50 P1 C60 C61 -62.2(3) . . . . ? C70 P1 C60 C61 -171.3(3) . . . . ? Pd1 P1 C60 C61 55.9(3) . . . . ? C70 P1 C50 C51 55.7(4) . . . . ? C60 P1 C50 C51 -53.1(4) . . . . ? Pd1 P1 C50 C51 -177.0(3) . . . . ? C50 P1 C70 C71 70.9(3) . . . . ? C60 P1 C70 C71 -178.2(3) . . . . ? Pd1 P1 C70 C71 -47.8(3) . . . . ? N11 C1 N31 N32 -169.2(3) . . . . ? N21 C1 N31 N32 12.2(5) . . . . ? N11 C1 N31 Pd1 2.7(5) . . . . ? N21 C1 N31 Pd1 -175.9(3) . . . . ? N12 Pd1 N31 C1 -8.2(3) . . . . ? O1 Pd1 N31 C1 -21.9(9) . . . . ? P1 Pd1 N31 C1 162.5(2) . . . . ? N12 Pd1 N31 N32 161.0(4) . . . . ? O1 Pd1 N31 N32 147.3(6) . . . . ? P1 Pd1 N31 N32 -28.3(4) . . . . ? C1 N31 N32 C31 158.6(3) . . . . ? Pd1 N31 N32 C31 -10.5(5) . . . . ? N31 N32 C31 C32 -179.2(3) . . . . ? N32 C31 C32 C37 6.1(6) . . . . ? N32 C31 C32 C33 -176.3(4) . . . . ? C37 C32 C33 O3 -175.8(4) . . . . ? C31 C32 C33 O3 6.6(5) . . . . ? C37 C32 C33 C34 3.0(6) . . . . ? C31 C32 C33 C34 -174.6(4) . . . . ? O3 C33 C34 C35 176.8(4) . . . . ? C32 C33 C34 C35 -1.9(6) . . . . ? C33 C34 C35 C36 -0.4(6) . . . . ? C34 C35 C36 C37 1.4(6) . . . . ? C35 C36 C37 C32 -0.2(6) . . . . ? C33 C32 C37 C36 -2.0(6) . . . . ? C31 C32 C37 C36 175.6(4) . . . . ? N11 C1 N21 N22 7.8(5) . . . . ? N31 C1 N21 N22 -173.5(3) . . . . ? C1 N21 N22 C21 175.7(3) . . . . ? N21 N22 C21 C22 178.6(3) . . . . ? N22 C21 C22 C27 -176.9(4) . . . . ? N22 C21 C22 C23 2.7(6) . . . . ? C27 C22 C23 O2 -179.5(4) . . . . ? C21 C22 C23 O2 0.9(6) . . . . ? C27 C22 C23 C24 0.4(6) . . . . ? C21 C22 C23 C24 -179.2(4) . . . . ? O2 C23 C24 C25 179.7(4) . . . . ? C22 C23 C24 C25 -0.2(6) . . . . ? C23 C24 C25 C26 -0.5(7) . . . . ? C24 C25 C26 C27 0.9(7) . . . . ? C25 C26 C27 C22 -0.7(7) . . . . ? C23 C22 C27 C26 0.0(6) . . . . ? C21 C22 C27 C26 179.6(4) . . . . ? N31 C1 N11 N12 7.6(5) . . . . ? N21 C1 N11 N12 -173.8(3) . . . . ? C1 N11 N12 C11 172.3(3) . . . . ? C1 N11 N12 Pd1 -14.9(4) . . . . ? O1 Pd1 N12 C11 2.8(3) . . . . ? N31 Pd1 N12 C11 -174.9(3) . . . . ? P1 Pd1 N12 C11 72.6(7) . . . . ? O1 Pd1 N12 N11 -169.3(3) . . . . ? N31 Pd1 N12 N11 13.1(2) . . . . ? P1 Pd1 N12 N11 -99.5(6) . . . . ? N11 N12 C11 C12 179.5(3) . . . . ? Pd1 N12 C11 C12 7.4(6) . . . . ? N12 C11 C12 C13 -9.4(6) . . . . ? N12 C11 C12 C17 169.3(4) . . . . ? C17 C12 C13 O1 177.6(4) . . . . ? C11 C12 C13 O1 -3.8(7) . . . . ? C17 C12 C13 C14 -1.4(6) . . . . ? C11 C12 C13 C14 177.1(4) . . . . ? O1 C13 C14 C15 -178.9(4) . . . . ? C12 C13 C14 C15 0.3(6) . . . . ? C13 C14 C15 C16 0.9(7) . . . . ? C14 C15 C16 C17 -0.8(7) . . . . ? C15 C16 C17 C12 -0.4(7) . . . . ? C13 C12 C17 C16 1.6(6) . . . . ? C11 C12 C17 C16 -177.1(4) . . . . ? C12 C13 O1 Pd1 16.4(6) . . . . ? C14 C13 O1 Pd1 -164.5(3) . . . . ? N12 Pd1 O1 C13 -14.0(3) . . . . ? N31 Pd1 O1 C13 -0.6(9) . . . . ? P1 Pd1 O1 C13 175.1(3) . . . . ? C92 OET C91 C90 169.5(6) . . . . ? C91 OET C92 C93 -173.3(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.626 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.088 _database_code_depnum_ccdc_archive 'CCDC 942798' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_10-[(pdpet3)h2br3l'] # begin Validation Reply Form _vrf_PLAT971_I ; PROBLEM: Large Calcd. Non-Metal Positive Residual Density 5.13 eA-3 RESPONSE: Our structure model does not contain major voids. Tentative assignment of a potential aqua oxygen atom to the residual density maximum resulted in a very high displacement parameter and did not give an acceptable geometry. Reliability factors did not improve, neither. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; (2,4-Dihydro-5-(5-bromo-2-hydroxyphenyl)-4-((5-bromo-2-hydroxyphenyl) methyleneamino)-1,2,4-triazol-3-ylidene 5-bromo-2-oxybenzaldehyde hydrazono)-(triethylphosphine)-palladium(ii) ; _chemical_name_common "[Pd(PEt3)H2Br3L']" _chemical_formula_moiety ? _chemical_formula_sum 'C28 H28 Br3 N6 O3 P1 Pd1' _chemical_formula_weight 873.63 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' Br Br -0.2901 2.4595 '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' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 21' _space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.2940(8) _cell_length_b 20.8512(14) _cell_length_c 14.0096(10) _cell_angle_alpha 90.00 _cell_angle_beta 111.9570(10) _cell_angle_gamma 90.00 _cell_volume 3059.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6611 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 24.57 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 4.618 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2595 _exptl_absorpt_correction_T_max 0.5641 _exptl_absorpt_process_details 'SADABS Medium Absorber' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42613 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.0789 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.68 _reflns_number_total 15386 _reflns_number_gt 13496 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0932P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.178(7) _refine_ls_number_reflns 15386 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0672 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1448 _refine_ls_wR_factor_gt 0.1383 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.020 _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 Pd1 Pd 0.54028(5) 0.19120(2) 0.87021(4) 0.01222(11) Uani 1 1 d . . . Br3 Br 0.78825(8) -0.09478(4) 0.46002(7) 0.02803(19) Uani 1 1 d . . . P1 P 0.33492(17) 0.21217(9) 0.76842(15) 0.0165(4) Uani 1 1 d . . . C70 C 0.3044(8) 0.2215(5) 0.6312(6) 0.029(2) Uani 1 1 d . . . H70B H 0.3544 0.2586 0.6230 0.035 Uiso 1 1 calc R . . H70A H 0.3371 0.1829 0.6079 0.035 Uiso 1 1 calc R . . C71 C 0.1648(8) 0.2312(5) 0.5599(7) 0.035(2) Uani 1 1 d . . . H71A H 0.1137 0.1949 0.5669 0.052 Uiso 1 1 calc R . . H71C H 0.1590 0.2341 0.4885 0.052 Uiso 1 1 calc R . . H71B H 0.1324 0.2709 0.5787 0.052 Uiso 1 1 calc R . . C74 C 0.2320(8) 0.1466(4) 0.7778(7) 0.0268(17) Uani 1 1 d . . . H74A H 0.1450 0.1529 0.7256 0.032 Uiso 1 1 calc R . . H74B H 0.2653 0.1055 0.7628 0.032 Uiso 1 1 calc R . . C75 C 0.2252(10) 0.1432(5) 0.8827(7) 0.036(2) Uani 1 1 d . . . H75C H 0.3106 0.1497 0.9353 0.054 Uiso 1 1 calc R . . H75B H 0.1930 0.1010 0.8922 0.054 Uiso 1 1 calc R . . H75A H 0.1676 0.1766 0.8890 0.054 Uiso 1 1 calc R . . C72 C 0.2749(8) 0.2849(4) 0.8088(7) 0.0270(18) Uani 1 1 d . . . H72A H 0.1862 0.2932 0.7611 0.032 Uiso 1 1 calc R . . H72B H 0.2744 0.2786 0.8786 0.032 Uiso 1 1 calc R . . C73 C 0.3550(7) 0.3400(4) 0.8090(8) 0.034(2) Uani 1 1 d . . . H73A H 0.4266 0.3424 0.8755 0.051 Uiso 1 1 calc R . . H73B H 0.3042 0.3794 0.7979 0.051 Uiso 1 1 calc R . . H73C H 0.3879 0.3351 0.7539 0.051 Uiso 1 1 calc R . . C1 C 0.7098(6) 0.1139(3) 0.8243(5) 0.0110(12) Uiso 1 1 d . . . N21 N 0.7388(5) 0.0763(3) 0.7538(4) 0.0112(11) Uani 1 1 d . . . N22 N 0.8496(5) 0.0446(3) 0.7655(5) 0.0161(12) Uani 1 1 d . . . C21 C 0.9234(6) 0.0290(3) 0.8585(5) 0.0119(13) Uani 1 1 d . . . H21 H 0.9003 0.0408 0.9147 0.014 Uiso 1 1 calc R . . C22 C 1.0405(6) -0.0063(3) 0.8775(5) 0.0117(13) Uani 1 1 d . . . C23 C 1.0914(7) -0.0163(4) 0.8011(6) 0.0167(14) Uani 1 1 d . . . C24 C 1.2043(7) -0.0495(4) 0.8254(5) 0.0199(16) Uani 1 1 d . . . H24 H 1.2376 -0.0574 0.7734 0.024 Uiso 1 1 calc R . . C25 C 1.2698(7) -0.0716(4) 0.9240(6) 0.0184(15) Uani 1 1 d . . . H25 H 1.3472 -0.0947 0.9397 0.022 Uiso 1 1 calc R . . C26 C 1.2217(7) -0.0596(4) 1.0007(6) 0.0205(15) Uani 1 1 d . . . C27 C 1.1058(7) -0.0294(3) 0.9763(5) 0.0161(14) Uani 1 1 d . . . H27 H 1.0700 -0.0244 1.0274 0.019 Uiso 1 1 calc R . . O2 O 1.0359(5) 0.0063(3) 0.7031(4) 0.0241(12) Uani 1 1 d . . . H2 H 0.9564 0.0076 0.6864 0.036 Uiso 1 1 calc R . . Br2 Br 1.30949(7) -0.08835(4) 1.13781(6) 0.02579(18) Uani 1 1 d . . . N31 N 0.5912(5) 0.1385(3) 0.7743(5) 0.0138(12) Uani 1 1 d . . . N32 N 0.5473(5) 0.1182(3) 0.6743(4) 0.0132(12) Uani 1 1 d . . . C31 C 0.6336(6) 0.0824(3) 0.6608(5) 0.0145(14) Uani 1 1 d . . . C32 C 0.6185(7) 0.0511(3) 0.5630(5) 0.0156(14) Uani 1 1 d . . . C33 C 0.5177(7) 0.0700(3) 0.4731(5) 0.0143(13) Uani 1 1 d . . . C35 C 0.5812(7) -0.0082(4) 0.3729(6) 0.0188(15) Uani 1 1 d . . . H35 H 0.5725 -0.0274 0.3092 0.023 Uiso 1 1 calc R . . C36 C 0.6775(7) -0.0271(4) 0.4648(6) 0.0186(15) Uani 1 1 d . . . C37 C 0.6967(7) 0.0004(4) 0.5565(6) 0.0185(15) Uani 1 1 d . . . H37 H 0.7634 -0.0146 0.6168 0.022 Uiso 1 1 calc R . . O3 O 0.4330(5) 0.1163(3) 0.4727(4) 0.0211(11) Uani 1 1 d . . . H3 H 0.4431 0.1257 0.5336 0.032 Uiso 1 1 calc R . . N11 N 0.7861(6) 0.1250(3) 0.9216(5) 0.0148(12) Uani 1 1 d . . . N12 N 0.7210(6) 0.1674(3) 0.9609(5) 0.0140(12) Uani 1 1 d . . . C11 C 0.7808(6) 0.1866(4) 1.0556(5) 0.0157(13) Uani 1 1 d . . . H11 H 0.8649 0.1709 1.0913 0.019 Uiso 1 1 calc R . . C12 C 0.7283(7) 0.2294(3) 1.1091(6) 0.0157(14) Uani 1 1 d . . . C13 C 0.6008(6) 0.2546(3) 1.0693(6) 0.0147(14) Uani 1 1 d . . . C14 C 0.5654(7) 0.2958(3) 1.1324(6) 0.0161(14) Uani 1 1 d . . . H14 H 0.4803 0.3114 1.1086 0.019 Uiso 1 1 calc R . . C15 C 0.6487(7) 0.3146(4) 1.2275(6) 0.0196(15) Uani 1 1 d . . . H15 H 0.6216 0.3437 1.2675 0.024 Uiso 1 1 calc R . . C16 C 0.7733(7) 0.2910(4) 1.2655(5) 0.0155(14) Uani 1 1 d . . . C17 C 0.8098(7) 0.2483(4) 1.2060(6) 0.0185(15) Uani 1 1 d . . . H17 H 0.8940 0.2314 1.2326 0.022 Uiso 1 1 calc R . . O1 O 0.5107(5) 0.2393(3) 0.9813(4) 0.0192(11) Uani 1 1 d . . . Br1 Br 0.89013(8) 0.31895(4) 1.39505(6) 0.02522(17) Uani 1 1 d . . . Pd2 Pd 0.79865(5) 0.04319(2) 0.21417(4) 0.01112(11) Uani 1 1 d . . . P2 P 1.00813(16) 0.02922(8) 0.31625(14) 0.0126(3) Uani 1 1 d . . . C80 C 1.0457(7) 0.0328(4) 0.4537(5) 0.0190(15) Uani 1 1 d . . . H80B H 1.0279 0.0768 0.4714 0.023 Uiso 1 1 calc R . . H80A H 0.9875 0.0034 0.4706 0.023 Uiso 1 1 calc R . . C81 C 1.1846(8) 0.0154(5) 0.5225(6) 0.0287(18) Uani 1 1 d . . . H81A H 1.2038 -0.0281 0.5062 0.043 Uiso 1 1 calc R . . H81B H 1.1947 0.0175 0.5950 0.043 Uiso 1 1 calc R . . H81C H 1.2433 0.0458 0.5100 0.043 Uiso 1 1 calc R . . C82 C 1.1039(8) 0.0929(4) 0.2910(7) 0.0227(16) Uani 1 1 d . . . H82B H 1.0685 0.1350 0.2991 0.027 Uiso 1 1 calc R . . H82A H 1.1924 0.0903 0.3423 0.027 Uiso 1 1 calc R . . C83 C 1.1064(9) 0.0880(4) 0.1808(7) 0.0292(19) Uani 1 1 d . . . H83A H 1.1546 0.0498 0.1762 0.044 Uiso 1 1 calc R . . H83B H 1.1474 0.1263 0.1666 0.044 Uiso 1 1 calc R . . H83C H 1.0189 0.0849 0.1302 0.044 Uiso 1 1 calc R . . C84 C 1.0746(7) -0.0457(4) 0.2908(6) 0.0189(15) Uani 1 1 d . . . H84B H 1.0577 -0.0482 0.2163 0.023 Uiso 1 1 calc R . . H84A H 1.1683 -0.0449 0.3280 0.023 Uiso 1 1 calc R . . C85 C 1.0218(10) -0.1053(4) 0.3221(7) 0.035(2) Uani 1 1 d . . . H85B H 1.0359 -0.1029 0.3954 0.053 Uiso 1 1 calc R . . H85A H 1.0652 -0.1432 0.3095 0.053 Uiso 1 1 calc R . . H85C H 0.9300 -0.1085 0.2816 0.053 Uiso 1 1 calc R . . C2 C 0.6287(6) 0.1261(3) 0.2503(5) 0.0106(12) Uani 1 1 d . . . N52 N 0.4903(5) 0.1991(3) 0.3077(4) 0.0107(11) Uani 1 1 d . . . C53 C 0.2557(7) 0.2616(3) 0.2871(6) 0.0165(14) Uani 1 1 d . . . N61 N 0.7515(5) 0.1052(3) 0.3010(4) 0.0120(11) Uani 1 1 d . . . N62 N 0.7990(5) 0.1302(3) 0.3975(4) 0.0104(11) Uani 1 1 d . . . C62 C 0.7281(6) 0.2034(3) 0.5028(5) 0.0141(14) Uani 1 1 d . . . C63 C 0.8214(6) 0.1808(3) 0.5972(5) 0.0136(13) Uani 1 1 d . . . C64 C 0.8421(7) 0.2060(3) 0.6964(5) 0.0141(13) Uiso 1 1 d . . . H64 H 0.9038 0.1901 0.7587 0.017 Uiso 1 1 calc R . . O6 O 0.9007(5) 0.1313(2) 0.6013(4) 0.0144(10) Uani 1 1 d . . . H6 H 0.8910 0.1201 0.5412 0.022 Uiso 1 1 calc R . . N41 N 0.5515(5) 0.1090(3) 0.1587(4) 0.0115(11) Uiso 1 1 d . . . N42 N 0.6165(5) 0.0657(3) 0.1214(5) 0.0131(11) Uani 1 1 d . . . C41 C 0.5599(6) 0.0455(4) 0.0275(5) 0.0155(13) Uani 1 1 d . . . H41 H 0.4758 0.0606 -0.0099 0.019 Uiso 1 1 calc R . . C42 C 0.6154(6) 0.0016(4) -0.0243(5) 0.0147(14) Uani 1 1 d . . . C43 C 0.7331(7) -0.0276(4) 0.0198(6) 0.0180(15) Uani 1 1 d . . . C45 C 0.6984(7) -0.0832(4) -0.1418(6) 0.0217(16) Uani 1 1 d . . . H45 H 0.7249 -0.1127 -0.1815 0.026 Uiso 1 1 calc R . . C46 C 0.5841(7) -0.0504(4) -0.1863(6) 0.0166(14) Uani 1 1 d . . . C47 C 0.5417(7) -0.0102(3) -0.1310(6) 0.0157(14) Uani 1 1 d . . . H47 H 0.4618 0.0107 -0.1631 0.019 Uiso 1 1 calc R . . O4 O 0.8217(5) -0.0189(3) 0.1146(4) 0.0196(11) Uani 1 1 d . . . Br4 Br 0.48856(8) -0.06215(4) -0.33007(6) 0.02247(16) Uani 1 1 d . . . C34 C 0.4972(7) 0.0408(4) 0.3783(5) 0.0163(13) Uani 1 1 d . . . H34 H 0.4278 0.0537 0.3182 0.020 Uiso 1 1 calc R . . C44 C 0.7730(7) -0.0731(4) -0.0405(6) 0.0202(16) Uani 1 1 d . . . H44 H 0.8510 -0.0959 -0.0098 0.024 Uiso 1 1 calc R . . N51 N 0.6037(5) 0.1682(3) 0.3169(4) 0.0129(11) Uani 1 1 d . . . C61 C 0.7117(6) 0.1694(3) 0.4077(5) 0.0120(13) Uani 1 1 d . . . C51 C 0.4057(7) 0.2039(3) 0.2178(6) 0.0167(14) Uani 1 1 d . . . H51 H 0.4187 0.1854 0.1605 0.020 Uiso 1 1 calc R . . C52 C 0.2865(6) 0.2388(3) 0.2042(5) 0.0115(13) Uani 1 1 d . . . C57 C 0.2018(7) 0.2492(4) 0.1041(5) 0.0176(15) Uani 1 1 d . . . H57 H 0.2208 0.2336 0.0478 0.021 Uiso 1 1 calc R . . C56 C 0.0897(7) 0.2824(3) 0.0866(6) 0.0194(15) Uani 1 1 d . . . C55 C 0.0612(7) 0.3079(4) 0.1646(7) 0.0240(17) Uani 1 1 d . . . H55 H -0.0159 0.3307 0.1522 0.029 Uiso 1 1 calc R . . Br5 Br -0.02591(8) 0.29442(4) -0.05135(7) 0.0315(2) Uani 1 1 d . . . C54 C 0.1515(8) 0.2986(4) 0.2642(6) 0.0241(17) Uani 1 1 d . . . H54 H 0.1382 0.3200 0.3192 0.029 Uiso 1 1 calc R . . C67 C 0.6561(6) 0.2571(3) 0.5057(5) 0.0153(14) Uani 1 1 d . . . H67 H 0.5964 0.2742 0.4434 0.018 Uiso 1 1 calc R . . C66 C 0.6706(7) 0.2855(3) 0.5981(5) 0.0139(13) Uiso 1 1 d . . . C65 C 0.7539(7) 0.2606(4) 0.6896(5) 0.0180(15) Uani 1 1 d . . . H65 H 0.7554 0.2793 0.7519 0.022 Uiso 1 1 calc R . . Br6 Br 0.57283(8) 0.36014(4) 0.59699(6) 0.02529(18) Uani 1 1 d . . . O5 O 0.3325(6) 0.2521(3) 0.3866(4) 0.0286(14) Uani 1 1 d . . . H5 H 0.3104 0.2184 0.4083 0.043 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 0.0077(2) 0.0140(2) 0.0139(2) 0.00056(19) 0.00276(18) 0.00194(19) Br3 0.0229(4) 0.0301(4) 0.0303(4) -0.0129(4) 0.0090(3) 0.0021(3) P1 0.0096(8) 0.0191(9) 0.0188(9) 0.0008(7) 0.0032(7) 0.0032(7) C70 0.020(4) 0.044(5) 0.019(4) 0.015(4) 0.004(3) 0.023(4) C71 0.020(4) 0.052(6) 0.019(4) 0.008(4) -0.008(3) -0.003(4) C74 0.025(4) 0.025(4) 0.029(4) -0.002(3) 0.007(3) -0.002(3) C75 0.042(5) 0.033(5) 0.035(5) 0.002(4) 0.016(4) -0.016(4) C72 0.020(4) 0.025(4) 0.029(4) 0.003(3) 0.002(3) 0.015(3) C73 0.012(4) 0.037(5) 0.044(5) 0.036(4) 0.001(4) 0.001(3) N21 0.009(3) 0.011(3) 0.010(3) -0.002(2) -0.001(2) 0.002(2) N22 0.012(3) 0.016(3) 0.023(3) -0.003(3) 0.010(2) -0.002(2) C21 0.014(3) 0.010(3) 0.012(3) 0.002(2) 0.006(3) 0.001(2) C22 0.007(3) 0.010(3) 0.014(3) 0.003(2) -0.001(2) 0.001(2) C23 0.009(3) 0.021(4) 0.017(3) 0.003(3) 0.001(3) 0.004(3) C24 0.022(4) 0.029(4) 0.011(3) 0.004(3) 0.007(3) 0.015(3) C25 0.012(3) 0.020(4) 0.019(4) 0.000(3) 0.001(3) 0.005(3) C26 0.020(4) 0.023(4) 0.014(3) -0.006(3) 0.001(3) 0.001(3) C27 0.022(4) 0.014(3) 0.010(3) -0.007(3) 0.002(3) 0.008(3) O2 0.021(3) 0.033(3) 0.017(3) 0.005(2) 0.005(2) 0.010(2) Br2 0.0179(4) 0.0335(4) 0.0183(4) 0.0042(3) -0.0021(3) 0.0062(3) N31 0.011(3) 0.014(3) 0.014(3) -0.004(2) 0.002(2) 0.000(2) N32 0.013(3) 0.016(3) 0.006(3) 0.002(2) -0.002(2) -0.004(2) C31 0.010(3) 0.017(3) 0.012(3) 0.006(3) 0.000(3) 0.002(3) C32 0.014(3) 0.013(3) 0.017(3) -0.001(3) 0.003(3) -0.003(3) C33 0.014(3) 0.015(3) 0.012(3) -0.002(3) 0.004(3) -0.002(3) C35 0.017(3) 0.023(4) 0.014(3) -0.005(3) 0.002(3) -0.007(3) C36 0.015(3) 0.021(4) 0.022(4) -0.002(3) 0.010(3) -0.005(3) C37 0.018(4) 0.024(4) 0.012(3) 0.002(3) 0.004(3) -0.002(3) O3 0.020(3) 0.019(3) 0.016(3) 0.004(2) -0.002(2) 0.002(2) N11 0.015(3) 0.010(3) 0.020(3) 0.002(2) 0.007(2) 0.006(2) N12 0.017(3) 0.013(3) 0.014(3) 0.002(2) 0.008(2) 0.001(2) C11 0.006(3) 0.019(3) 0.021(3) -0.001(3) 0.004(3) 0.003(3) C12 0.017(3) 0.013(3) 0.017(3) 0.000(3) 0.007(3) 0.003(3) C13 0.009(3) 0.013(3) 0.024(4) 0.004(3) 0.008(3) 0.003(2) C14 0.013(3) 0.014(3) 0.025(4) 0.000(3) 0.010(3) -0.001(3) C15 0.023(4) 0.020(4) 0.019(4) -0.003(3) 0.012(3) 0.001(3) C16 0.016(3) 0.017(3) 0.012(3) -0.002(3) 0.005(3) 0.000(3) C17 0.014(3) 0.021(4) 0.024(4) 0.005(3) 0.012(3) 0.002(3) O1 0.013(2) 0.024(3) 0.020(3) -0.005(2) 0.005(2) 0.006(2) Br1 0.0225(4) 0.0307(4) 0.0199(4) -0.0090(3) 0.0050(3) -0.0001(3) Pd2 0.0075(2) 0.0113(2) 0.0131(2) -0.00129(19) 0.00229(18) 0.00042(18) P2 0.0076(7) 0.0134(9) 0.0150(8) -0.0003(6) 0.0020(6) 0.0018(6) C80 0.017(3) 0.031(4) 0.007(3) 0.000(3) 0.002(3) 0.007(3) C81 0.028(4) 0.035(5) 0.024(4) 0.007(4) 0.009(4) 0.006(4) C82 0.021(4) 0.019(4) 0.029(4) 0.000(3) 0.011(3) -0.002(3) C83 0.031(5) 0.022(4) 0.036(5) -0.002(4) 0.014(4) -0.008(3) C84 0.013(3) 0.019(4) 0.023(4) -0.005(3) 0.006(3) -0.001(3) C85 0.058(6) 0.018(4) 0.033(5) -0.008(4) 0.021(5) -0.018(4) C2 0.005(3) 0.010(3) 0.015(3) 0.004(2) 0.001(2) -0.001(2) N52 0.006(2) 0.011(3) 0.014(3) -0.002(2) 0.001(2) 0.001(2) C53 0.020(4) 0.014(3) 0.016(3) 0.006(3) 0.007(3) 0.003(3) N61 0.009(3) 0.013(3) 0.012(3) 0.004(2) 0.002(2) 0.002(2) N62 0.008(3) 0.012(3) 0.010(3) 0.000(2) 0.002(2) 0.001(2) C62 0.008(3) 0.018(4) 0.018(3) 0.004(3) 0.007(3) 0.005(2) C63 0.010(3) 0.010(3) 0.017(3) -0.002(3) 0.000(3) -0.002(2) O6 0.009(2) 0.014(2) 0.018(3) 0.0036(19) 0.0029(19) 0.0068(18) N42 0.014(3) 0.009(3) 0.017(3) -0.003(2) 0.007(2) -0.002(2) C41 0.010(3) 0.017(3) 0.015(3) 0.001(3) 0.001(3) 0.003(3) C42 0.013(3) 0.018(3) 0.015(3) 0.005(3) 0.008(3) 0.000(3) C43 0.013(3) 0.023(4) 0.021(4) 0.006(3) 0.009(3) 0.003(3) C45 0.023(4) 0.022(4) 0.024(4) -0.010(3) 0.013(3) -0.007(3) C46 0.009(3) 0.017(4) 0.019(3) 0.001(3) 0.000(3) -0.009(3) C47 0.014(3) 0.011(3) 0.019(4) -0.002(3) 0.004(3) -0.005(3) O4 0.011(2) 0.022(3) 0.022(3) -0.009(2) 0.002(2) 0.005(2) Br4 0.0304(4) 0.0219(4) 0.0147(3) -0.0016(3) 0.0080(3) -0.0072(3) C34 0.024(4) 0.013(3) 0.014(3) 0.002(3) 0.009(3) -0.003(3) C44 0.016(3) 0.026(4) 0.021(4) -0.004(3) 0.009(3) 0.006(3) N51 0.005(2) 0.014(3) 0.013(3) 0.004(2) -0.004(2) 0.004(2) C61 0.008(3) 0.013(3) 0.014(3) 0.002(2) 0.002(2) 0.001(2) C51 0.021(4) 0.010(3) 0.019(3) -0.002(3) 0.007(3) 0.001(3) C52 0.012(3) 0.012(3) 0.009(3) -0.001(2) 0.003(2) -0.003(2) C57 0.016(3) 0.018(4) 0.013(3) -0.006(3) -0.002(3) -0.001(3) C56 0.015(3) 0.013(3) 0.020(4) 0.004(3) -0.006(3) 0.000(3) C55 0.013(3) 0.018(4) 0.042(5) 0.009(3) 0.011(3) 0.003(3) Br5 0.0217(4) 0.0296(4) 0.0267(4) 0.0023(3) -0.0101(3) 0.0027(3) C54 0.039(5) 0.011(3) 0.013(3) 0.001(3) -0.002(3) 0.011(3) C67 0.011(3) 0.017(3) 0.013(3) 0.003(3) -0.001(3) 0.004(3) C65 0.020(4) 0.022(4) 0.007(3) -0.003(3) 0.001(3) 0.000(3) Br6 0.0244(4) 0.0291(4) 0.0176(4) -0.0058(3) 0.0024(3) 0.0113(3) O5 0.029(3) 0.044(4) 0.016(3) 0.010(3) 0.013(2) 0.013(3) _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 Pd1 N31 1.980(6) . ? Pd1 O1 1.982(5) . ? Pd1 N12 2.021(6) . ? Pd1 P1 2.2651(19) . ? Br3 C36 1.903(8) . ? P1 C74 1.831(9) . ? P1 C70 1.832(8) . ? P1 C72 1.834(8) . ? C70 C71 1.532(11) . ? C70 H70B 0.9900 . ? C70 H70A 0.9900 . ? C71 H71A 0.9800 . ? C71 H71C 0.9800 . ? C71 H71B 0.9800 . ? C74 C75 1.502(12) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 H75C 0.9800 . ? C75 H75B 0.9800 . ? C75 H75A 0.9800 . ? C72 C73 1.461(12) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C1 N11 1.332(9) . ? C1 N31 1.358(9) . ? C1 N21 1.393(9) . ? N21 N22 1.369(8) . ? N21 C31 1.403(8) . ? N22 C21 1.299(9) . ? C21 C22 1.449(9) . ? C21 H21 0.9500 . ? C22 C27 1.389(9) . ? C22 C23 1.406(10) . ? C23 O2 1.363(9) . ? C23 C24 1.377(10) . ? C24 C25 1.380(10) . ? C24 H24 0.9500 . ? C25 C26 1.395(11) . ? C25 H25 0.9500 . ? C26 C27 1.375(10) . ? C26 Br2 1.900(8) . ? C27 H27 0.9500 . ? O2 H2 0.8400 . ? N31 N32 1.367(8) . ? N32 C31 1.296(9) . ? C31 C32 1.470(10) . ? C32 C33 1.402(10) . ? C32 C37 1.402(10) . ? C33 O3 1.359(9) . ? C33 C34 1.400(10) . ? C35 C36 1.396(10) . ? C35 C34 1.414(11) . ? C35 H35 0.9500 . ? C36 C37 1.348(11) . ? C37 H37 0.9500 . ? O3 H3 0.8400 . ? N11 N12 1.389(8) . ? N12 C11 1.306(9) . ? C11 C12 1.429(10) . ? C11 H11 0.9500 . ? C12 C17 1.381(11) . ? C12 C13 1.436(9) . ? C13 O1 1.311(9) . ? C13 C14 1.394(10) . ? C14 C15 1.370(11) . ? C14 H14 0.9500 . ? C15 C16 1.396(10) . ? C15 H15 0.9500 . ? C16 C17 1.384(10) . ? C16 Br1 1.893(7) . ? C17 H17 0.9500 . ? Pd2 N61 1.980(6) . ? Pd2 O4 1.990(5) . ? Pd2 N42 2.035(6) . ? Pd2 P2 2.2797(18) . ? P2 C80 1.812(7) . ? P2 C84 1.824(8) . ? P2 C82 1.829(8) . ? C80 C81 1.547(10) . ? C80 H80B 0.9900 . ? C80 H80A 0.9900 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 C83 1.559(12) . ? C82 H82B 0.9900 . ? C82 H82A 0.9900 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 C85 1.513(11) . ? C84 H84B 0.9900 . ? C84 H84A 0.9900 . ? C85 H85B 0.9800 . ? C85 H85A 0.9800 . ? C85 H85C 0.9800 . ? C2 N41 1.303(9) . ? C2 N61 1.372(8) . ? C2 N51 1.384(9) . ? N52 C51 1.269(9) . ? N52 N51 1.397(8) . ? C53 C54 1.341(11) . ? C53 O5 1.353(9) . ? C53 C52 1.414(10) . ? N61 N62 1.359(8) . ? N62 C61 1.329(8) . ? C62 C67 1.392(9) . ? C62 C63 1.428(9) . ? C62 C61 1.458(10) . ? C63 O6 1.354(8) . ? C63 C64 1.421(10) . ? C64 C65 1.493(10) . ? C64 H64 0.9500 . ? O6 H6 0.8400 . ? N41 N42 1.384(8) . ? N42 C41 1.299(9) . ? C41 C42 1.448(10) . ? C41 H41 0.9500 . ? C42 C43 1.380(10) . ? C42 C47 1.435(10) . ? C43 O4 1.344(9) . ? C43 C44 1.451(10) . ? C45 C44 1.369(11) . ? C45 C46 1.385(11) . ? C45 H45 0.9500 . ? C46 C47 1.345(11) . ? C46 Br4 1.912(7) . ? C47 H47 0.9500 . ? C34 H34 0.9500 . ? C44 H44 0.9500 . ? N51 C61 1.395(8) . ? C51 C52 1.479(10) . ? C51 H51 0.9500 . ? C52 C57 1.387(9) . ? C57 C56 1.382(11) . ? C57 H57 0.9500 . ? C56 C55 1.357(12) . ? C56 Br5 1.902(7) . ? C55 C54 1.400(11) . ? C55 H55 0.9500 . ? C54 H54 0.9500 . ? C67 C66 1.378(10) . ? C67 H67 0.9500 . ? C66 C65 1.377(10) . ? C66 Br6 1.904(7) . ? C65 H65 0.9500 . ? O5 H5 0.8400 . ? 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 N31 Pd1 O1 172.1(2) . . ? N31 Pd1 N12 79.0(2) . . ? O1 Pd1 N12 93.3(2) . . ? N31 Pd1 P1 99.71(17) . . ? O1 Pd1 P1 87.87(16) . . ? N12 Pd1 P1 176.90(18) . . ? C74 P1 C70 106.2(4) . . ? C74 P1 C72 106.1(4) . . ? C70 P1 C72 106.8(4) . . ? C74 P1 Pd1 109.8(3) . . ? C70 P1 Pd1 115.3(3) . . ? C72 P1 Pd1 112.0(3) . . ? C71 C70 P1 116.2(6) . . ? C71 C70 H70B 108.2 . . ? P1 C70 H70B 108.2 . . ? C71 C70 H70A 108.2 . . ? P1 C70 H70A 108.2 . . ? H70B C70 H70A 107.4 . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? H71C C71 H71B 109.5 . . ? C75 C74 P1 111.9(6) . . ? C75 C74 H74A 109.2 . . ? P1 C74 H74A 109.2 . . ? C75 C74 H74B 109.2 . . ? P1 C74 H74B 109.2 . . ? H74A C74 H74B 107.9 . . ? C74 C75 H75C 109.5 . . ? C74 C75 H75B 109.5 . . ? H75C C75 H75B 109.5 . . ? C74 C75 H75A 109.5 . . ? H75C C75 H75A 109.5 . . ? H75B C75 H75A 109.5 . . ? C73 C72 P1 110.6(6) . . ? C73 C72 H72A 109.5 . . ? P1 C72 H72A 109.5 . . ? C73 C72 H72B 109.5 . . ? P1 C72 H72B 109.5 . . ? H72A C72 H72B 108.1 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? N11 C1 N31 126.8(6) . . ? N11 C1 N21 126.1(6) . . ? N31 C1 N21 107.1(6) . . ? N22 N21 C1 129.3(6) . . ? N22 N21 C31 125.0(6) . . ? C1 N21 C31 105.4(5) . . ? C21 N22 N21 117.1(6) . . ? N22 C21 C22 120.7(6) . . ? N22 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C27 C22 C23 119.4(6) . . ? C27 C22 C21 117.8(6) . . ? C23 C22 C21 122.7(6) . . ? O2 C23 C24 117.2(7) . . ? O2 C23 C22 123.4(6) . . ? C24 C23 C22 119.4(6) . . ? C23 C24 C25 121.0(7) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C24 C25 C26 119.6(7) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C27 C26 C25 119.9(7) . . ? C27 C26 Br2 118.9(6) . . ? C25 C26 Br2 121.0(6) . . ? C26 C27 C22 120.5(7) . . ? C26 C27 H27 119.8 . . ? C22 C27 H27 119.8 . . ? C23 O2 H2 109.5 . . ? C1 N31 N32 108.8(6) . . ? C1 N31 Pd1 109.9(4) . . ? N32 N31 Pd1 141.4(5) . . ? C31 N32 N31 108.9(5) . . ? N32 C31 N21 109.8(6) . . ? N32 C31 C32 124.1(6) . . ? N21 C31 C32 126.0(6) . . ? C33 C32 C37 118.2(7) . . ? C33 C32 C31 119.0(6) . . ? C37 C32 C31 122.6(6) . . ? O3 C33 C34 116.1(6) . . ? O3 C33 C32 122.5(6) . . ? C34 C33 C32 121.4(7) . . ? C36 C35 C34 117.5(7) . . ? C36 C35 H35 121.2 . . ? C34 C35 H35 121.2 . . ? C37 C36 C35 123.4(7) . . ? C37 C36 Br3 118.4(6) . . ? C35 C36 Br3 118.2(6) . . ? C36 C37 C32 120.1(7) . . ? C36 C37 H37 120.0 . . ? C32 C37 H37 120.0 . . ? C33 O3 H3 109.5 . . ? C1 N11 N12 106.2(5) . . ? C11 N12 N11 116.6(6) . . ? C11 N12 Pd1 125.5(5) . . ? N11 N12 Pd1 117.9(4) . . ? N12 C11 C12 124.4(6) . . ? N12 C11 H11 117.8 . . ? C12 C11 H11 117.8 . . ? C17 C12 C11 116.0(6) . . ? C17 C12 C13 118.7(7) . . ? C11 C12 C13 125.2(7) . . ? O1 C13 C14 116.1(6) . . ? O1 C13 C12 126.2(7) . . ? C14 C13 C12 117.5(7) . . ? C15 C14 C13 122.6(7) . . ? C15 C14 H14 118.7 . . ? C13 C14 H14 118.7 . . ? C14 C15 C16 119.8(7) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 118.9(7) . . ? C17 C16 Br1 121.2(5) . . ? C15 C16 Br1 119.9(5) . . ? C12 C17 C16 122.4(7) . . ? C12 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? C13 O1 Pd1 124.2(4) . . ? N61 Pd2 O4 172.4(2) . . ? N61 Pd2 N42 78.6(2) . . ? O4 Pd2 N42 93.9(2) . . ? N61 Pd2 P2 98.76(17) . . ? O4 Pd2 P2 88.82(15) . . ? N42 Pd2 P2 173.83(17) . . ? C80 P2 C84 107.1(4) . . ? C80 P2 C82 104.8(4) . . ? C84 P2 C82 105.5(4) . . ? C80 P2 Pd2 115.9(2) . . ? C84 P2 Pd2 113.1(2) . . ? C82 P2 Pd2 109.7(3) . . ? C81 C80 P2 115.6(5) . . ? C81 C80 H80B 108.4 . . ? P2 C80 H80B 108.4 . . ? C81 C80 H80A 108.4 . . ? P2 C80 H80A 108.4 . . ? H80B C80 H80A 107.4 . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C83 C82 P2 112.1(6) . . ? C83 C82 H82B 109.2 . . ? P2 C82 H82B 109.2 . . ? C83 C82 H82A 109.2 . . ? P2 C82 H82A 109.2 . . ? H82B C82 H82A 107.9 . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C85 C84 P2 114.3(6) . . ? C85 C84 H84B 108.7 . . ? P2 C84 H84B 108.7 . . ? C85 C84 H84A 108.7 . . ? P2 C84 H84A 108.7 . . ? H84B C84 H84A 107.6 . . ? C84 C85 H85B 109.5 . . ? C84 C85 H85A 109.5 . . ? H85B C85 H85A 109.5 . . ? C84 C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? N41 C2 N61 126.7(6) . . ? N41 C2 N51 127.4(6) . . ? N61 C2 N51 105.9(6) . . ? C51 N52 N51 116.9(6) . . ? C54 C53 O5 119.9(7) . . ? C54 C53 C52 117.4(7) . . ? O5 C53 C52 122.5(7) . . ? N62 N61 C2 109.8(5) . . ? N62 N61 Pd2 140.0(4) . . ? C2 N61 Pd2 110.0(5) . . ? C61 N62 N61 108.1(5) . . ? C67 C62 C63 118.4(6) . . ? C67 C62 C61 122.8(6) . . ? C63 C62 C61 118.8(6) . . ? O6 C63 C64 112.1(6) . . ? O6 C63 C62 122.6(6) . . ? C64 C63 C62 125.3(6) . . ? C63 C64 C65 111.0(6) . . ? C63 C64 H64 124.5 . . ? C65 C64 H64 124.5 . . ? C63 O6 H6 109.5 . . ? C2 N41 N42 107.2(5) . . ? C41 N42 N41 117.6(6) . . ? C41 N42 Pd2 124.8(5) . . ? N41 N42 Pd2 117.5(4) . . ? N42 C41 C42 124.8(6) . . ? N42 C41 H41 117.6 . . ? C42 C41 H41 117.6 . . ? C43 C42 C47 118.5(7) . . ? C43 C42 C41 125.4(7) . . ? C47 C42 C41 116.1(6) . . ? O4 C43 C42 128.3(7) . . ? O4 C43 C44 112.6(6) . . ? C42 C43 C44 119.0(7) . . ? C44 C45 C46 120.0(7) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C47 C46 C45 121.4(7) . . ? C47 C46 Br4 120.3(6) . . ? C45 C46 Br4 118.4(6) . . ? C46 C47 C42 120.9(7) . . ? C46 C47 H47 119.5 . . ? C42 C47 H47 119.5 . . ? C43 O4 Pd2 122.4(4) . . ? C33 C34 C35 119.2(7) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C45 C44 C43 119.9(7) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C2 N51 C61 107.3(5) . . ? C2 N51 N52 129.9(5) . . ? C61 N51 N52 122.3(6) . . ? N62 C61 N51 108.8(6) . . ? N62 C61 C62 123.4(6) . . ? N51 C61 C62 127.7(6) . . ? N52 C51 C52 118.6(6) . . ? N52 C51 H51 120.7 . . ? C52 C51 H51 120.7 . . ? C57 C52 C53 119.3(7) . . ? C57 C52 C51 117.3(6) . . ? C53 C52 C51 123.4(6) . . ? C56 C57 C52 119.9(7) . . ? C56 C57 H57 120.1 . . ? C52 C57 H57 120.1 . . ? C55 C56 C57 122.0(7) . . ? C55 C56 Br5 119.2(6) . . ? C57 C56 Br5 118.8(6) . . ? C56 C55 C54 116.4(7) . . ? C56 C55 H55 121.8 . . ? C54 C55 H55 121.8 . . ? C53 C54 C55 124.4(8) . . ? C53 C54 H54 117.8 . . ? C55 C54 H54 117.8 . . ? C66 C67 C62 120.5(6) . . ? C66 C67 H67 119.7 . . ? C62 C67 H67 119.7 . . ? C65 C66 C67 120.8(7) . . ? C65 C66 Br6 120.5(5) . . ? C67 C66 Br6 118.6(5) . . ? C66 C65 C64 123.7(6) . . ? C66 C65 H65 118.2 . . ? C64 C65 H65 118.2 . . ? C53 O5 H5 109.5 . . ? 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 N31 Pd1 P1 C74 85.7(4) . . . . ? O1 Pd1 P1 C74 -92.2(4) . . . . ? N12 Pd1 P1 C74 21(3) . . . . ? N31 Pd1 P1 C70 -34.2(4) . . . . ? O1 Pd1 P1 C70 147.9(4) . . . . ? N12 Pd1 P1 C70 -99(3) . . . . ? N31 Pd1 P1 C72 -156.7(4) . . . . ? O1 Pd1 P1 C72 25.4(4) . . . . ? N12 Pd1 P1 C72 138(3) . . . . ? C74 P1 C70 C71 54.2(9) . . . . ? C72 P1 C70 C71 -58.8(9) . . . . ? Pd1 P1 C70 C71 176.1(6) . . . . ? C70 P1 C74 C75 -167.3(6) . . . . ? C72 P1 C74 C75 -53.9(7) . . . . ? Pd1 P1 C74 C75 67.4(7) . . . . ? C74 P1 C72 C73 177.1(6) . . . . ? C70 P1 C72 C73 -69.8(7) . . . . ? Pd1 P1 C72 C73 57.3(6) . . . . ? N11 C1 N21 N22 -2.4(11) . . . . ? N31 C1 N21 N22 175.8(6) . . . . ? N11 C1 N21 C31 -176.1(7) . . . . ? N31 C1 N21 C31 2.0(7) . . . . ? C1 N21 N22 C21 24.6(10) . . . . ? C31 N21 N22 C21 -162.7(6) . . . . ? N21 N22 C21 C22 178.1(6) . . . . ? N22 C21 C22 C27 -171.0(7) . . . . ? N22 C21 C22 C23 10.7(10) . . . . ? C27 C22 C23 O2 -178.0(7) . . . . ? C21 C22 C23 O2 0.2(11) . . . . ? C27 C22 C23 C24 0.8(11) . . . . ? C21 C22 C23 C24 179.0(7) . . . . ? O2 C23 C24 C25 177.0(7) . . . . ? C22 C23 C24 C25 -1.8(12) . . . . ? C23 C24 C25 C26 -0.5(12) . . . . ? C24 C25 C26 C27 3.9(12) . . . . ? C24 C25 C26 Br2 -179.4(6) . . . . ? C25 C26 C27 C22 -5.0(11) . . . . ? Br2 C26 C27 C22 178.3(5) . . . . ? C23 C22 C27 C26 2.6(11) . . . . ? C21 C22 C27 C26 -175.7(7) . . . . ? N11 C1 N31 N32 176.9(7) . . . . ? N21 C1 N31 N32 -1.3(7) . . . . ? N11 C1 N31 Pd1 -3.2(9) . . . . ? N21 C1 N31 Pd1 178.7(4) . . . . ? O1 Pd1 N31 C1 -9(2) . . . . ? N12 Pd1 N31 C1 4.1(5) . . . . ? P1 Pd1 N31 C1 -173.0(4) . . . . ? O1 Pd1 N31 N32 171.2(15) . . . . ? N12 Pd1 N31 N32 -176.0(8) . . . . ? P1 Pd1 N31 N32 6.9(8) . . . . ? C1 N31 N32 C31 -0.1(8) . . . . ? Pd1 N31 N32 C31 -180.0(6) . . . . ? N31 N32 C31 N21 1.4(8) . . . . ? N31 N32 C31 C32 178.8(6) . . . . ? N22 N21 C31 N32 -176.3(6) . . . . ? C1 N21 C31 N32 -2.2(7) . . . . ? N22 N21 C31 C32 6.4(11) . . . . ? C1 N21 C31 C32 -179.5(7) . . . . ? N32 C31 C32 C33 13.3(11) . . . . ? N21 C31 C32 C33 -169.8(7) . . . . ? N32 C31 C32 C37 -163.1(7) . . . . ? N21 C31 C32 C37 13.8(11) . . . . ? C37 C32 C33 O3 176.6(7) . . . . ? C31 C32 C33 O3 -0.1(10) . . . . ? C37 C32 C33 C34 -2.0(11) . . . . ? C31 C32 C33 C34 -178.6(7) . . . . ? C34 C35 C36 C37 -2.6(11) . . . . ? C34 C35 C36 Br3 178.1(5) . . . . ? C35 C36 C37 C32 -0.4(12) . . . . ? Br3 C36 C37 C32 178.9(5) . . . . ? C33 C32 C37 C36 2.7(11) . . . . ? C31 C32 C37 C36 179.2(7) . . . . ? N31 C1 N11 N12 -0.9(9) . . . . ? N21 C1 N11 N12 176.9(6) . . . . ? C1 N11 N12 C11 -178.0(6) . . . . ? C1 N11 N12 Pd1 4.8(7) . . . . ? N31 Pd1 N12 C11 177.7(6) . . . . ? O1 Pd1 N12 C11 -4.0(6) . . . . ? P1 Pd1 N12 C11 -117(3) . . . . ? N31 Pd1 N12 N11 -5.3(5) . . . . ? O1 Pd1 N12 N11 173.0(5) . . . . ? P1 Pd1 N12 N11 60(3) . . . . ? N11 N12 C11 C12 -179.1(7) . . . . ? Pd1 N12 C11 C12 -2.1(11) . . . . ? N12 C11 C12 C17 -174.8(7) . . . . ? N12 C11 C12 C13 3.7(12) . . . . ? C17 C12 C13 O1 -176.7(7) . . . . ? C11 C12 C13 O1 4.8(12) . . . . ? C17 C12 C13 C14 -1.7(10) . . . . ? C11 C12 C13 C14 179.8(7) . . . . ? O1 C13 C14 C15 178.4(7) . . . . ? C12 C13 C14 C15 2.8(11) . . . . ? C13 C14 C15 C16 -1.8(12) . . . . ? C14 C15 C16 C17 -0.5(11) . . . . ? C14 C15 C16 Br1 178.0(6) . . . . ? C11 C12 C17 C16 178.2(7) . . . . ? C13 C12 C17 C16 -0.5(11) . . . . ? C15 C16 C17 C12 1.6(11) . . . . ? Br1 C16 C17 C12 -176.9(6) . . . . ? C14 C13 O1 Pd1 171.7(5) . . . . ? C12 C13 O1 Pd1 -13.2(10) . . . . ? N31 Pd1 O1 C13 24(2) . . . . ? N12 Pd1 O1 C13 11.2(6) . . . . ? P1 Pd1 O1 C13 -171.6(6) . . . . ? N61 Pd2 P2 C80 34.0(3) . . . . ? O4 Pd2 P2 C80 -145.5(3) . . . . ? N42 Pd2 P2 C80 98.3(16) . . . . ? N61 Pd2 P2 C84 158.2(3) . . . . ? O4 Pd2 P2 C84 -21.3(3) . . . . ? N42 Pd2 P2 C84 -137.5(16) . . . . ? N61 Pd2 P2 C82 -84.3(3) . . . . ? O4 Pd2 P2 C82 96.2(3) . . . . ? N42 Pd2 P2 C82 -20.0(16) . . . . ? C84 P2 C80 C81 45.8(7) . . . . ? C82 P2 C80 C81 -66.0(7) . . . . ? Pd2 P2 C80 C81 173.1(5) . . . . ? C80 P2 C82 C83 167.9(6) . . . . ? C84 P2 C82 C83 55.1(7) . . . . ? Pd2 P2 C82 C83 -67.0(6) . . . . ? C80 P2 C84 C85 60.2(7) . . . . ? C82 P2 C84 C85 171.4(6) . . . . ? Pd2 P2 C84 C85 -68.7(6) . . . . ? N41 C2 N61 N62 -175.9(6) . . . . ? N51 C2 N61 N62 3.4(7) . . . . ? N41 C2 N61 Pd2 -0.1(8) . . . . ? N51 C2 N61 Pd2 179.2(4) . . . . ? O4 Pd2 N61 N62 164.5(15) . . . . ? N42 Pd2 N61 N62 174.0(7) . . . . ? P2 Pd2 N61 N62 -11.6(7) . . . . ? O4 Pd2 N61 C2 -9(2) . . . . ? N42 Pd2 N61 C2 0.2(4) . . . . ? P2 Pd2 N61 C2 174.5(4) . . . . ? C2 N61 N62 C61 -3.3(7) . . . . ? Pd2 N61 N62 C61 -177.1(6) . . . . ? C67 C62 C63 O6 -176.3(6) . . . . ? C61 C62 C63 O6 4.1(10) . . . . ? C67 C62 C63 C64 4.4(10) . . . . ? C61 C62 C63 C64 -175.2(7) . . . . ? O6 C63 C64 C65 179.7(6) . . . . ? C62 C63 C64 C65 -0.8(10) . . . . ? N61 C2 N41 N42 -0.2(9) . . . . ? N51 C2 N41 N42 -179.3(6) . . . . ? C2 N41 N42 C41 -175.4(6) . . . . ? C2 N41 N42 Pd2 0.4(7) . . . . ? N61 Pd2 N42 C41 175.1(6) . . . . ? O4 Pd2 N42 C41 -6.1(6) . . . . ? P2 Pd2 N42 C41 109.9(16) . . . . ? N61 Pd2 N42 N41 -0.3(5) . . . . ? O4 Pd2 N42 N41 178.4(5) . . . . ? P2 Pd2 N42 N41 -65.6(18) . . . . ? N41 N42 C41 C42 178.3(6) . . . . ? Pd2 N42 C41 C42 2.8(10) . . . . ? N42 C41 C42 C43 3.6(12) . . . . ? N42 C41 C42 C47 -174.5(7) . . . . ? C47 C42 C43 O4 173.5(7) . . . . ? C41 C42 C43 O4 -4.5(12) . . . . ? C47 C42 C43 C44 -5.1(10) . . . . ? C41 C42 C43 C44 176.8(7) . . . . ? C44 C45 C46 C47 -2.5(11) . . . . ? C44 C45 C46 Br4 176.1(6) . . . . ? C45 C46 C47 C42 1.8(11) . . . . ? Br4 C46 C47 C42 -176.8(5) . . . . ? C43 C42 C47 C46 2.1(10) . . . . ? C41 C42 C47 C46 -179.6(7) . . . . ? C42 C43 O4 Pd2 -1.3(11) . . . . ? C44 C43 O4 Pd2 177.5(5) . . . . ? N61 Pd2 O4 C43 15(2) . . . . ? N42 Pd2 O4 C43 5.3(6) . . . . ? P2 Pd2 O4 C43 -169.2(6) . . . . ? O3 C33 C34 C35 -179.6(6) . . . . ? C32 C33 C34 C35 -1.0(11) . . . . ? C36 C35 C34 C33 3.2(10) . . . . ? C46 C45 C44 C43 -0.6(12) . . . . ? O4 C43 C44 C45 -174.4(7) . . . . ? C42 C43 C44 C45 4.5(11) . . . . ? N41 C2 N51 C61 177.0(7) . . . . ? N61 C2 N51 C61 -2.2(7) . . . . ? N41 C2 N51 N52 5.1(11) . . . . ? N61 C2 N51 N52 -174.1(6) . . . . ? C51 N52 N51 C2 -20.4(10) . . . . ? C51 N52 N51 C61 168.8(6) . . . . ? N61 N62 C61 N51 1.8(7) . . . . ? N61 N62 C61 C62 178.1(6) . . . . ? C2 N51 C61 N62 0.3(7) . . . . ? N52 N51 C61 N62 173.0(6) . . . . ? C2 N51 C61 C62 -175.8(7) . . . . ? N52 N51 C61 C62 -3.1(11) . . . . ? C67 C62 C61 N62 161.1(7) . . . . ? C63 C62 C61 N62 -19.4(10) . . . . ? C67 C62 C61 N51 -23.4(11) . . . . ? C63 C62 C61 N51 156.2(7) . . . . ? N51 N52 C51 C52 -177.3(6) . . . . ? C54 C53 C52 C57 -7.2(11) . . . . ? O5 C53 C52 C57 178.7(7) . . . . ? C54 C53 C52 C51 172.8(7) . . . . ? O5 C53 C52 C51 -1.3(11) . . . . ? N52 C51 C52 C57 173.3(7) . . . . ? N52 C51 C52 C53 -6.7(10) . . . . ? C53 C52 C57 C56 0.9(11) . . . . ? C51 C52 C57 C56 -179.0(7) . . . . ? C52 C57 C56 C55 2.8(12) . . . . ? C52 C57 C56 Br5 -178.8(5) . . . . ? C57 C56 C55 C54 -0.1(11) . . . . ? Br5 C56 C55 C54 -178.6(6) . . . . ? O5 C53 C54 C55 -175.3(8) . . . . ? C52 C53 C54 C55 10.4(12) . . . . ? C56 C55 C54 C53 -6.8(12) . . . . ? C63 C62 C67 C66 -3.0(10) . . . . ? C61 C62 C67 C66 176.6(7) . . . . ? C62 C67 C66 C65 -1.8(11) . . . . ? C62 C67 C66 Br6 178.3(5) . . . . ? C67 C66 C65 C64 5.7(11) . . . . ? Br6 C66 C65 C64 -174.4(5) . . . . ? C63 C64 C65 C66 -4.2(10) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.68 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 4.888 _refine_diff_density_min -1.174 _refine_diff_density_rms 0.225 _database_code_depnum_ccdc_archive 'CCDC 942799' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_11-[(pdpet3)h2l'] _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,4-Dihydro-5-(2-hydroxyphenyl)-4-((2-hydroxyphenyl)methyleneamino) -1,2,4-triazol-3-ylidene 2-oxybenzaldehyde hydrazono)-(triethylphosphine) -palladium(ii) ; _chemical_name_common '[(PdPEt3)H2L]' _chemical_melting_point ? _chemical_formula_moiety 'C28 H31 N6 O3 P Pd' _chemical_formula_sum 'C28 H31 N6 O3 P Pd' _chemical_formula_weight 636.96 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' 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 10.2404(19) _cell_length_b 10.596(2) _cell_length_c 13.021(2) _cell_angle_alpha 90.997(3) _cell_angle_beta 99.318(3) _cell_angle_gamma 102.809(3) _cell_volume 1357.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1754 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 20.58 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 0.785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6096 _exptl_absorpt_correction_T_max 0.6950 _exptl_absorpt_process_details 'SADABS Medium Absorber' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14564 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.10 _reflns_number_total 4847 _reflns_number_gt 4118 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0394P)^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 constr. _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4847 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0916 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _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 Pd1 Pd 0.55696(3) 0.77277(3) -0.02359(2) 0.01729(10) Uani 1 1 d . . . P1 P 0.68883(10) 0.93212(9) -0.09913(7) 0.0193(2) Uani 1 1 d . . . C1 C 0.6397(3) 0.6802(3) 0.1664(3) 0.0179(8) Uani 1 1 d . . . C70 C 0.8381(4) 0.8781(4) -0.1220(3) 0.0263(9) Uani 1 1 d . . . H70A H 0.8971 0.9477 -0.1541 0.032 Uiso 1 1 calc R . . H70B H 0.8899 0.8622 -0.0543 0.032 Uiso 1 1 calc R . . C71 C 0.8032(5) 0.7552(4) -0.1924(3) 0.0385(11) Uani 1 1 d . . . H71C H 0.7293 0.6922 -0.1697 0.058 Uiso 1 1 calc R . . H71B H 0.8834 0.7182 -0.1885 0.058 Uiso 1 1 calc R . . H71A H 0.7745 0.7758 -0.2644 0.058 Uiso 1 1 calc R . . C60 C 0.7549(4) 1.0846(3) -0.0217(3) 0.0223(8) Uani 1 1 d . . . H60A H 0.6773 1.1159 -0.0029 0.027 Uiso 1 1 calc R . . H60B H 0.8105 1.0675 0.0440 0.027 Uiso 1 1 calc R . . C61 C 0.8415(4) 1.1929(4) -0.0746(3) 0.0317(10) Uani 1 1 d . . . H61C H 0.9172 1.1623 -0.0959 0.047 Uiso 1 1 calc R . . H61B H 0.8773 1.2686 -0.0256 0.047 Uiso 1 1 calc R . . H61A H 0.7854 1.2169 -0.1361 0.047 Uiso 1 1 calc R . . C50 C 0.6075(4) 0.9724(4) -0.2253(3) 0.0271(9) Uani 1 1 d . . . H50B H 0.6763 1.0303 -0.2588 0.033 Uiso 1 1 calc R . . H50A H 0.5717 0.8920 -0.2704 0.033 Uiso 1 1 calc R . . C51 C 0.4914(4) 1.0390(4) -0.2172(3) 0.0292(9) Uani 1 1 d . . . H51C H 0.4223 0.9818 -0.1849 0.044 Uiso 1 1 calc R . . H51A H 0.4508 1.0578 -0.2870 0.044 Uiso 1 1 calc R . . H51B H 0.5267 1.1201 -0.1744 0.044 Uiso 1 1 calc R . . N11 N 0.5212(3) 0.5960(3) 0.1461(2) 0.0190(7) Uani 1 1 d . . . N12 N 0.4554(3) 0.6269(3) 0.0510(2) 0.0182(7) Uani 1 1 d . . . C11 C 0.3367(4) 0.5562(3) 0.0152(3) 0.0190(8) Uani 1 1 d . . . H11 H 0.3015 0.4872 0.0558 0.023 Uiso 1 1 calc R . . C12 C 0.2531(4) 0.5729(3) -0.0810(3) 0.0191(8) Uani 1 1 d . . . C13 C 0.2912(4) 0.6673(3) -0.1537(3) 0.0189(8) Uani 1 1 d . . . C14 C 0.1944(4) 0.6742(4) -0.2424(3) 0.0233(9) Uani 1 1 d . . . H14 H 0.2176 0.7374 -0.2913 0.028 Uiso 1 1 calc R . . C15 C 0.0678(4) 0.5928(4) -0.2605(3) 0.0264(9) Uani 1 1 d . . . H15 H 0.0051 0.6002 -0.3211 0.032 Uiso 1 1 calc R . . C16 C 0.0306(4) 0.4985(4) -0.1898(3) 0.0250(9) Uani 1 1 d . . . H16 H -0.0570 0.4417 -0.2023 0.030 Uiso 1 1 calc R . . C17 C 0.1218(4) 0.4892(4) -0.1030(3) 0.0248(9) Uani 1 1 d . . . H17 H 0.0965 0.4246 -0.0557 0.030 Uiso 1 1 calc R . . O1 O 0.4113(2) 0.7490(2) -0.14724(18) 0.0209(6) Uani 1 1 d . . . N31 N 0.6883(3) 0.7743(3) 0.1053(2) 0.0186(7) Uani 1 1 d . . . N32 N 0.8126(3) 0.8487(3) 0.1562(2) 0.0204(7) Uani 1 1 d . . . C31 C 0.8399(3) 0.7980(3) 0.2456(3) 0.0171(8) Uani 1 1 d . . . C32 C 0.9594(3) 0.8490(3) 0.3252(3) 0.0190(8) Uani 1 1 d . . . C33 C 1.0065(4) 0.9832(4) 0.3424(3) 0.0224(8) Uani 1 1 d . . . C34 C 1.1203(4) 1.0343(4) 0.4182(3) 0.0265(9) Uani 1 1 d . . . H34 H 1.1526 1.1255 0.4296 0.032 Uiso 1 1 calc R . . C35 C 1.1849(4) 0.9527(4) 0.4757(3) 0.0303(10) Uani 1 1 d . . . H35 H 1.2615 0.9880 0.5278 0.036 Uiso 1 1 calc R . . C36 C 1.1409(4) 0.8184(4) 0.4597(3) 0.0264(9) Uani 1 1 d . . . H36 H 1.1871 0.7625 0.4999 0.032 Uiso 1 1 calc R . . C37 C 1.0301(4) 0.7688(4) 0.3850(3) 0.0236(9) Uani 1 1 d . . . H37 H 1.0003 0.6774 0.3733 0.028 Uiso 1 1 calc R . . O3 O 0.9434(3) 1.0687(2) 0.2882(2) 0.0286(6) Uani 1 1 d . . . H3 H 0.8836 1.0282 0.2398 0.043 Uiso 1 1 calc R . . N21 N 0.7362(3) 0.6914(3) 0.2565(2) 0.0173(6) Uani 1 1 d . . . N22 N 0.7317(3) 0.6281(3) 0.3474(2) 0.0178(7) Uani 1 1 d . . . C21 C 0.6453(3) 0.5200(3) 0.3454(3) 0.0180(8) Uani 1 1 d . . . H21 H 0.5890 0.4838 0.2817 0.022 Uiso 1 1 calc R . . C22 C 0.6336(4) 0.4529(3) 0.4409(3) 0.0181(8) Uani 1 1 d . . . C23 C 0.7083(4) 0.5055(3) 0.5395(3) 0.0212(8) Uani 1 1 d . . . C24 C 0.6857(4) 0.4392(4) 0.6278(3) 0.0243(9) Uani 1 1 d . . . H24 H 0.7336 0.4755 0.6942 0.029 Uiso 1 1 calc R . . C25 C 0.5948(4) 0.3217(4) 0.6206(3) 0.0274(9) Uani 1 1 d . . . H25 H 0.5814 0.2770 0.6820 0.033 Uiso 1 1 calc R . . C26 C 0.5227(4) 0.2677(4) 0.5254(3) 0.0278(9) Uani 1 1 d . . . H26 H 0.4609 0.1856 0.5212 0.033 Uiso 1 1 calc R . . C27 C 0.5405(4) 0.3328(3) 0.4371(3) 0.0236(9) Uani 1 1 d . . . H27 H 0.4888 0.2962 0.3719 0.028 Uiso 1 1 calc R . . O2 O 0.7996(3) 0.6197(2) 0.54986(19) 0.0266(6) Uani 1 1 d . . . H2 H 0.7993 0.6528 0.4917 0.040 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 0.01666(17) 0.01898(17) 0.01521(16) 0.00293(11) 0.00126(11) 0.00282(12) P1 0.0213(5) 0.0191(5) 0.0180(5) 0.0019(4) 0.0050(4) 0.0044(4) C1 0.0162(19) 0.022(2) 0.0142(18) 0.0029(15) -0.0003(15) 0.0041(16) C70 0.021(2) 0.033(2) 0.028(2) 0.0061(18) 0.0127(18) 0.0074(18) C71 0.046(3) 0.029(2) 0.047(3) 0.001(2) 0.024(2) 0.010(2) C60 0.026(2) 0.020(2) 0.021(2) 0.0010(16) 0.0053(17) 0.0048(17) C61 0.029(2) 0.025(2) 0.041(3) -0.0004(19) 0.011(2) 0.0014(18) C50 0.039(2) 0.023(2) 0.019(2) 0.0033(16) 0.0037(18) 0.0054(19) C51 0.032(2) 0.027(2) 0.028(2) 0.0121(17) 0.0009(18) 0.0066(19) N11 0.0172(16) 0.0239(17) 0.0147(16) 0.0052(13) 0.0012(13) 0.0030(14) N12 0.0193(17) 0.0192(16) 0.0144(15) 0.0012(12) -0.0008(13) 0.0037(13) C11 0.020(2) 0.0183(19) 0.0175(19) 0.0038(15) 0.0016(16) 0.0034(16) C12 0.0166(19) 0.0192(19) 0.0192(19) -0.0056(15) -0.0011(15) 0.0027(16) C13 0.019(2) 0.0166(19) 0.021(2) -0.0042(15) 0.0011(16) 0.0057(16) C14 0.024(2) 0.025(2) 0.020(2) -0.0015(16) -0.0005(17) 0.0079(17) C15 0.021(2) 0.035(2) 0.021(2) -0.0062(17) -0.0047(17) 0.0092(18) C16 0.0110(19) 0.029(2) 0.030(2) -0.0029(18) -0.0033(16) -0.0001(16) C17 0.024(2) 0.026(2) 0.024(2) 0.0011(17) 0.0028(17) 0.0069(18) O1 0.0200(14) 0.0232(14) 0.0172(13) 0.0034(11) -0.0005(11) 0.0026(11) N31 0.0131(15) 0.0202(16) 0.0209(16) 0.0040(13) 0.0015(13) 0.0011(13) N32 0.0156(16) 0.0231(17) 0.0204(17) -0.0009(13) 0.0002(13) 0.0020(13) C31 0.0138(18) 0.0210(19) 0.0178(19) 0.0024(15) 0.0062(15) 0.0042(15) C32 0.0150(19) 0.023(2) 0.0178(19) 0.0037(15) 0.0059(15) -0.0001(16) C33 0.019(2) 0.028(2) 0.021(2) 0.0040(16) 0.0070(16) 0.0041(17) C34 0.030(2) 0.024(2) 0.021(2) -0.0032(17) 0.0094(18) -0.0055(18) C35 0.021(2) 0.041(3) 0.023(2) -0.0050(19) -0.0001(17) -0.0025(19) C36 0.017(2) 0.040(2) 0.023(2) 0.0059(18) 0.0015(17) 0.0097(18) C37 0.020(2) 0.023(2) 0.026(2) -0.0028(16) 0.0004(17) 0.0034(17) O3 0.0329(17) 0.0204(14) 0.0301(16) 0.0046(12) 0.0031(13) 0.0021(13) N21 0.0118(15) 0.0210(16) 0.0167(16) 0.0057(13) 0.0001(12) 0.0006(13) N22 0.0166(16) 0.0213(17) 0.0156(16) 0.0069(13) 0.0025(13) 0.0045(13) C21 0.0154(19) 0.021(2) 0.0183(19) -0.0023(15) 0.0012(15) 0.0078(16) C22 0.0180(19) 0.0179(19) 0.0197(19) 0.0060(15) 0.0040(15) 0.0062(16) C23 0.017(2) 0.021(2) 0.026(2) 0.0020(16) 0.0017(16) 0.0058(16) C24 0.025(2) 0.030(2) 0.019(2) 0.0065(17) 0.0032(17) 0.0086(18) C25 0.029(2) 0.028(2) 0.030(2) 0.0154(18) 0.0112(18) 0.0112(19) C26 0.025(2) 0.019(2) 0.039(2) 0.0107(18) 0.0077(19) 0.0020(17) C27 0.019(2) 0.019(2) 0.029(2) -0.0040(17) 0.0005(17) 0.0018(16) O2 0.0282(15) 0.0241(15) 0.0204(14) 0.0029(11) -0.0029(12) -0.0042(12) _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 Pd1 N31 1.971(3) . ? Pd1 O1 1.981(2) . ? Pd1 N12 2.020(3) . ? Pd1 P1 2.2626(10) . ? P1 C70 1.811(4) . ? P1 C50 1.821(4) . ? P1 C60 1.823(4) . ? C1 N11 1.321(4) . ? C1 N31 1.346(4) . ? C1 N21 1.391(4) . ? C70 C71 1.520(5) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 H71C 0.9800 . ? C71 H71B 0.9800 . ? C71 H71A 0.9800 . ? C60 C61 1.534(5) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61C 0.9800 . ? C61 H61B 0.9800 . ? C61 H61A 0.9800 . ? C50 C51 1.527(5) . ? C50 H50B 0.9900 . ? C50 H50A 0.9900 . ? C51 H51C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? N11 N12 1.391(4) . ? N12 C11 1.287(4) . ? C11 C12 1.436(5) . ? C11 H11 0.9500 . ? C12 C17 1.420(5) . ? C12 C13 1.424(5) . ? C13 O1 1.327(4) . ? C13 C14 1.410(5) . ? C14 C15 1.371(5) . ? C14 H14 0.9500 . ? C15 C16 1.402(5) . ? C15 H15 0.9500 . ? C16 C17 1.365(5) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? N31 N32 1.395(4) . ? N32 C31 1.306(4) . ? C31 N21 1.395(4) . ? C31 C32 1.462(5) . ? C32 C33 1.398(5) . ? C32 C37 1.403(5) . ? C33 O3 1.367(4) . ? C33 C34 1.398(5) . ? C34 C35 1.365(5) . ? C34 H34 0.9500 . ? C35 C36 1.395(5) . ? C35 H35 0.9500 . ? C36 C37 1.367(5) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? O3 H3 0.8400 . ? N21 N22 1.373(4) . ? N22 C21 1.280(4) . ? C21 C22 1.451(5) . ? C21 H21 0.9500 . ? C22 C27 1.405(5) . ? C22 C23 1.418(5) . ? C23 O2 1.346(4) . ? C23 C24 1.383(5) . ? C24 C25 1.370(5) . ? C24 H24 0.9500 . ? C25 C26 1.378(5) . ? C25 H25 0.9500 . ? C26 C27 1.369(5) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? O2 H2 0.8400 . ? 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 N31 Pd1 O1 172.31(10) . . ? N31 Pd1 N12 78.61(11) . . ? O1 Pd1 N12 93.83(10) . . ? N31 Pd1 P1 96.66(9) . . ? O1 Pd1 P1 90.83(7) . . ? N12 Pd1 P1 174.66(8) . . ? C70 P1 C50 106.34(18) . . ? C70 P1 C60 104.93(18) . . ? C50 P1 C60 106.49(17) . . ? C70 P1 Pd1 108.43(13) . . ? C50 P1 Pd1 114.04(13) . . ? C60 P1 Pd1 115.85(12) . . ? N11 C1 N31 126.6(3) . . ? N11 C1 N21 126.6(3) . . ? N31 C1 N21 106.8(3) . . ? C71 C70 P1 112.7(3) . . ? C71 C70 H70A 109.0 . . ? P1 C70 H70A 109.0 . . ? C71 C70 H70B 109.0 . . ? P1 C70 H70B 109.0 . . ? H70A C70 H70B 107.8 . . ? C70 C71 H71C 109.5 . . ? C70 C71 H71B 109.5 . . ? H71C C71 H71B 109.5 . . ? C70 C71 H71A 109.5 . . ? H71C C71 H71A 109.5 . . ? H71B C71 H71A 109.5 . . ? C61 C60 P1 115.4(2) . . ? C61 C60 H60A 108.4 . . ? P1 C60 H60A 108.4 . . ? C61 C60 H60B 108.4 . . ? P1 C60 H60B 108.4 . . ? H60A C60 H60B 107.5 . . ? C60 C61 H61C 109.5 . . ? C60 C61 H61B 109.5 . . ? H61C C61 H61B 109.5 . . ? C60 C61 H61A 109.5 . . ? H61C C61 H61A 109.5 . . ? H61B C61 H61A 109.5 . . ? C51 C50 P1 112.8(3) . . ? C51 C50 H50B 109.0 . . ? P1 C50 H50B 109.0 . . ? C51 C50 H50A 109.0 . . ? P1 C50 H50A 109.0 . . ? H50B C50 H50A 107.8 . . ? C50 C51 H51C 109.5 . . ? C50 C51 H51A 109.5 . . ? H51C C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51C C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C1 N11 N12 106.4(3) . . ? C11 N12 N11 117.2(3) . . ? C11 N12 Pd1 125.1(2) . . ? N11 N12 Pd1 117.7(2) . . ? N12 C11 C12 125.4(3) . . ? N12 C11 H11 117.3 . . ? C12 C11 H11 117.3 . . ? C17 C12 C13 118.5(3) . . ? C17 C12 C11 116.4(3) . . ? C13 C12 C11 125.1(3) . . ? O1 C13 C14 116.1(3) . . ? O1 C13 C12 126.1(3) . . ? C14 C13 C12 117.8(3) . . ? C15 C14 C13 122.1(4) . . ? C15 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? C14 C15 C16 120.2(3) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 119.2(3) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C12 122.2(4) . . ? C16 C17 H17 118.9 . . ? C12 C17 H17 118.9 . . ? C13 O1 Pd1 124.0(2) . . ? C1 N31 N32 109.8(3) . . ? C1 N31 Pd1 110.7(2) . . ? N32 N31 Pd1 139.3(2) . . ? C31 N32 N31 106.8(3) . . ? N32 C31 N21 110.5(3) . . ? N32 C31 C32 124.8(3) . . ? N21 C31 C32 124.6(3) . . ? C33 C32 C37 118.1(3) . . ? C33 C32 C31 119.1(3) . . ? C37 C32 C31 122.8(3) . . ? O3 C33 C34 117.7(3) . . ? O3 C33 C32 122.1(3) . . ? C34 C33 C32 120.2(3) . . ? C35 C34 C33 119.7(4) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 121.4(4) . . ? C34 C35 H35 119.3 . . ? C36 C35 H35 119.3 . . ? C37 C36 C35 118.7(4) . . ? C37 C36 H36 120.6 . . ? C35 C36 H36 120.6 . . ? C36 C37 C32 121.9(4) . . ? C36 C37 H37 119.1 . . ? C32 C37 H37 119.1 . . ? C33 O3 H3 109.5 . . ? N22 N21 C1 130.6(3) . . ? N22 N21 C31 122.7(3) . . ? C1 N21 C31 106.2(3) . . ? C21 N22 N21 118.1(3) . . ? N22 C21 C22 119.7(3) . . ? N22 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C27 C22 C23 118.0(3) . . ? C27 C22 C21 119.1(3) . . ? C23 C22 C21 122.9(3) . . ? O2 C23 C24 118.7(3) . . ? O2 C23 C22 121.7(3) . . ? C24 C23 C22 119.5(3) . . ? C25 C24 C23 120.6(4) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 120.9(4) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C27 C26 C25 119.7(4) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C22 121.3(4) . . ? C26 C27 H27 119.4 . . ? C22 C27 H27 119.4 . . ? C23 O2 H2 109.5 . . ? 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 N31 Pd1 P1 C70 63.33(16) . . . . ? O1 Pd1 P1 C70 -114.95(15) . . . . ? N12 Pd1 P1 C70 35.9(9) . . . . ? N31 Pd1 P1 C50 -178.41(16) . . . . ? O1 Pd1 P1 C50 3.31(15) . . . . ? N12 Pd1 P1 C50 154.1(9) . . . . ? N31 Pd1 P1 C60 -54.26(16) . . . . ? O1 Pd1 P1 C60 127.47(16) . . . . ? N12 Pd1 P1 C60 -81.7(9) . . . . ? C50 P1 C70 C71 -63.5(3) . . . . ? C60 P1 C70 C71 -176.1(3) . . . . ? Pd1 P1 C70 C71 59.5(3) . . . . ? C70 P1 C60 C61 61.8(3) . . . . ? C50 P1 C60 C61 -50.7(3) . . . . ? Pd1 P1 C60 C61 -178.7(2) . . . . ? C70 P1 C50 C51 -171.4(3) . . . . ? C60 P1 C50 C51 -59.9(3) . . . . ? Pd1 P1 C50 C51 69.2(3) . . . . ? N31 C1 N11 N12 -2.0(5) . . . . ? N21 C1 N11 N12 175.8(3) . . . . ? C1 N11 N12 C11 179.7(3) . . . . ? C1 N11 N12 Pd1 2.8(3) . . . . ? N31 Pd1 N12 C11 -179.0(3) . . . . ? O1 Pd1 N12 C11 -0.4(3) . . . . ? P1 Pd1 N12 C11 -151.1(7) . . . . ? N31 Pd1 N12 N11 -2.4(2) . . . . ? O1 Pd1 N12 N11 176.2(2) . . . . ? P1 Pd1 N12 N11 25.5(10) . . . . ? N11 N12 C11 C12 179.9(3) . . . . ? Pd1 N12 C11 C12 -3.5(5) . . . . ? N12 C11 C12 C17 -176.2(3) . . . . ? N12 C11 C12 C13 2.7(6) . . . . ? C17 C12 C13 O1 -177.1(3) . . . . ? C11 C12 C13 O1 4.0(6) . . . . ? C17 C12 C13 C14 1.6(5) . . . . ? C11 C12 C13 C14 -177.3(3) . . . . ? O1 C13 C14 C15 178.0(3) . . . . ? C12 C13 C14 C15 -0.9(5) . . . . ? C13 C14 C15 C16 0.0(6) . . . . ? C14 C15 C16 C17 0.2(5) . . . . ? C15 C16 C17 C12 0.6(6) . . . . ? C13 C12 C17 C16 -1.5(5) . . . . ? C11 C12 C17 C16 177.5(3) . . . . ? C14 C13 O1 Pd1 172.7(2) . . . . ? C12 C13 O1 Pd1 -8.6(5) . . . . ? N31 Pd1 O1 C13 16.4(9) . . . . ? N12 Pd1 O1 C13 6.1(3) . . . . ? P1 Pd1 O1 C13 -176.5(2) . . . . ? N11 C1 N31 N32 176.1(3) . . . . ? N21 C1 N31 N32 -2.0(4) . . . . ? N11 C1 N31 Pd1 0.1(4) . . . . ? N21 C1 N31 Pd1 -178.0(2) . . . . ? O1 Pd1 N31 C1 -9.3(9) . . . . ? N12 Pd1 N31 C1 1.2(2) . . . . ? P1 Pd1 N31 C1 -176.3(2) . . . . ? O1 Pd1 N31 N32 176.5(7) . . . . ? N12 Pd1 N31 N32 -173.0(4) . . . . ? P1 Pd1 N31 N32 9.5(3) . . . . ? C1 N31 N32 C31 1.5(4) . . . . ? Pd1 N31 N32 C31 175.7(3) . . . . ? N31 N32 C31 N21 -0.4(4) . . . . ? N31 N32 C31 C32 -177.9(3) . . . . ? N32 C31 C32 C33 37.9(5) . . . . ? N21 C31 C32 C33 -139.3(3) . . . . ? N32 C31 C32 C37 -141.6(4) . . . . ? N21 C31 C32 C37 41.2(5) . . . . ? C37 C32 C33 O3 -179.6(3) . . . . ? C31 C32 C33 O3 0.9(5) . . . . ? C37 C32 C33 C34 -0.6(5) . . . . ? C31 C32 C33 C34 179.9(3) . . . . ? O3 C33 C34 C35 178.7(3) . . . . ? C32 C33 C34 C35 -0.4(5) . . . . ? C33 C34 C35 C36 0.9(6) . . . . ? C34 C35 C36 C37 -0.4(6) . . . . ? C35 C36 C37 C32 -0.6(6) . . . . ? C33 C32 C37 C36 1.1(5) . . . . ? C31 C32 C37 C36 -179.4(3) . . . . ? N11 C1 N21 N22 -5.1(6) . . . . ? N31 C1 N21 N22 173.0(3) . . . . ? N11 C1 N21 C31 -176.4(3) . . . . ? N31 C1 N21 C31 1.7(4) . . . . ? N32 C31 N21 N22 -173.0(3) . . . . ? C32 C31 N21 N22 4.5(5) . . . . ? N32 C31 N21 C1 -0.8(4) . . . . ? C32 C31 N21 C1 176.7(3) . . . . ? C1 N21 N22 C21 20.6(5) . . . . ? C31 N21 N22 C21 -169.3(3) . . . . ? N21 N22 C21 C22 -177.5(3) . . . . ? N22 C21 C22 C27 -178.6(3) . . . . ? N22 C21 C22 C23 4.1(5) . . . . ? C27 C22 C23 O2 179.9(3) . . . . ? C21 C22 C23 O2 -2.8(5) . . . . ? C27 C22 C23 C24 -1.2(5) . . . . ? C21 C22 C23 C24 176.1(3) . . . . ? O2 C23 C24 C25 -179.2(3) . . . . ? C22 C23 C24 C25 1.9(5) . . . . ? C23 C24 C25 C26 -0.8(6) . . . . ? C24 C25 C26 C27 -0.9(6) . . . . ? C25 C26 C27 C22 1.6(6) . . . . ? C23 C22 C27 C26 -0.5(5) . . . . ? C21 C22 C27 C26 -178.0(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.477 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.096 _database_code_depnum_ccdc_archive 'CCDC 942800'