# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Murray Baker' _publ_contact_author_email MURRAY.BAKER@UWA.EDU.AU _publ_section_title ; Palladium complexes of o-xylyl-linked alkoxybenzimidazolin-2-ylidenes: interesting structural conformations and application as pre-catalysts ; loop_ _publ_author_name 'Murray Baker' 'David H Brown' 'Peter V Simpson' 'Brian W Skelton' 'Allan H. White' #===END data_dhb238 _database_code_depnum_ccdc_archive 'CCDC 726625' _audit_creation_date 2009-07-15T14:07:56-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C63 H74 Br2 N5 O4 Pd' _chemical_formula_moiety ; C46 H56 Br2 N4 O4 Pd, 5/2(C6 H6), C2 H3 N ; _chemical_formula_weight 1231.49 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.652(5) _cell_length_b 18.280(5) _cell_length_c 18.705(5) _cell_angle_alpha 82.53(2) _cell_angle_beta 80.84(2) _cell_angle_gamma 73.94(2) _cell_volume 5703(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 35551 _cell_measurement_theta_min 2.5844 _cell_measurement_theta_max 31.9903 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_size_max .43 _exptl_crystal_size_mid .08 _exptl_crystal_size_min .07 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2540 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.779 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.7 (release 06-03-2006 CrysAlis171 .NET) (compiled Mar 6 2006,22:55:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.88 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 -0.0287441416 _diffrn_orient_matrix_ub_12 0.0252561588 _diffrn_orient_matrix_ub_13 0.0224998473 _diffrn_orient_matrix_ub_21 0.006096327 _diffrn_orient_matrix_ub_22 -0.0278806461 _diffrn_orient_matrix_ub_23 0.0298057507 _diffrn_orient_matrix_ub_31 0.0301650098 _diffrn_orient_matrix_ub_32 0.014951982 _diffrn_orient_matrix_ub_33 0.0085735015 _diffrn_reflns_av_R_equivalents 0.1181 _diffrn_reflns_av_unetI/netI 0.2138 _diffrn_reflns_number 152638 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 32 _diffrn_reflns_theta_full 30 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.904 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 35791 _reflns_number_gt 16905 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.7 (release 06-03-2006 CrysAlis171 .NET) (compiled Mar 6 2006,22:55:04) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.7 (release 06-03-2006 CrysAlis171 .NET) (compiled Mar 6 2006,22:55:04) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.7 (release 06-03-2006 CrysAlis171 .NET) (compiled Mar 6 2006,22:55:04) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics OrtepII _computing_publication_material WinGX #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.1955P)^2^+62.2856P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 35791 _refine_ls_number_parameters 1352 _refine_ls_number_restraints 141 _refine_ls_R_factor_all 0.2099 _refine_ls_R_factor_gt 0.123 _refine_ls_wR_factor_ref 0.3772 _refine_ls_wR_factor_gt 0.348 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 7.177 _refine_diff_density_min -2.925 _refine_diff_density_rms 0.287 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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 0.48514(5) 0.89381(4) 0.29461(4) 0.01653(17) Uani 1 1 d . . . Pd2 Pd -0.11283(5) 0.50054(4) 0.78918(4) 0.01576(17) Uani 1 1 d . . . Br11 Br 0.53424(7) 0.76695(6) 0.36073(6) 0.0224(2) Uani 1 1 d . . . Br12 Br 0.39259(7) 0.94716(6) 0.40060(6) 0.0247(2) Uani 1 1 d . . . Br21 Br -0.06712(7) 0.40561(6) 0.89031(6) 0.0254(2) Uani 1 1 d . . . Br22 Br -0.24780(7) 0.54820(6) 0.85439(6) 0.0246(2) Uani 1 1 d . . . C11 C 0.6702(6) 0.9773(6) 0.2029(6) 0.021(2) Uani 1 1 d . . . C12 C 0.6135(7) 1.0441(6) 0.2238(6) 0.023(2) Uani 1 1 d . . . C13 C 0.6201(7) 1.1132(6) 0.1817(6) 0.020(2) Uani 1 1 d . . . H13 H 0.5827 1.1595 0.1946 0.024 Uiso 1 1 calc R . . C14 C 0.6769(7) 1.1166(7) 0.1238(7) 0.027(2) Uani 1 1 d . . . H14 H 0.6782 1.1639 0.0965 0.033 Uiso 1 1 calc R . . C15 C 0.7333(8) 1.0493(7) 0.1055(7) 0.032(3) Uani 1 1 d . . . H15 H 0.7748 1.05 0.0664 0.038 Uiso 1 1 calc R . . C16 C 0.7271(7) 0.9812(7) 0.1458(6) 0.028(2) Uani 1 1 d . . . H16 H 0.7647 0.9351 0.1326 0.034 Uiso 1 1 calc R . . C1 C 0.6727(6) 0.8991(5) 0.2432(6) 0.0176(19) Uani 1 1 d . . . H1A H 0.7284 0.8721 0.2496 0.021 Uiso 1 1 calc R . . H1B H 0.6419 0.9057 0.292 0.021 Uiso 1 1 calc R . . N21 N 0.6395(5) 0.8515(5) 0.2038(5) 0.0177(17) Uani 1 1 d . . . C22 C 0.5617(7) 0.8538(6) 0.2112(6) 0.021(2) Uani 1 1 d . . . N23 N 0.5509(5) 0.8145(5) 0.1606(4) 0.0147(16) Uani 1 1 d . . . C23A C 0.6250(6) 0.7805(5) 0.1221(5) 0.017(2) Uani 1 1 d . . . C24 C 0.6454(7) 0.7284(6) 0.0668(5) 0.020(2) Uani 1 1 d . . . O24 O 0.5876(5) 0.7026(4) 0.0464(4) 0.0243(16) Uani 1 1 d . . . C241 C 0.6130(8) 0.6560(8) -0.0126(6) 0.032(3) Uani 1 1 d . . . H24A H 0.6565 0.611 0.0002 0.038 Uiso 1 1 calc R . . H24B H 0.6336 0.6853 -0.056 0.038 Uiso 1 1 calc R . . C242 C 0.5426(9) 0.6290(8) -0.0300(8) 0.039(3) Uani 1 1 d . . . H24C H 0.5632 0.5885 -0.0638 0.047 Uiso 1 1 calc R . . H24D H 0.5173 0.6065 0.0155 0.047 Uiso 1 1 calc R . . C243 C 0.4804(10) 0.6929(9) -0.0636(9) 0.048(4) Uani 1 1 d . . . H24E H 0.5062 0.7217 -0.1043 0.057 Uiso 1 1 calc R . . H24F H 0.4516 0.7288 -0.0269 0.057 Uiso 1 1 calc R . . C244 C 0.4201(11) 0.6570(11) -0.0924(11) 0.063(5) Uani 1 1 d . . . H24G H 0.4496 0.6189 -0.126 0.095 Uiso 1 1 calc R . . H24H H 0.382 0.6975 -0.1178 0.095 Uiso 1 1 calc R . . H24I H 0.3915 0.6325 -0.0513 0.095 Uiso 1 1 calc R . . C25 C 0.7259(7) 0.7036(6) 0.0435(6) 0.024(2) Uani 1 1 d . . . H25 H 0.7434 0.6691 0.0068 0.029 Uiso 1 1 calc R . . C26 C 0.7824(7) 0.7277(6) 0.0722(6) 0.025(2) Uani 1 1 d . . . H26 H 0.8369 0.7092 0.054 0.03 Uiso 1 1 calc R . . C27 C 0.7625(7) 0.7769(6) 0.1254(6) 0.022(2) Uani 1 1 d . . . O27 O 0.8155(4) 0.8008(4) 0.1573(4) 0.0218(15) Uani 1 1 d . . . C271 C 0.8977(7) 0.7652(7) 0.1359(7) 0.030(3) Uani 1 1 d . . . H27A H 0.9121 0.7769 0.0832 0.036 Uiso 1 1 calc R . . H27B H 0.9086 0.709 0.1466 0.036 Uiso 1 1 calc R . . C272 C 0.9455(8) 0.7973(8) 0.1796(8) 0.038(3) Uani 1 1 d . . . H27C H 0.9327 0.7812 0.2317 0.046 Uiso 1 1 calc R . . H27D H 1.0027 0.7736 0.1654 0.046 Uiso 1 1 calc R . . C273 C 0.9322(9) 0.8816(9) 0.1710(8) 0.041(3) Uani 1 1 d . . . H27E H 0.9694 0.8949 0.1984 0.049 Uiso 1 1 calc R . . H27F H 0.8775 0.9052 0.1934 0.049 Uiso 1 1 calc R . . C274 C 0.9431(10) 0.9164(10) 0.0929(9) 0.053(4) Uani 1 1 d . . . H27G H 0.9987 0.898 0.0719 0.079 Uiso 1 1 calc R . . H27H H 0.9289 0.9722 0.0921 0.079 Uiso 1 1 calc R . . H27I H 0.9087 0.9013 0.0645 0.079 Uiso 1 1 calc R . . C27A C 0.6810(6) 0.8050(6) 0.1485(5) 0.018(2) Uani 1 1 d . . . C2 C 0.4713(6) 0.8183(6) 0.1425(5) 0.019(2) Uani 1 1 d . . . H2A H 0.4323 0.8241 0.1871 0.022 Uiso 1 1 calc R . . H2B H 0.4726 0.7701 0.1229 0.022 Uiso 1 1 calc R . . C31 C 0.3889(6) 0.9534(6) 0.1019(5) 0.018(2) Uani 1 1 d . . . C32 C 0.4453(6) 0.8851(6) 0.0867(5) 0.0164(19) Uani 1 1 d . . . C33 C 0.4796(7) 0.8752(7) 0.0147(6) 0.022(2) Uani 1 1 d . . . H33 H 0.5158 0.828 0.0028 0.027 Uiso 1 1 calc R . . C34 C 0.4607(7) 0.9343(6) -0.0397(5) 0.021(2) Uani 1 1 d . . . H34 H 0.4868 0.9281 -0.0878 0.025 Uiso 1 1 calc R . . C35 C 0.4055(7) 1.0008(7) -0.0250(7) 0.028(3) Uani 1 1 d . . . H35 H 0.3912 1.0399 -0.0629 0.034 Uiso 1 1 calc R . . C36 C 0.3704(7) 1.0108(6) 0.0460(6) 0.023(2) Uani 1 1 d . . . H36 H 0.333 1.0577 0.0567 0.028 Uiso 1 1 calc R . . C3 C 0.3470(6) 0.9715(6) 0.1785(6) 0.022(2) Uani 1 1 d . . . H3A H 0.29 0.9968 0.1762 0.026 Uiso 1 1 calc R . . H3B H 0.3509 0.9234 0.2105 0.026 Uiso 1 1 calc R . . N41 N 0.4703(5) 1.0578(5) 0.2587(5) 0.0191(17) Uani 1 1 d U . . C42 C 0.4453(6) 0.9959(6) 0.2473(6) 0.0194(18) Uani 1 1 d U . . N43 N 0.3831(5) 1.0216(5) 0.2092(5) 0.0205(17) Uani 1 1 d U . . C43A C 0.3623(6) 1.1027(6) 0.2025(5) 0.020(2) Uani 1 1 d . . . C44 C 0.2972(6) 1.1570(6) 0.1738(6) 0.023(2) Uani 1 1 d U . . O44 O 0.2436(5) 1.1293(5) 0.1459(5) 0.0315(19) Uani 1 1 d . . . C441 C 0.1816(8) 1.1839(7) 0.1115(6) 0.030(3) Uani 1 1 d . . . H44A H 0.2047 1.2167 0.0728 0.035 Uiso 1 1 calc R . . H44B H 0.1456 1.2169 0.1476 0.035 Uiso 1 1 calc R . . C442 C 0.1365(8) 1.1398(8) 0.0796(8) 0.037(3) Uani 1 1 d . . . H44C H 0.0953 1.1761 0.053 0.044 Uiso 1 1 calc R . . H44D H 0.1735 1.1065 0.0443 0.044 Uiso 1 1 calc R . . C443 C 0.0982(12) 1.0923(10) 0.1363(11) 0.063(5) Uani 1 1 d . . . H44E H 0.1402 1.0512 0.1575 0.076 Uiso 1 1 calc R . . H44F H 0.0685 1.1245 0.1756 0.076 Uiso 1 1 calc R . . C444 C 0.0432(12) 1.0573(11) 0.1099(11) 0.069(5) Uani 1 1 d . . . H44G H 0.0017 1.0974 0.0881 0.103 Uiso 1 1 calc R . . H44H H 0.0187 1.0286 0.1507 0.103 Uiso 1 1 calc R . . H44I H 0.0727 1.0225 0.0733 0.103 Uiso 1 1 calc R . . C45 C 0.2927(7) 1.2324(6) 0.1797(6) 0.025(2) Uani 1 1 d U . . H45 H 0.2511 1.271 0.1602 0.03 Uiso 1 1 calc R . . C46 C 0.3474(7) 1.2543(6) 0.2135(6) 0.026(2) Uani 1 1 d . . . H46 H 0.3416 1.307 0.217 0.031 Uiso 1 1 calc R . . C47 C 0.4086(7) 1.2012(6) 0.2414(6) 0.022(2) Uani 1 1 d . . . O47 O 0.4624(5) 1.2172(4) 0.2801(5) 0.0265(17) Uani 1 1 d . . . C471 C 0.4573(8) 1.2949(6) 0.2889(7) 0.033(3) Uani 1 1 d . . . H47A H 0.4035 1.3201 0.3119 0.039 Uiso 1 1 calc R . . H47B H 0.4675 1.3229 0.2409 0.039 Uiso 1 1 calc R . . C472 C 0.5198(12) 1.2955(9) 0.3371(12) 0.070(5) Uani 1 1 d U . . H47C H 0.5179 1.3493 0.3416 0.084 Uiso 1 1 calc R . . H47D H 0.5047 1.2724 0.3863 0.084 Uiso 1 1 calc R . . C473 C 0.6042(13) 1.2542(10) 0.3112(13) 0.081(5) Uani 1 1 d U . . H47E H 0.621 1.278 0.2628 0.097 Uiso 1 1 calc R . . H47F H 0.6071 1.2003 0.306 0.097 Uiso 1 1 calc R . . C474 C 0.6612(13) 1.2568(11) 0.3643(12) 0.096(5) Uani 1 1 d U . . H47G H 0.7154 1.2296 0.3459 0.144 Uiso 1 1 calc R . . H47H H 0.6452 1.2325 0.412 0.144 Uiso 1 1 calc R . . H47I H 0.6591 1.3102 0.3689 0.144 Uiso 1 1 calc RD . . C47A C 0.4175(7) 1.1244(6) 0.2345(6) 0.022(2) Uani 1 1 d . . . C4 C 0.5460(6) 1.0487(6) 0.2864(6) 0.020(2) Uani 1 1 d . . . H4A H 0.5575 1.0015 0.3199 0.024 Uiso 1 1 calc R . . H4B H 0.5421 1.0925 0.314 0.024 Uiso 1 1 calc R . . C51 C 0.0603(6) 0.6092(5) 0.7192(5) 0.0159(19) Uani 1 1 d . . . C52 C -0.0058(6) 0.6682(6) 0.7015(6) 0.019(2) Uani 1 1 d . . . C53 C 0.0055(7) 0.7250(6) 0.6441(6) 0.021(2) Uani 1 1 d . . . H53 H -0.0386 0.7653 0.6312 0.026 Uiso 1 1 calc R . . C54 C 0.0796(7) 0.7215(6) 0.6077(7) 0.026(2) Uani 1 1 d . . . H54 H 0.0862 0.7596 0.5693 0.031 Uiso 1 1 calc R . . C55 C 0.1441(7) 0.6650(7) 0.6248(7) 0.029(3) Uani 1 1 d . . . H55 H 0.195 0.6636 0.5985 0.035 Uiso 1 1 calc R . . C56 C 0.1350(7) 0.6102(6) 0.6801(6) 0.023(2) Uani 1 1 d . . . H56 H 0.1806 0.5716 0.6926 0.028 Uiso 1 1 calc R . . C5 C 0.0578(6) 0.5477(6) 0.7800(5) 0.018(2) Uani 1 1 d . . . H5A H 0.1036 0.5401 0.8071 0.021 Uiso 1 1 calc R . . H5B H 0.0085 0.5634 0.814 0.021 Uiso 1 1 calc R . . N61 N 0.0606(5) 0.4749(5) 0.7513(5) 0.0179(12) Uani 1 1 d U . . C62 C -0.0045(6) 0.4581(5) 0.7392(5) 0.0131(16) Uani 1 1 d U . . N63 N 0.0170(5) 0.3958(5) 0.7022(5) 0.0179(12) Uani 1 1 d U . . C63A C 0.0989(7) 0.3681(6) 0.6931(6) 0.023(2) Uani 1 1 d . . . C64 C 0.1499(7) 0.3019(6) 0.6655(6) 0.025(2) Uani 1 1 d U . . O64 O 0.1166(5) 0.2564(4) 0.6364(5) 0.0281(18) Uani 1 1 d . . . C641 C 0.1654(8) 0.1811(7) 0.6181(7) 0.035(3) Uani 1 1 d . . . H64A H 0.1774 0.1475 0.6631 0.042 Uiso 1 1 calc R . . H64B H 0.2163 0.1855 0.5892 0.042 Uiso 1 1 calc R . . C642 C 0.1214(12) 0.1488(10) 0.5763(14) 0.080(5) Uani 1 1 d U . . H64C H 0.12 0.1785 0.5281 0.096 Uiso 1 1 calc R . . H64D H 0.1536 0.0963 0.5679 0.096 Uiso 1 1 calc R . . C643 C 0.0449(13) 0.1444(11) 0.6011(15) 0.083(5) Uani 1 1 d U . . H64E H 0.0113 0.1954 0.6132 0.1 Uiso 1 1 calc R . . H64F H 0.0448 0.1089 0.6458 0.1 Uiso 1 1 calc R . . C644 C 0.0093(12) 0.1146(10) 0.5397(14) 0.077(5) Uani 1 1 d U . . H64G H 0.0291 0.1352 0.4915 0.115 Uiso 1 1 calc R . . H64H H -0.0489 0.1319 0.5473 0.115 Uiso 1 1 calc R . . H64I H 0.0259 0.0587 0.5429 0.115 Uiso 1 1 calc R . . C65 C 0.2311(7) 0.2896(7) 0.6715(7) 0.028(2) Uani 1 1 d U . . H65 H 0.2677 0.2453 0.6531 0.034 Uiso 1 1 calc R . . C66 C 0.2600(7) 0.3391(7) 0.7029(7) 0.031(3) Uani 1 1 d . . . H66 H 0.3155 0.3283 0.7046 0.037 Uiso 1 1 calc R . . C67 C 0.2091(6) 0.4052(6) 0.7325(6) 0.022(2) Uani 1 1 d . . . O67 O 0.2311(5) 0.4547(5) 0.7675(6) 0.040(2) Uani 1 1 d U B . C671 C 0.3153(9) 0.4470(9) 0.7682(9) 0.051(3) Uani 1 1 d DU . . H67A H 0.3369 0.4772 0.7261 0.061 Uiso 0.5 1 calc PR A 1 H67B H 0.3463 0.3928 0.7678 0.061 Uiso 0.5 1 calc PR A 1 H67J H 0.3464 0.4237 0.7242 0.061 Uiso 0.5 1 d PR A 2 H67K H 0.3337 0.4134 0.8115 0.061 Uiso 0.5 1 d PR A 2 C672 C 0.317(2) 0.4780(16) 0.8382(16) 0.051(5) Uiso 0.5 1 d PDU B 1 H67C H 0.3711 0.4634 0.8519 0.061 Uiso 0.5 1 calc PR B 1 H67D H 0.2809 0.4588 0.878 0.061 Uiso 0.5 1 calc PR B 1 C673 C 0.288(3) 0.5636(19) 0.823(2) 0.049(7) Uiso 0.5 1 d PDU B 1 H67E H 0.2292 0.5781 0.8227 0.059 Uiso 0.5 1 calc PR B 1 H67F H 0.2994 0.5891 0.8616 0.059 Uiso 0.5 1 calc PR B 1 C674 C 0.326(2) 0.591(2) 0.7505(15) 0.059(7) Uiso 0.5 1 d PDU B 1 H67G H 0.3063 0.6466 0.7421 0.089 Uiso 0.5 1 calc PR B 1 H67H H 0.3139 0.5666 0.7117 0.089 Uiso 0.5 1 calc PR B 1 H67I H 0.3841 0.5775 0.7505 0.089 Uiso 0.5 1 calc PR B 1 C675 C 0.3292(17) 0.5307(14) 0.7712(14) 0.038(6) Uiso 0.5 1 d PD B 2 H67L H 0.3861 0.526 0.7727 0.046 Uiso 0.5 1 calc PR B 2 H67M H 0.3127 0.5644 0.7274 0.046 Uiso 0.5 1 calc PR B 2 C676 C 0.279(2) 0.5644(18) 0.8397(15) 0.037(8) Uiso 0.5 1 d PD B 2 H67N H 0.2225 0.5688 0.8374 0.044 Uiso 0.5 1 calc PR B 2 H67O H 0.2851 0.6165 0.8412 0.044 Uiso 0.5 1 calc PR B 2 C677 C 0.304(2) 0.5154(19) 0.9101(17) 0.056(8) Uiso 0.5 1 d PD B 2 H67P H 0.2928 0.4656 0.9115 0.084 Uiso 0.5 1 calc PR B 2 H67Q H 0.2739 0.5415 0.9524 0.084 Uiso 0.5 1 calc PR B 2 H67R H 0.361 0.5079 0.9111 0.084 Uiso 0.5 1 calc PR B 2 C67A C 0.1268(7) 0.4175(6) 0.7250(6) 0.021(2) Uani 1 1 d . . . C6 C -0.0422(7) 0.3663(6) 0.6744(6) 0.023(2) Uani 1 1 d . . . H6A H -0.0922 0.3762 0.7085 0.028 Uiso 1 1 calc R . . H6B H -0.0218 0.3104 0.6724 0.028 Uiso 1 1 calc R . . C71 C -0.1279(6) 0.4614(5) 0.5852(5) 0.0147(18) Uani 1 1 d . . . C72 C -0.0595(6) 0.4039(6) 0.5988(5) 0.0173(19) Uani 1 1 d . . . C73 C -0.0004(6) 0.3805(6) 0.5406(6) 0.019(2) Uani 1 1 d . . . H73 H 0.0467 0.3419 0.5493 0.023 Uiso 1 1 calc R . . C74 C -0.0102(7) 0.4132(6) 0.4711(6) 0.021(2) Uani 1 1 d . . . H74 H 0.0304 0.3971 0.4321 0.026 Uiso 1 1 calc R . . C75 C -0.0774(7) 0.4684(6) 0.4574(6) 0.021(2) Uani 1 1 d . . . H75 H -0.0839 0.4902 0.409 0.025 Uiso 1 1 calc R . . C76 C -0.1354(7) 0.4924(6) 0.5136(6) 0.021(2) Uani 1 1 d . . . H76 H -0.182 0.531 0.5037 0.025 Uiso 1 1 calc R . . C7 C -0.1952(6) 0.4941(6) 0.6433(5) 0.0168(19) Uani 1 1 d . . . H7A H -0.2469 0.4988 0.6264 0.02 Uiso 1 1 calc R . . H7B H -0.1917 0.4588 0.6883 0.02 Uiso 1 1 calc R . . N81 N -0.1421(5) 0.6495(5) 0.7007(5) 0.0183(16) Uani 1 1 d U . . C82 C -0.1485(6) 0.5774(6) 0.7082(6) 0.0176(17) Uani 1 1 d U . . N83 N -0.1910(5) 0.5699(5) 0.6592(5) 0.0198(17) Uani 1 1 d U . . C83A C -0.2201(6) 0.6407(6) 0.6215(5) 0.0168(19) Uani 1 1 d . . . C84 C -0.2746(6) 0.6644(6) 0.5703(6) 0.0179(18) Uani 1 1 d U . . O84 O -0.3101(5) 0.6117(4) 0.5523(4) 0.0220(16) Uani 1 1 d . . . C841 C -0.3574(7) 0.6368(7) 0.4927(6) 0.028(3) Uani 1 1 d . . . H84A H -0.3234 0.6464 0.447 0.034 Uiso 1 1 calc R . . H84B H -0.3989 0.6847 0.5027 0.034 Uiso 1 1 calc R . . C842 C -0.3951(7) 0.5743(7) 0.4863(7) 0.032(3) Uani 1 1 d . . . H84C H -0.4315 0.5921 0.4488 0.039 Uiso 1 1 calc R . . H84D H -0.4276 0.5653 0.5331 0.039 Uiso 1 1 calc R . . C843 C -0.3380(8) 0.4989(8) 0.4669(9) 0.040(3) Uani 1 1 d . . . H84E H -0.3032 0.5076 0.4214 0.048 Uiso 1 1 calc R . . H84F H -0.3039 0.4784 0.5059 0.048 Uiso 1 1 calc R . . C844 C -0.3807(9) 0.4411(9) 0.4569(9) 0.048(4) Uani 1 1 d . . . H84G H -0.4091 0.4268 0.5037 0.072 Uiso 1 1 calc R . . H84H H -0.342 0.3957 0.4385 0.072 Uiso 1 1 calc R . . H84I H -0.4187 0.4632 0.4221 0.072 Uiso 1 1 calc R . . C85 C -0.2916(7) 0.7410(6) 0.5446(6) 0.025(2) Uani 1 1 d U . . H85 H -0.3252 0.7588 0.5075 0.03 Uiso 1 1 calc R . . C86 C -0.2602(7) 0.7935(6) 0.5722(6) 0.026(2) Uani 1 1 d . . . H86 H -0.2742 0.8458 0.5541 0.031 Uiso 1 1 calc R . . C87 C -0.2097(6) 0.7702(6) 0.6248(5) 0.018(2) Uani 1 1 d . . . O87 O -0.1787(5) 0.8173(4) 0.6559(4) 0.0243(16) Uani 1 1 d U . . C871 C -0.2013(8) 0.8984(6) 0.6320(5) 0.025(2) Uani 1 1 d U . . H87A H -0.2596 0.9192 0.6415 0.03 Uiso 1 1 calc R . . H87B H -0.1843 0.907 0.5792 0.03 Uiso 1 1 calc R . . C872 C -0.1595(8) 0.9370(6) 0.6752(6) 0.028(2) Uani 1 1 d U . . H87C H -0.1017 0.9127 0.6683 0.034 Uiso 1 1 calc R . . H87D H -0.1791 0.9301 0.7276 0.034 Uiso 1 1 calc R . . C873 C -0.1746(8) 1.0221(7) 0.6509(8) 0.034(2) Uani 1 1 d U . . H87E H -0.2327 1.0456 0.6547 0.041 Uiso 1 1 calc R . . H87F H -0.1522 1.0288 0.5992 0.041 Uiso 1 1 calc R . . C874 C -0.1372(9) 1.0639(8) 0.6971(8) 0.040(3) Uani 1 1 d . . . H87G H -0.1651 1.0644 0.7467 0.06 Uiso 1 1 calc R . . H87H H -0.1418 1.1165 0.6756 0.06 Uiso 1 1 calc R . . H87I H -0.081 1.0371 0.6981 0.06 Uiso 1 1 calc R . . C87A C -0.1875(6) 0.6917(6) 0.6466(5) 0.0170(19) Uani 1 1 d . . . C8 C -0.0907(6) 0.6774(6) 0.7405(5) 0.0174(19) Uani 1 1 d . . . H8A H -0.0883 0.6489 0.7893 0.021 Uiso 1 1 calc R . . H8B H -0.1151 0.7321 0.7474 0.021 Uiso 1 1 calc R . . C101 C 1.3179(9) 0.7719(9) 0.3416(8) 0.042(3) Uani 1 1 d . . . H101 H 1.3581 0.7938 0.315 0.05 Uiso 1 1 calc R . . C102 C 1.2806(9) 0.7355(10) 0.3057(8) 0.051(4) Uani 1 1 d . . . H102 H 1.296 0.7295 0.2553 0.061 Uiso 1 1 calc R . . C103 C 1.2184(8) 0.7066(8) 0.3444(9) 0.042(3) Uani 1 1 d . . . H103 H 1.1901 0.682 0.3204 0.05 Uiso 1 1 calc R . . C104 C 1.1992(10) 0.7147(9) 0.4173(8) 0.049(4) Uani 1 1 d . . . H104 H 1.1589 0.6934 0.4445 0.058 Uiso 1 1 calc R . . C105 C 1.2380(10) 0.7535(9) 0.4520(9) 0.047(4) Uani 1 1 d . . . H105 H 1.2213 0.7628 0.5016 0.056 Uiso 1 1 calc R . . C106 C 1.3001(8) 0.7783(7) 0.4143(7) 0.035(3) Uani 1 1 d . . . H106 H 1.3308 0.7999 0.4386 0.042 Uiso 1 1 calc R . . C201 C 0.9350(9) 0.2788(8) 0.1390(7) 0.036(3) Uani 1 1 d . . . H201 H 0.9729 0.2951 0.1594 0.043 Uiso 1 1 calc R . . C202 C 0.8824(9) 0.2444(9) 0.1835(7) 0.043(3) Uani 1 1 d . . . H202 H 0.8815 0.239 0.2348 0.052 Uiso 1 1 calc R . . C203 C 0.8305(10) 0.2177(10) 0.1514(8) 0.053(4) Uani 1 1 d . . . H203 H 0.7939 0.1937 0.1813 0.063 Uiso 1 1 calc R . . C204 C 0.8312(11) 0.2254(10) 0.0778(9) 0.058(5) Uani 1 1 d . . . H204 H 0.7973 0.2046 0.0564 0.069 Uiso 1 1 calc R . . C205 C 0.8811(10) 0.2634(9) 0.0353(8) 0.046(4) Uani 1 1 d . . . H205 H 0.8795 0.2717 -0.0157 0.055 Uiso 1 1 calc R . . C206 C 0.9331(9) 0.2896(8) 0.0647(6) 0.034(3) Uani 1 1 d . . . H206 H 0.968 0.3153 0.0343 0.041 Uiso 1 1 calc R . . C301 C 0.4795(9) 0.6211(9) 0.2515(9) 0.048(4) Uani 1 1 d . . . H301 H 0.5064 0.6591 0.2534 0.057 Uiso 1 1 calc R . . C302 C 0.4522(9) 0.5822(11) 0.3148(8) 0.051(4) Uani 1 1 d . . . H302 H 0.4604 0.5937 0.3606 0.061 Uiso 1 1 calc R . . C303 C 0.4138(10) 0.5277(11) 0.3117(9) 0.058(5) Uani 1 1 d . . . H303 H 0.3958 0.5013 0.3555 0.07 Uiso 1 1 calc R . . C304 C 0.4013(9) 0.5111(8) 0.2484(9) 0.047(4) Uani 1 1 d . . . H304 H 0.3753 0.4724 0.2472 0.057 Uiso 1 1 calc R . . C305 C 0.4262(11) 0.5501(9) 0.1835(10) 0.055(4) Uani 1 1 d . . . H305 H 0.4151 0.5398 0.1383 0.066 Uiso 1 1 calc R . . C306 C 0.4667(10) 0.6034(7) 0.1861(8) 0.045(4) Uani 1 1 d . . . H306 H 0.4862 0.6284 0.1422 0.053 Uiso 1 1 calc R . . C401 C 0.2927(11) 0.7986(13) 0.0756(9) 0.065(6) Uani 1 1 d . . . H401 H 0.3343 0.8181 0.0485 0.079 Uiso 1 1 calc R . . C402 C 0.2989(11) 0.7193(12) 0.0835(10) 0.063(5) Uani 1 1 d . . . H402 H 0.3442 0.6856 0.0596 0.075 Uiso 1 1 calc R . . C403 C 0.2423(10) 0.6908(11) 0.1241(9) 0.055(4) Uani 1 1 d . . . H403 H 0.2495 0.6371 0.1321 0.066 Uiso 1 1 calc R . . C404 C 0.1756(11) 0.7381(13) 0.1533(10) 0.061(5) Uani 1 1 d . . . H404 H 0.1347 0.7168 0.1791 0.073 Uiso 1 1 calc R . . C405 C 0.1638(12) 0.8148(13) 0.1477(11) 0.067(5) Uani 1 1 d . . . H405 H 0.1157 0.8463 0.1697 0.081 Uiso 1 1 calc R . . C406 C 0.2238(12) 0.8478(12) 0.1085(12) 0.069(6) Uani 1 1 d . . . H406 H 0.2176 0.9014 0.1047 0.083 Uiso 1 1 calc R . . C501 C 0.7490(11) 1.0476(10) 0.3685(12) 0.060(5) Uani 1 1 d . . . H501 H 0.6998 1.0355 0.37 0.073 Uiso 1 1 calc R . . C502 C 0.7972(12) 1.0487(10) 0.3068(10) 0.057(5) Uani 1 1 d . . . H502 H 0.7828 1.0352 0.2645 0.068 Uiso 1 1 calc R . . C503 C 0.8673(12) 1.0686(9) 0.3018(9) 0.056(5) Uani 1 1 d . . . H503 H 0.9002 1.0701 0.2565 0.067 Uiso 1 1 calc R . . C504 C 0.8884(11) 1.0858(9) 0.3616(11) 0.056(4) Uani 1 1 d . . . H504 H 0.9371 1.0991 0.3588 0.067 Uiso 1 1 calc R . . C505 C 0.8410(11) 1.0844(9) 0.4266(8) 0.049(4) Uani 1 1 d . . . H505 H 0.8563 1.0974 0.4687 0.058 Uiso 1 1 calc R . . C506 C 0.7714(12) 1.0644(10) 0.4309(10) 0.068(6) Uani 1 1 d . . . H506 H 0.7386 1.062 0.4761 0.082 Uiso 1 1 calc R . . N601 N 0.9155(7) 0.6248(6) -0.0721(5) 0.032(2) Uani 1 1 d . . . C601 C 0.9039(6) 0.5825(7) -0.0268(6) 0.024(2) Uani 1 1 d . . . C602 C 0.8915(10) 0.5287(9) 0.0379(8) 0.051(4) Uani 1 1 d . . . H60A H 0.9404 0.5105 0.0608 0.077 Uiso 1 1 calc R . . H60B H 0.8777 0.4851 0.0228 0.077 Uiso 1 1 calc R . . H60C H 0.8481 0.5549 0.0728 0.077 Uiso 1 1 calc R . . N701 N 0.6311(7) 0.9189(6) 0.4272(5) 0.032(2) Uani 1 1 d . . . C701 C 0.5861(8) 0.9055(6) 0.4733(6) 0.028(3) Uani 1 1 d . . . C702 C 0.5294(8) 0.8891(8) 0.5328(7) 0.037(3) Uani 1 1 d . . . H70A H 0.5573 0.8604 0.5731 0.056 Uiso 1 1 calc R . . H70B H 0.4984 0.8585 0.5171 0.056 Uiso 1 1 calc R . . H70C H 0.4936 0.9371 0.5489 0.056 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 0.0202(4) 0.0157(3) 0.0121(3) -0.0008(3) -0.0021(3) -0.0022(3) Pd2 0.0188(4) 0.0161(3) 0.0113(3) -0.0001(3) -0.0032(3) -0.0027(3) Br11 0.0236(5) 0.0195(5) 0.0207(5) 0.0029(4) -0.0023(4) -0.0028(4) Br12 0.0254(6) 0.0239(5) 0.0199(5) -0.0007(4) 0.0013(4) -0.0017(4) Br21 0.0301(6) 0.0225(5) 0.0191(5) 0.0035(4) -0.0025(4) -0.0020(4) Br22 0.0234(5) 0.0223(5) 0.0228(5) -0.0002(4) 0.0037(4) -0.0018(4) C11 0.019(5) 0.016(5) 0.026(5) -0.012(4) -0.008(4) 0.006(4) C12 0.024(5) 0.019(5) 0.031(6) -0.007(4) -0.013(5) -0.007(4) C13 0.028(6) 0.014(4) 0.024(5) -0.006(4) -0.009(4) -0.011(4) C14 0.029(6) 0.022(5) 0.039(7) -0.003(5) -0.012(5) -0.016(5) C15 0.030(6) 0.036(7) 0.033(6) -0.001(5) -0.005(5) -0.015(5) C16 0.029(6) 0.036(6) 0.023(5) -0.006(5) -0.009(5) -0.009(5) C1 0.024(5) 0.012(4) 0.018(5) -0.007(4) -0.004(4) -0.004(4) N21 0.024(4) 0.011(4) 0.018(4) -0.011(3) -0.006(3) 0.002(3) C22 0.026(6) 0.011(4) 0.028(6) 0.002(4) -0.013(4) -0.004(4) N23 0.016(4) 0.017(4) 0.009(3) 0.000(3) -0.002(3) 0.000(3) C23A 0.025(5) 0.012(4) 0.011(4) 0.000(3) -0.002(4) 0.000(4) C24 0.028(6) 0.023(5) 0.010(4) 0.001(4) -0.004(4) -0.009(4) O24 0.029(4) 0.025(4) 0.021(4) -0.010(3) 0.002(3) -0.009(3) C241 0.041(7) 0.042(7) 0.014(5) -0.013(5) -0.001(5) -0.009(6) C242 0.048(8) 0.046(8) 0.035(7) -0.014(6) -0.003(6) -0.028(7) C243 0.054(10) 0.049(9) 0.047(9) -0.008(7) -0.006(7) -0.023(8) C244 0.061(11) 0.069(12) 0.063(11) -0.017(9) -0.028(9) -0.007(9) C25 0.029(6) 0.022(5) 0.019(5) -0.009(4) -0.001(4) 0.003(4) C26 0.024(6) 0.029(6) 0.013(5) -0.002(4) 0.006(4) 0.004(4) C27 0.032(6) 0.018(5) 0.016(5) -0.008(4) -0.003(4) -0.003(4) O27 0.021(4) 0.029(4) 0.015(3) -0.005(3) -0.001(3) -0.005(3) C271 0.023(6) 0.021(5) 0.043(7) -0.002(5) -0.011(5) 0.004(4) C272 0.021(6) 0.051(8) 0.041(7) -0.011(6) -0.003(5) -0.002(6) C273 0.034(7) 0.054(9) 0.038(7) 0.009(6) -0.007(6) -0.021(7) C274 0.055(10) 0.061(10) 0.047(9) -0.001(8) -0.010(8) -0.022(8) C27A 0.021(5) 0.020(5) 0.007(4) -0.004(4) 0.002(4) 0.001(4) C2 0.021(5) 0.025(5) 0.016(5) 0.003(4) -0.003(4) -0.017(4) C31 0.014(5) 0.027(5) 0.018(5) 0.006(4) -0.006(4) -0.016(4) C32 0.018(5) 0.021(5) 0.012(4) -0.001(4) 0.001(4) -0.010(4) C33 0.030(6) 0.029(5) 0.015(5) -0.004(4) -0.007(4) -0.014(5) C34 0.025(5) 0.033(6) 0.011(4) -0.006(4) -0.004(4) -0.015(5) C35 0.017(5) 0.038(6) 0.032(6) 0.004(5) -0.009(5) -0.010(5) C36 0.029(6) 0.025(5) 0.020(5) 0.002(4) -0.009(4) -0.010(5) C3 0.017(5) 0.024(5) 0.021(5) 0.004(4) 0.001(4) -0.006(4) N41 0.022(4) 0.012(3) 0.023(4) -0.006(3) -0.008(3) 0.000(3) C42 0.024(4) 0.019(4) 0.018(4) -0.013(3) -0.008(3) 0.000(3) N43 0.019(4) 0.013(4) 0.027(4) 0.007(3) -0.010(3) 0.000(3) C43A 0.025(5) 0.020(5) 0.013(4) 0.001(4) 0.009(4) -0.006(4) C44 0.021(5) 0.021(4) 0.021(5) 0.009(4) 0.007(4) -0.005(4) O44 0.019(4) 0.029(4) 0.039(5) 0.013(4) -0.006(3) -0.001(3) C441 0.037(7) 0.029(6) 0.018(5) -0.001(4) -0.009(5) 0.002(5) C442 0.026(6) 0.040(7) 0.041(7) 0.007(6) -0.011(5) -0.007(5) C443 0.072(13) 0.052(10) 0.066(12) 0.018(9) -0.031(10) -0.016(9) C444 0.073(13) 0.065(12) 0.062(12) 0.011(10) -0.008(10) -0.015(10) C45 0.026(5) 0.021(4) 0.020(5) 0.005(4) 0.000(4) 0.002(4) C46 0.026(6) 0.014(5) 0.028(6) 0.005(4) 0.012(4) -0.002(4) C47 0.025(5) 0.016(5) 0.018(5) -0.002(4) 0.009(4) 0.001(4) O47 0.032(4) 0.012(3) 0.037(5) -0.009(3) -0.011(4) -0.001(3) C471 0.043(7) 0.016(5) 0.035(7) -0.009(5) -0.003(6) 0.000(5) C472 0.091(10) 0.028(6) 0.103(11) -0.033(7) -0.060(9) 0.001(6) C473 0.092(10) 0.041(7) 0.121(11) -0.038(7) -0.073(9) 0.012(6) C474 0.102(11) 0.058(8) 0.137(13) -0.046(9) -0.082(10) 0.018(8) C47A 0.025(5) 0.018(5) 0.018(5) -0.003(4) 0.002(4) -0.002(4) C4 0.028(6) 0.014(4) 0.020(5) -0.003(4) -0.008(4) -0.005(4) C51 0.021(5) 0.014(4) 0.016(4) -0.007(4) -0.002(4) -0.007(4) C52 0.026(5) 0.018(5) 0.017(5) -0.005(4) -0.005(4) -0.012(4) C53 0.025(5) 0.019(5) 0.019(5) 0.000(4) -0.001(4) -0.005(4) C54 0.027(6) 0.021(5) 0.032(6) -0.003(5) 0.000(5) -0.013(5) C55 0.020(5) 0.037(6) 0.033(6) -0.004(5) 0.003(5) -0.015(5) C56 0.026(6) 0.026(5) 0.021(5) 0.000(4) -0.004(4) -0.011(5) C5 0.022(5) 0.023(5) 0.011(4) -0.006(4) -0.006(4) -0.006(4) N61 0.016(3) 0.015(3) 0.017(3) -0.002(2) -0.004(2) 0.007(2) C62 0.016(4) 0.017(4) 0.004(3) 0.001(3) -0.004(3) 0.000(3) N63 0.016(3) 0.015(3) 0.017(3) -0.002(2) -0.004(2) 0.007(2) C63A 0.023(5) 0.024(5) 0.019(5) 0.002(4) -0.001(4) -0.004(4) C64 0.024(5) 0.022(5) 0.023(5) 0.005(4) 0.001(4) 0.000(4) O64 0.031(5) 0.021(4) 0.031(4) -0.004(3) -0.004(4) -0.003(3) C641 0.040(7) 0.030(6) 0.028(6) -0.007(5) -0.007(5) 0.009(5) C642 0.062(8) 0.042(7) 0.141(14) -0.044(8) -0.030(9) 0.004(7) C643 0.070(8) 0.043(7) 0.143(13) -0.034(8) -0.024(9) -0.009(7) C644 0.061(9) 0.042(7) 0.130(14) -0.017(8) -0.032(9) -0.004(7) C65 0.025(5) 0.024(5) 0.033(5) -0.001(4) 0.000(4) -0.005(4) C66 0.023(6) 0.026(6) 0.031(6) 0.006(5) -0.001(5) 0.011(5) C67 0.019(5) 0.029(5) 0.017(5) 0.006(4) -0.007(4) -0.008(4) O67 0.023(4) 0.045(5) 0.055(5) -0.025(4) -0.017(4) 0.002(4) C671 0.034(5) 0.060(6) 0.066(6) -0.027(5) -0.022(5) -0.006(5) C67A 0.023(5) 0.024(5) 0.015(5) 0.009(4) -0.005(4) -0.005(4) C6 0.034(6) 0.019(5) 0.015(5) -0.001(4) -0.005(4) -0.003(4) C71 0.017(5) 0.012(4) 0.018(5) -0.004(4) -0.002(4) -0.009(4) C72 0.026(5) 0.015(4) 0.011(4) 0.002(4) -0.004(4) -0.006(4) C73 0.021(5) 0.021(5) 0.018(5) -0.008(4) -0.007(4) -0.007(4) C74 0.028(6) 0.019(5) 0.022(5) -0.009(4) -0.002(4) -0.012(4) C75 0.027(6) 0.020(5) 0.015(5) -0.006(4) 0.004(4) -0.008(4) C76 0.027(6) 0.019(5) 0.018(5) -0.003(4) -0.007(4) -0.006(4) C7 0.018(5) 0.017(4) 0.015(4) -0.001(4) -0.002(4) -0.003(4) N81 0.014(4) 0.015(3) 0.021(4) -0.004(3) -0.006(3) 0.009(3) C82 0.011(4) 0.017(4) 0.022(4) -0.010(3) -0.001(3) 0.004(3) N83 0.019(4) 0.020(4) 0.019(4) 0.000(3) -0.007(3) -0.001(3) C83A 0.021(5) 0.017(4) 0.011(4) -0.003(4) -0.003(4) -0.003(4) C84 0.017(4) 0.019(4) 0.019(4) -0.003(4) -0.008(4) -0.003(4) O84 0.025(4) 0.024(4) 0.020(4) -0.002(3) -0.014(3) -0.005(3) C841 0.032(6) 0.032(6) 0.023(5) 0.009(5) -0.017(5) -0.013(5) C842 0.027(6) 0.037(7) 0.036(7) 0.007(5) -0.014(5) -0.013(5) C843 0.025(6) 0.042(7) 0.062(9) -0.020(7) -0.009(6) -0.014(6) C844 0.044(9) 0.042(8) 0.060(10) -0.011(7) -0.022(8) -0.003(7) C85 0.022(5) 0.025(5) 0.023(5) 0.003(4) -0.012(4) 0.004(4) C86 0.030(6) 0.013(5) 0.029(6) -0.003(4) -0.007(5) 0.006(4) C87 0.015(5) 0.019(5) 0.017(5) -0.005(4) 0.002(4) 0.000(4) O87 0.035(4) 0.016(3) 0.022(4) 0.000(3) -0.006(3) -0.006(3) C871 0.044(5) 0.023(4) 0.008(4) -0.001(3) -0.007(4) -0.009(4) C872 0.041(5) 0.024(4) 0.020(4) -0.004(4) -0.008(4) -0.005(4) C873 0.040(6) 0.025(5) 0.039(6) -0.004(5) -0.014(5) -0.007(5) C874 0.054(9) 0.032(7) 0.042(8) -0.012(6) -0.012(7) -0.016(6) C87A 0.022(5) 0.018(4) 0.011(4) -0.003(4) -0.002(4) -0.002(4) C8 0.017(5) 0.021(5) 0.014(4) -0.008(4) -0.007(4) 0.001(4) C101 0.034(7) 0.053(9) 0.043(8) -0.008(7) -0.011(6) -0.015(7) C102 0.044(9) 0.070(11) 0.030(7) -0.004(7) 0.004(6) -0.004(8) C103 0.033(7) 0.035(7) 0.058(9) -0.013(7) -0.011(7) -0.004(6) C104 0.059(10) 0.053(9) 0.042(8) -0.018(7) 0.004(7) -0.028(8) C105 0.053(10) 0.048(9) 0.042(8) -0.002(7) -0.002(7) -0.022(8) C106 0.038(7) 0.032(6) 0.035(7) -0.005(5) -0.006(6) -0.010(6) C201 0.047(8) 0.043(7) 0.021(6) -0.005(5) -0.009(5) -0.011(6) C202 0.049(9) 0.051(8) 0.020(6) 0.005(6) 0.003(6) -0.007(7) C203 0.055(10) 0.071(11) 0.036(8) 0.017(8) -0.001(7) -0.035(9) C204 0.075(12) 0.072(11) 0.042(8) 0.023(8) -0.022(8) -0.051(10) C205 0.060(10) 0.063(10) 0.027(7) 0.015(7) -0.018(6) -0.040(8) C206 0.049(8) 0.041(7) 0.016(5) 0.005(5) -0.010(5) -0.017(6) C301 0.035(8) 0.049(9) 0.056(10) -0.016(7) -0.005(7) 0.000(7) C302 0.036(8) 0.081(12) 0.029(7) -0.011(7) -0.010(6) 0.002(8) C303 0.042(9) 0.078(12) 0.043(9) 0.011(9) -0.006(7) -0.003(9) C304 0.046(9) 0.036(7) 0.062(10) 0.008(7) -0.014(8) -0.015(7) C305 0.077(12) 0.040(8) 0.054(10) -0.007(7) -0.023(9) -0.014(8) C306 0.069(11) 0.023(6) 0.040(8) -0.005(6) -0.007(7) -0.009(6) C401 0.068(12) 0.119(17) 0.040(9) -0.013(10) 0.001(8) -0.076(13) C402 0.045(10) 0.097(15) 0.055(11) -0.034(10) 0.001(8) -0.025(10) C403 0.043(9) 0.068(11) 0.052(10) 0.001(8) -0.008(8) -0.015(8) C404 0.043(10) 0.095(15) 0.051(10) 0.001(10) -0.011(8) -0.029(10) C405 0.054(11) 0.079(14) 0.067(12) -0.018(11) -0.002(9) -0.013(10) C406 0.060(12) 0.067(12) 0.097(16) -0.032(11) -0.026(11) -0.023(10) C501 0.048(10) 0.048(9) 0.090(15) 0.013(10) -0.030(10) -0.018(8) C502 0.074(12) 0.053(10) 0.055(10) -0.018(8) -0.034(10) -0.016(9) C503 0.082(13) 0.038(8) 0.033(8) -0.004(6) 0.007(8) 0.002(8) C504 0.054(10) 0.041(8) 0.074(12) 0.002(8) -0.013(9) -0.017(8) C505 0.070(11) 0.049(9) 0.024(7) -0.003(6) -0.012(7) -0.009(8) C506 0.069(12) 0.048(9) 0.048(10) 0.019(8) 0.024(9) 0.022(9) N601 0.040(6) 0.038(6) 0.017(5) -0.006(4) 0.000(4) -0.012(5) C601 0.020(5) 0.033(6) 0.021(5) -0.016(5) -0.001(4) -0.005(5) C602 0.064(11) 0.043(8) 0.031(7) 0.007(6) 0.006(7) -0.001(7) N701 0.041(6) 0.034(5) 0.019(5) 0.004(4) -0.010(4) -0.008(5) C701 0.040(7) 0.018(5) 0.024(6) -0.002(4) -0.012(5) 0.001(5) C702 0.036(7) 0.039(7) 0.027(6) 0.008(5) -0.006(5) 0.003(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C42 1.950(11) . ? Pd1 C22 1.969(12) . ? Pd1 Br12 2.4778(15) . ? Pd1 Br11 2.4782(15) . ? Pd2 C82 1.982(10) . ? Pd2 C62 1.983(9) . ? Pd2 Br21 2.4696(14) . ? Pd2 Br22 2.4750(15) . ? C11 C16 1.354(16) . ? C11 C12 1.403(14) . ? C11 C1 1.519(14) . ? C12 C13 1.421(15) . ? C12 C4 1.525(16) . ? C13 C14 1.362(17) . ? C13 H13 0.95 . ? C14 C15 1.393(17) . ? C14 H14 0.95 . ? C15 C16 1.392(17) . ? C15 H15 0.95 . ? C16 H16 0.95 . ? C1 N21 1.493(12) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? N21 C22 1.348(14) . ? N21 C27A 1.404(12) . ? C22 N23 1.326(13) . ? N23 C23A 1.409(13) . ? N23 C2 1.478(13) . ? C23A C27A 1.369(15) . ? C23A C24 1.434(14) . ? C24 O24 1.358(13) . ? C24 C25 1.384(16) . ? O24 C241 1.422(13) . ? C241 C242 1.550(18) . ? C241 H24A 0.99 . ? C241 H24B 0.99 . ? C242 C243 1.51(2) . ? C242 H24C 0.99 . ? C242 H24D 0.99 . ? C243 C244 1.59(2) . ? C243 H24E 0.99 . ? C243 H24F 0.99 . ? C244 H24G 0.98 . ? C244 H24H 0.98 . ? C244 H24I 0.98 . ? C25 C26 1.397(17) . ? C25 H25 0.95 . ? C26 C27 1.367(15) . ? C26 H26 0.95 . ? C27 O27 1.376(13) . ? C27 C27A 1.405(15) . ? O27 C271 1.431(14) . ? C271 C272 1.529(18) . ? C271 H27A 0.99 . ? C271 H27B 0.99 . ? C272 C273 1.48(2) . ? C272 H27C 0.99 . ? C272 H27D 0.99 . ? C273 C274 1.52(2) . ? C273 H27E 0.99 . ? C273 H27F 0.99 . ? C274 H27G 0.98 . ? C274 H27H 0.98 . ? C274 H27I 0.98 . ? C2 C32 1.517(14) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C31 C36 1.390(14) . ? C31 C32 1.395(15) . ? C31 C3 1.536(15) . ? C32 C33 1.399(14) . ? C33 C34 1.390(15) . ? C33 H33 0.95 . ? C34 C35 1.361(16) . ? C34 H34 0.95 . ? C35 C36 1.385(16) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C3 N43 1.466(14) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? N41 C42 1.375(13) . ? N41 C47A 1.386(13) . ? N41 C4 1.469(13) . ? C42 N43 1.346(13) . ? N43 C43A 1.419(13) . ? C43A C47A 1.388(16) . ? C43A C44 1.422(15) . ? C44 C45 1.377(15) . ? C44 O44 1.383(15) . ? O44 C441 1.435(13) . ? C441 C442 1.507(18) . ? C441 H44A 0.99 . ? C441 H44B 0.99 . ? C442 C443 1.48(2) . ? C442 H44C 0.99 . ? C442 H44D 0.99 . ? C443 C444 1.47(3) . ? C443 H44E 0.99 . ? C443 H44F 0.99 . ? C444 H44G 0.98 . ? C444 H44H 0.98 . ? C444 H44I 0.98 . ? C45 C46 1.401(17) . ? C45 H45 0.95 . ? C46 C47 1.361(15) . ? C46 H46 0.95 . ? C47 C47A 1.390(14) . ? C47 O47 1.392(14) . ? O47 C471 1.426(13) . ? C471 C472 1.53(2) . ? C471 H47A 0.99 . ? C471 H47B 0.99 . ? C472 C473 1.51(3) . ? C472 H47C 0.99 . ? C472 H47D 0.99 . ? C473 C474 1.53(2) . ? C473 H47E 0.99 . ? C473 H47F 0.99 . ? C474 H47G 0.98 . ? C474 H47H 0.98 . ? C474 H47I 0.98 . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C51 C52 1.403(14) . ? C51 C56 1.405(15) . ? C51 C5 1.496(14) . ? C52 C53 1.423(14) . ? C52 C8 1.533(15) . ? C53 C54 1.365(16) . ? C53 H53 0.95 . ? C54 C55 1.358(17) . ? C54 H54 0.95 . ? C55 C56 1.366(16) . ? C55 H55 0.95 . ? C56 H56 0.95 . ? C5 N61 1.484(13) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? N61 C62 1.327(13) . ? N61 C67A 1.407(13) . ? C62 N63 1.342(12) . ? N63 C63A 1.382(14) . ? N63 C6 1.487(14) . ? C63A C67A 1.377(16) . ? C63A C64 1.399(15) . ? C64 O64 1.350(14) . ? C64 C65 1.409(16) . ? O64 C641 1.457(14) . ? C641 C642 1.46(2) . ? C641 H64A 0.99 . ? C641 H64B 0.99 . ? C642 C643 1.38(3) . ? C642 H64C 0.99 . ? C642 H64D 0.99 . ? C643 C644 1.61(3) . ? C643 H64E 0.99 . ? C643 H64F 0.99 . ? C644 H64G 0.98 . ? C644 H64H 0.98 . ? C644 H64I 0.98 . ? C65 C66 1.384(18) . ? C65 H65 0.95 . ? C66 C67 1.410(16) . ? C66 H66 0.95 . ? C67 O67 1.350(14) . ? C67 C67A 1.434(15) . ? O67 C671 1.456(16) . ? C671 C672 1.50(3) . ? C671 C675 1.62(2) . ? C671 H67A 0.99 . ? C671 H67B 0.99 . ? C671 H67J 0.99 . ? C671 H67K 0.99 . ? C672 C673 1.51(3) . ? C672 H67K 1.2819 . ? C672 H67C 0.99 . ? C672 H67D 0.99 . ? C673 C674 1.50(3) . ? C673 H67E 0.99 . ? C673 H67F 0.99 . ? C674 H67G 0.98 . ? C674 H67H 0.98 . ? C674 H67I 0.98 . ? C675 C676 1.53(3) . ? C675 H67L 0.99 . ? C675 H67M 0.99 . ? C676 C677 1.55(3) . ? C676 H67N 0.99 . ? C676 H67O 0.99 . ? C677 H67P 0.98 . ? C677 H67Q 0.98 . ? C677 H67R 0.98 . ? C6 C72 1.527(14) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C71 C76 1.396(14) . ? C71 C72 1.397(14) . ? C71 C7 1.522(14) . ? C72 C73 1.404(14) . ? C73 C74 1.375(15) . ? C73 H73 0.95 . ? C74 C75 1.363(15) . ? C74 H74 0.95 . ? C75 C76 1.371(15) . ? C75 H75 0.95 . ? C76 H76 0.95 . ? C7 N83 1.478(13) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? N81 C82 1.341(13) . ? N81 C87A 1.405(13) . ? N81 C8 1.487(13) . ? C82 N83 1.316(13) . ? N83 C83A 1.396(13) . ? C83A C87A 1.385(14) . ? C83A C84 1.408(14) . ? C84 O84 1.384(12) . ? C84 C85 1.386(15) . ? O84 C841 1.449(12) . ? C841 C842 1.498(17) . ? C841 H84A 0.99 . ? C841 H84B 0.99 . ? C842 C843 1.513(18) . ? C842 H84C 0.99 . ? C842 H84D 0.99 . ? C843 C844 1.500(19) . ? C843 H84E 0.99 . ? C843 H84F 0.99 . ? C844 H84G 0.98 . ? C844 H84H 0.98 . ? C844 H84I 0.98 . ? C85 C86 1.417(17) . ? C85 H85 0.95 . ? C86 C87 1.381(15) . ? C86 H86 0.95 . ? C87 O87 1.369(13) . ? C87 C87A 1.401(14) . ? O87 C871 1.454(13) . ? C871 C872 1.523(16) . ? C871 H87A 0.99 . ? C871 H87B 0.99 . ? C872 C873 1.524(16) . ? C872 H87C 0.99 . ? C872 H87D 0.99 . ? C873 C874 1.549(17) . ? C873 H87E 0.99 . ? C873 H87F 0.99 . ? C874 H87G 0.98 . ? C874 H87H 0.98 . ? C874 H87I 0.98 . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C101 C102 1.35(2) . ? C101 C106 1.359(19) . ? C101 H101 0.95 . ? C102 C103 1.41(2) . ? C102 H102 0.95 . ? C103 C104 1.37(2) . ? C103 H103 0.95 . ? C104 C105 1.39(2) . ? C104 H104 0.95 . ? C105 C106 1.36(2) . ? C105 H105 0.95 . ? C106 H106 0.95 . ? C201 C202 1.38(2) . ? C201 C206 1.381(16) . ? C201 H201 0.95 . ? C202 C203 1.39(2) . ? C202 H202 0.95 . ? C203 C204 1.36(2) . ? C203 H203 0.95 . ? C204 C205 1.37(2) . ? C204 H204 0.95 . ? C205 C206 1.359(18) . ? C205 H205 0.95 . ? C206 H206 0.95 . ? C301 C306 1.37(2) . ? C301 C302 1.39(2) . ? C301 H301 0.95 . ? C302 C303 1.36(3) . ? C302 H302 0.95 . ? C303 C304 1.32(2) . ? C303 H303 0.95 . ? C304 C305 1.40(2) . ? C304 H304 0.95 . ? C305 C306 1.37(2) . ? C305 H305 0.95 . ? C306 H306 0.95 . ? C401 C406 1.40(3) . ? C401 C402 1.41(3) . ? C401 H401 0.95 . ? C402 C403 1.34(2) . ? C402 H402 0.95 . ? C403 C404 1.34(3) . ? C403 H403 0.95 . ? C404 C405 1.35(3) . ? C404 H404 0.95 . ? C405 C406 1.42(3) . ? C405 H405 0.95 . ? C406 H406 0.95 . ? C501 C502 1.32(3) . ? C501 C506 1.39(3) . ? C501 H501 0.95 . ? C502 C503 1.37(3) . ? C502 H502 0.95 . ? C503 C504 1.33(2) . ? C503 H503 0.95 . ? C504 C505 1.36(2) . ? C504 H504 0.95 . ? C505 C506 1.36(3) . ? C505 H505 0.95 . ? C506 H506 0.95 . ? N601 C601 1.104(15) . ? C601 C602 1.485(18) . ? C602 H60A 0.98 . ? C602 H60B 0.98 . ? C602 H60C 0.98 . ? N701 C701 1.126(16) . ? C701 C702 1.435(18) . ? C702 H70A 0.98 . ? C702 H70B 0.98 . ? C702 H70C 0.98 . ? 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 C42 Pd1 C22 96.0(4) . . ? C42 Pd1 Br12 83.4(3) . . ? C22 Pd1 Br12 177.6(3) . . ? C42 Pd1 Br11 177.1(3) . . ? C22 Pd1 Br11 86.5(3) . . ? Br12 Pd1 Br11 94.04(5) . . ? C82 Pd2 C62 95.6(4) . . ? C82 Pd2 Br21 179.3(3) . . ? C62 Pd2 Br21 84.1(3) . . ? C82 Pd2 Br22 86.5(3) . . ? C62 Pd2 Br22 177.6(3) . . ? Br21 Pd2 Br22 93.85(5) . . ? C16 C11 C12 120.0(11) . . ? C16 C11 C1 117.1(9) . . ? C12 C11 C1 122.9(10) . . ? C11 C12 C13 116.2(11) . . ? C11 C12 C4 125.9(10) . . ? C13 C12 C4 117.9(9) . . ? C14 C13 C12 123.5(10) . . ? C14 C13 H13 118.2 . . ? C12 C13 H13 118.2 . . ? C13 C14 C15 118.7(11) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C16 C15 C14 118.3(12) . . ? C16 C15 H15 120.8 . . ? C14 C15 H15 120.8 . . ? C11 C16 C15 123.2(12) . . ? C11 C16 H16 118.4 . . ? C15 C16 H16 118.4 . . ? N21 C1 C11 112.4(8) . . ? N21 C1 H1A 109.1 . . ? C11 C1 H1A 109.1 . . ? N21 C1 H1B 109.1 . . ? C11 C1 H1B 109.1 . . ? H1A C1 H1B 107.9 . . ? C22 N21 C27A 109.5(8) . . ? C22 N21 C1 123.8(8) . . ? C27A N21 C1 126.4(9) . . ? N23 C22 N21 108.2(9) . . ? N23 C22 Pd1 127.6(8) . . ? N21 C22 Pd1 123.4(8) . . ? C22 N23 C23A 109.3(9) . . ? C22 N23 C2 122.7(9) . . ? C23A N23 C2 127.2(8) . . ? C27A C23A N23 106.8(8) . . ? C27A C23A C24 122.5(10) . . ? N23 C23A C24 130.7(10) . . ? O24 C24 C25 125.6(10) . . ? O24 C24 C23A 119.4(10) . . ? C25 C24 C23A 114.7(10) . . ? C24 O24 C241 114.8(9) . . ? O24 C241 C242 110.1(10) . . ? O24 C241 H24A 109.7 . . ? C242 C241 H24A 109.7 . . ? O24 C241 H24B 109.7 . . ? C242 C241 H24B 109.7 . . ? H24A C241 H24B 108.2 . . ? C243 C242 C241 112.9(11) . . ? C243 C242 H24C 109 . . ? C241 C242 H24C 109 . . ? C243 C242 H24D 109 . . ? C241 C242 H24D 109 . . ? H24C C242 H24D 107.8 . . ? C242 C243 C244 108.7(13) . . ? C242 C243 H24E 110 . . ? C244 C243 H24E 110 . . ? C242 C243 H24F 110 . . ? C244 C243 H24F 110 . . ? H24E C243 H24F 108.3 . . ? C243 C244 H24G 109.5 . . ? C243 C244 H24H 109.5 . . ? H24G C244 H24H 109.5 . . ? C243 C244 H24I 109.5 . . ? H24G C244 H24I 109.5 . . ? H24H C244 H24I 109.5 . . ? C24 C25 C26 122.1(10) . . ? C24 C25 H25 119 . . ? C26 C25 H25 119 . . ? C27 C26 C25 122.8(10) . . ? C27 C26 H26 118.6 . . ? C25 C26 H26 118.6 . . ? C26 C27 O27 125.4(10) . . ? C26 C27 C27A 116.3(10) . . ? O27 C27 C27A 118.2(9) . . ? C27 O27 C271 115.4(8) . . ? O27 C271 C272 106.8(10) . . ? O27 C271 H27A 110.4 . . ? C272 C271 H27A 110.4 . . ? O27 C271 H27B 110.4 . . ? C272 C271 H27B 110.4 . . ? H27A C271 H27B 108.6 . . ? C273 C272 C271 116.1(11) . . ? C273 C272 H27C 108.3 . . ? C271 C272 H27C 108.3 . . ? C273 C272 H27D 108.3 . . ? C271 C272 H27D 108.3 . . ? H27C C272 H27D 107.4 . . ? C272 C273 C274 114.9(13) . . ? C272 C273 H27E 108.5 . . ? C274 C273 H27E 108.5 . . ? C272 C273 H27F 108.5 . . ? C274 C273 H27F 108.5 . . ? H27E C273 H27F 107.5 . . ? C273 C274 H27G 109.5 . . ? C273 C274 H27H 109.5 . . ? H27G C274 H27H 109.5 . . ? C273 C274 H27I 109.5 . . ? H27G C274 H27I 109.5 . . ? H27H C274 H27I 109.5 . . ? C23A C27A N21 106.0(9) . . ? C23A C27A C27 121.5(9) . . ? N21 C27A C27 132.1(10) . . ? N23 C2 C32 110.8(8) . . ? N23 C2 H2A 109.5 . . ? C32 C2 H2A 109.5 . . ? N23 C2 H2B 109.5 . . ? C32 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C36 C31 C32 119.5(10) . . ? C36 C31 C3 116.6(10) . . ? C32 C31 C3 123.9(9) . . ? C31 C32 C33 118.7(9) . . ? C31 C32 C2 124.9(9) . . ? C33 C32 C2 116.4(9) . . ? C34 C33 C32 120.2(11) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C35 C34 C33 121.1(10) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C34 C35 C36 119.0(11) . . ? C34 C35 H35 120.5 . . ? C36 C35 H35 120.5 . . ? C35 C36 C31 121.4(11) . . ? C35 C36 H36 119.3 . . ? C31 C36 H36 119.3 . . ? N43 C3 C31 110.8(8) . . ? N43 C3 H3A 109.5 . . ? C31 C3 H3A 109.5 . . ? N43 C3 H3B 109.5 . . ? C31 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C42 N41 C47A 109.3(9) . . ? C42 N41 C4 121.8(8) . . ? C47A N41 C4 128.7(9) . . ? N43 C42 N41 108.0(9) . . ? N43 C42 Pd1 128.4(8) . . ? N41 C42 Pd1 122.8(7) . . ? C42 N43 C43A 108.6(9) . . ? C42 N43 C3 123.7(9) . . ? C43A N43 C3 127.6(9) . . ? C47A C43A N43 106.8(9) . . ? C47A C43A C44 122.1(10) . . ? N43 C43A C44 131.0(10) . . ? C45 C44 O44 126.8(10) . . ? C45 C44 C43A 115.6(11) . . ? O44 C44 C43A 117.5(9) . . ? C44 O44 C441 117.6(9) . . ? O44 C441 C442 107.6(10) . . ? O44 C441 H44A 110.2 . . ? C442 C441 H44A 110.2 . . ? O44 C441 H44B 110.2 . . ? C442 C441 H44B 110.2 . . ? H44A C441 H44B 108.5 . . ? C443 C442 C441 111.9(12) . . ? C443 C442 H44C 109.2 . . ? C441 C442 H44C 109.2 . . ? C443 C442 H44D 109.2 . . ? C441 C442 H44D 109.2 . . ? H44C C442 H44D 107.9 . . ? C444 C443 C442 114.3(15) . . ? C444 C443 H44E 108.7 . . ? C442 C443 H44E 108.7 . . ? C444 C443 H44F 108.7 . . ? C442 C443 H44F 108.7 . . ? H44E C443 H44F 107.6 . . ? C443 C444 H44G 109.5 . . ? C443 C444 H44H 109.5 . . ? H44G C444 H44H 109.5 . . ? C443 C444 H44I 109.5 . . ? H44G C444 H44I 109.5 . . ? H44H C444 H44I 109.5 . . ? C44 C45 C46 122.4(10) . . ? C44 C45 H45 118.8 . . ? C46 C45 H45 118.8 . . ? C47 C46 C45 121.0(10) . . ? C47 C46 H46 119.5 . . ? C45 C46 H46 119.5 . . ? C46 C47 C47A 118.9(11) . . ? C46 C47 O47 124.9(10) . . ? C47A C47 O47 116.1(9) . . ? C47 O47 C471 119.2(9) . . ? O47 C471 C472 108.1(10) . . ? O47 C471 H47A 110.1 . . ? C472 C471 H47A 110.1 . . ? O47 C471 H47B 110.1 . . ? C472 C471 H47B 110.1 . . ? H47A C471 H47B 108.4 . . ? C473 C472 C471 116.0(14) . . ? C473 C472 H47C 108.3 . . ? C471 C472 H47C 108.3 . . ? C473 C472 H47D 108.3 . . ? C471 C472 H47D 108.3 . . ? H47C C472 H47D 107.4 . . ? C472 C473 C474 111.5(17) . . ? C472 C473 H47E 109.3 . . ? C474 C473 H47E 109.3 . . ? C472 C473 H47F 109.3 . . ? C474 C473 H47F 109.3 . . ? H47E C473 H47F 108 . . ? C473 C474 H47G 109.5 . . ? C473 C474 H47H 109.5 . . ? H47G C474 H47H 109.5 . . ? C473 C474 H47I 109.5 . . ? H47G C474 H47I 109.5 . . ? H47H C474 H47I 109.5 . . ? N41 C47A C43A 106.9(9) . . ? N41 C47A C47 132.9(11) . . ? C43A C47A C47 120.0(10) . . ? N41 C4 C12 110.4(8) . . ? N41 C4 H4A 109.6 . . ? C12 C4 H4A 109.6 . . ? N41 C4 H4B 109.6 . . ? C12 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C52 C51 C56 118.0(9) . . ? C52 C51 C5 124.5(9) . . ? C56 C51 C5 117.4(9) . . ? C51 C52 C53 118.8(10) . . ? C51 C52 C8 124.7(9) . . ? C53 C52 C8 116.5(9) . . ? C54 C53 C52 119.9(10) . . ? C54 C53 H53 120 . . ? C52 C53 H53 120 . . ? C55 C54 C53 121.8(11) . . ? C55 C54 H54 119.1 . . ? C53 C54 H54 119.1 . . ? C54 C55 C56 119.5(11) . . ? C54 C55 H55 120.3 . . ? C56 C55 H55 120.3 . . ? C55 C56 C51 122.0(11) . . ? C55 C56 H56 119 . . ? C51 C56 H56 119 . . ? N61 C5 C51 110.5(8) . . ? N61 C5 H5A 109.5 . . ? C51 C5 H5A 109.5 . . ? N61 C5 H5B 109.5 . . ? C51 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C62 N61 C67A 108.1(8) . . ? C62 N61 C5 122.2(8) . . ? C67A N61 C5 129.4(9) . . ? N61 C62 N63 108.8(8) . . ? N61 C62 Pd2 124.8(7) . . ? N63 C62 Pd2 124.7(7) . . ? C62 N63 C63A 110.0(9) . . ? C62 N63 C6 122.0(8) . . ? C63A N63 C6 127.9(9) . . ? C67A C63A N63 105.6(9) . . ? C67A C63A C64 121.6(11) . . ? N63 C63A C64 132.6(11) . . ? O64 C64 C63A 117.2(10) . . ? O64 C64 C65 126.8(10) . . ? C63A C64 C65 116.0(11) . . ? C64 O64 C641 118.6(9) . . ? O64 C641 C642 108.2(11) . . ? O64 C641 H64A 110.1 . . ? C642 C641 H64A 110.1 . . ? O64 C641 H64B 110.1 . . ? C642 C641 H64B 110.1 . . ? H64A C641 H64B 108.4 . . ? C643 C642 C641 122(2) . . ? C643 C642 H64C 106.9 . . ? C641 C642 H64C 106.9 . . ? C643 C642 H64D 106.9 . . ? C641 C642 H64D 106.9 . . ? H64C C642 H64D 106.7 . . ? C642 C643 C644 110(2) . . ? C642 C643 H64E 109.7 . . ? C644 C643 H64E 109.7 . . ? C642 C643 H64F 109.7 . . ? C644 C643 H64F 109.7 . . ? H64E C643 H64F 108.2 . . ? C643 C644 H64G 109.5 . . ? C643 C644 H64H 109.5 . . ? H64G C644 H64H 109.5 . . ? C643 C644 H64I 109.5 . . ? H64G C644 H64I 109.5 . . ? H64H C644 H64I 109.5 . . ? C66 C65 C64 123.0(11) . . ? C66 C65 H65 118.5 . . ? C64 C65 H65 118.5 . . ? C65 C66 C67 121.7(11) . . ? C65 C66 H66 119.1 . . ? C67 C66 H66 119.1 . . ? O67 C67 C66 126.0(10) . . ? O67 C67 C67A 119.4(10) . . ? C66 C67 C67A 114.6(11) . . ? C67 O67 C671 119.2(10) . . ? O67 C671 C672 103.0(17) . . ? O67 C671 C675 109.4(14) . . ? O67 C671 H67A 111.2 . . ? C672 C671 H67A 111.2 . . ? O67 C671 H67B 111.2 . . ? C672 C671 H67B 111.2 . . ? H67A C671 H67B 109.1 . . ? O67 C671 H67J 109.8 . . ? C675 C671 H67J 110.2 . . ? O67 C671 H67K 109.8 . . ? C675 C671 H67K 109.2 . . ? H67J C671 H67K 108.4 . . ? C671 C672 C673 104(2) . . ? C671 C672 H67C 110.9 . . ? C673 C672 H67C 110.9 . . ? C671 C672 H67D 110.9 . . ? C673 C672 H67D 110.9 . . ? H67C C672 H67D 108.9 . . ? C674 C673 C672 112(3) . . ? C674 C673 H67E 108.0 . . ? C672 C673 H67E 109.3 . . ? C674 C673 H67F 109.3 . . ? C672 C673 H67F 109.3 . . ? H67E C673 H67F 108.0 . . ? C673 C674 H67G 109.5 . . ? C673 C674 H67H 109.5 . . ? H67G C674 H67H 109.5 . . ? C673 C674 H67I 109.5 . . ? H67G C674 H67I 109.5 . . ? H67H C674 H67I 109.5 . . ? C676 C675 C671 108(2) . . ? C676 C675 H67L 110.1 . . ? C671 C675 H67L 110.1 . . ? C676 C675 H67M 110.1 . . ? C671 C675 H67M 110.1 . . ? H67L C675 H67M 108.4 . . ? C675 C676 C677 112(3) . . ? C675 C676 H67N 109.1 . . ? C677 C676 H67N 109.1 . . ? C675 C676 H67O 109.1 . . ? C677 C676 H67O 109.1 . . ? H67N C676 H67O 107.8 . . ? C676 C677 H67P 109.5 . . ? C676 C677 H67Q 109.5 . . ? H67P C677 H67Q 109.5 . . ? C676 C677 H67R 109.5 . . ? H67P C677 H67R 109.5 . . ? H67Q C677 H67R 109.5 . . ? C63A C67A N61 107.4(9) . . ? C63A C67A C67 123.1(10) . . ? N61 C67A C67 129.3(10) . . ? N63 C6 C72 111.8(9) . . ? N63 C6 H6A 109.3 . . ? C72 C6 H6A 109.3 . . ? N63 C6 H6B 109.3 . . ? C72 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? C76 C71 C72 118.5(9) . . ? C76 C71 C7 116.9(9) . . ? C72 C71 C7 124.6(9) . . ? C71 C72 C73 119.1(9) . . ? C71 C72 C6 124.2(9) . . ? C73 C72 C6 116.6(9) . . ? C74 C73 C72 120.3(10) . . ? C74 C73 H73 119.8 . . ? C72 C73 H73 119.8 . . ? C75 C74 C73 120.8(10) . . ? C75 C74 H74 119.6 . . ? C73 C74 H74 119.6 . . ? C74 C75 C76 119.7(10) . . ? C74 C75 H75 120.2 . . ? C76 C75 H75 120.2 . . ? C75 C76 C71 121.6(10) . . ? C75 C76 H76 119.2 . . ? C71 C76 H76 119.2 . . ? N83 C7 C71 110.6(8) . . ? N83 C7 H7A 109.5 . . ? C71 C7 H7A 109.5 . . ? N83 C7 H7B 109.5 . . ? C71 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C82 N81 C87A 109.0(9) . . ? C82 N81 C8 124.4(8) . . ? C87A N81 C8 126.5(9) . . ? N83 C82 N81 108.8(9) . . ? N83 C82 Pd2 126.0(8) . . ? N81 C82 Pd2 124.6(7) . . ? C82 N83 C83A 109.8(9) . . ? C82 N83 C7 121.8(8) . . ? C83A N83 C7 127.9(8) . . ? C87A C83A N83 106.4(8) . . ? C87A C83A C84 121.8(9) . . ? N83 C83A C84 131.7(9) . . ? O84 C84 C85 124.9(9) . . ? O84 C84 C83A 118.8(9) . . ? C85 C84 C83A 116.2(9) . . ? C84 O84 C841 115.9(8) . . ? O84 C841 C842 107.0(9) . . ? O84 C841 H84A 110.3 . . ? C842 C841 H84A 110.3 . . ? O84 C841 H84B 110.3 . . ? C842 C841 H84B 110.3 . . ? H84A C841 H84B 108.6 . . ? C841 C842 C843 115.6(11) . . ? C841 C842 H84C 108.4 . . ? C843 C842 H84C 108.4 . . ? C841 C842 H84D 108.4 . . ? C843 C842 H84D 108.4 . . ? H84C C842 H84D 107.4 . . ? C844 C843 C842 112.1(11) . . ? C844 C843 H84E 109.2 . . ? C842 C843 H84E 109.2 . . ? C844 C843 H84F 109.2 . . ? C842 C843 H84F 109.2 . . ? H84E C843 H84F 107.9 . . ? C843 C844 H84G 109.5 . . ? C843 C844 H84H 109.5 . . ? H84G C844 H84H 109.5 . . ? C843 C844 H84I 109.5 . . ? H84G C844 H84I 109.5 . . ? H84H C844 H84I 109.5 . . ? C84 C85 C86 121.7(10) . . ? C84 C85 H85 119.1 . . ? C86 C85 H85 119.1 . . ? C87 C86 C85 121.4(10) . . ? C87 C86 H86 119.3 . . ? C85 C86 H86 119.3 . . ? O87 C87 C86 125.1(9) . . ? O87 C87 C87A 118.0(9) . . ? C86 C87 C87A 116.8(10) . . ? C87 O87 C871 117.4(8) . . ? O87 C871 C872 106.4(9) . . ? O87 C871 H87A 110.4 . . ? C872 C871 H87A 110.4 . . ? O87 C871 H87B 110.4 . . ? C872 C871 H87B 110.4 . . ? H87A C871 H87B 108.6 . . ? C871 C872 C873 111.0(10) . . ? C871 C872 H87C 109.4 . . ? C873 C872 H87C 109.4 . . ? C871 C872 H87D 109.4 . . ? C873 C872 H87D 109.4 . . ? H87C C872 H87D 108 . . ? C872 C873 C874 112.2(11) . . ? C872 C873 H87E 109.2 . . ? C874 C873 H87E 109.2 . . ? C872 C873 H87F 109.2 . . ? C874 C873 H87F 109.2 . . ? H87E C873 H87F 107.9 . . ? C873 C874 H87G 109.5 . . ? C873 C874 H87H 109.5 . . ? H87G C874 H87H 109.5 . . ? C873 C874 H87I 109.5 . . ? H87G C874 H87I 109.5 . . ? H87H C874 H87I 109.5 . . ? C83A C87A C87 121.7(9) . . ? C83A C87A N81 105.8(8) . . ? C87 C87A N81 131.9(9) . . ? N81 C8 C52 113.5(8) . . ? N81 C8 H8A 108.9 . . ? C52 C8 H8A 108.9 . . ? N81 C8 H8B 108.9 . . ? C52 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C102 C101 C106 122.3(15) . . ? C102 C101 H101 118.8 . . ? C106 C101 H101 118.8 . . ? C101 C102 C103 118.6(14) . . ? C101 C102 H102 120.7 . . ? C103 C102 H102 120.7 . . ? C104 C103 C102 119.0(14) . . ? C104 C103 H103 120.5 . . ? C102 C103 H103 120.5 . . ? C103 C104 C105 120.7(15) . . ? C103 C104 H104 119.6 . . ? C105 C104 H104 119.6 . . ? C106 C105 C104 119.3(15) . . ? C106 C105 H105 120.3 . . ? C104 C105 H105 120.3 . . ? C105 C106 C101 119.7(14) . . ? C105 C106 H106 120.1 . . ? C101 C106 H106 120.1 . . ? C202 C201 C206 120.3(13) . . ? C202 C201 H201 119.9 . . ? C206 C201 H201 119.9 . . ? C201 C202 C203 118.2(12) . . ? C201 C202 H202 120.9 . . ? C203 C202 H202 120.9 . . ? C204 C203 C202 121.3(14) . . ? C204 C203 H203 119.3 . . ? C202 C203 H203 119.3 . . ? C205 C204 C203 119.1(15) . . ? C205 C204 H204 120.5 . . ? C203 C204 H204 120.5 . . ? C206 C205 C204 121.1(13) . . ? C206 C205 H205 119.4 . . ? C204 C205 H205 119.4 . . ? C205 C206 C201 119.8(13) . . ? C205 C206 H206 120.1 . . ? C201 C206 H206 120.1 . . ? C306 C301 C302 118.4(16) . . ? C306 C301 H301 120.8 . . ? C302 C301 H301 120.8 . . ? C303 C302 C301 120.6(15) . . ? C303 C302 H302 119.7 . . ? C301 C302 H302 119.7 . . ? C304 C303 C302 120.6(16) . . ? C304 C303 H303 119.7 . . ? C302 C303 H303 119.7 . . ? C303 C304 C305 120.7(16) . . ? C303 C304 H304 119.7 . . ? C305 C304 H304 119.7 . . ? C306 C305 C304 118.8(15) . . ? C306 C305 H305 120.6 . . ? C304 C305 H305 120.6 . . ? C305 C306 C301 120.8(15) . . ? C305 C306 H306 119.6 . . ? C301 C306 H306 119.6 . . ? C406 C401 C402 118.6(16) . . ? C406 C401 H401 120.7 . . ? C402 C401 H401 120.7 . . ? C403 C402 C401 121.2(18) . . ? C403 C402 H402 119.4 . . ? C401 C402 H402 119.4 . . ? C402 C403 C404 119.9(19) . . ? C402 C403 H403 120.1 . . ? C404 C403 H403 120.1 . . ? C403 C404 C405 123.0(18) . . ? C403 C404 H404 118.5 . . ? C405 C404 H404 118.5 . . ? C404 C405 C406 119.4(19) . . ? C404 C405 H405 120.3 . . ? C406 C405 H405 120.3 . . ? C401 C406 C405 117.7(18) . . ? C401 C406 H406 121.1 . . ? C405 C406 H406 121.1 . . ? C502 C501 C506 118.9(17) . . ? C502 C501 H501 120.5 . . ? C506 C501 H501 120.5 . . ? C501 C502 C503 122.3(16) . . ? C501 C502 H502 118.8 . . ? C503 C502 H502 118.8 . . ? C504 C503 C502 118.8(16) . . ? C504 C503 H503 120.6 . . ? C502 C503 H503 120.6 . . ? C503 C504 C505 121.0(17) . . ? C503 C504 H504 119.5 . . ? C505 C504 H504 119.5 . . ? C506 C505 C504 119.6(16) . . ? C506 C505 H505 120.2 . . ? C504 C505 H505 120.2 . . ? C505 C506 C501 119.3(16) . . ? C505 C506 H506 120.3 . . ? C501 C506 H506 120.3 . . ? N601 C601 C602 175.3(13) . . ? C601 C602 H60A 109.5 . . ? C601 C602 H60B 109.5 . . ? H60A C602 H60B 109.5 . . ? C601 C602 H60C 109.5 . . ? H60A C602 H60C 109.5 . . ? H60B C602 H60C 109.5 . . ? N701 C701 C702 179.0(14) . . ? C701 C702 H70A 109.5 . . ? C701 C702 H70B 109.5 . . ? H70A C702 H70B 109.5 . . ? C701 C702 H70C 109.5 . . ? H70A C702 H70C 109.5 . . ? H70B C702 H70C 109.5 . . ? # Attachment 'ps88b_dhb238_ps91g_ps97_ps97x_ps93f4_paper.cif' data_ps88b _database_code_depnum_ccdc_archive 'CCDC 726626' _audit_creation_date 2009-07-13T21:14:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C40 H58 Br2 N4 O5' _chemical_formula_moiety 'C40 H56 N4 O4, 2(Br), H2O' _chemical_formula_weight 834.72 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 30.686(3) _cell_length_b 15.0391(6) _cell_length_c 18.3270(10) _cell_angle_alpha 90 _cell_angle_beta 102.091(7) _cell_angle_gamma 90 _cell_volume 8270.1(10) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20053 _cell_measurement_theta_min 3.3223 _cell_measurement_theta_max 32.5174 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3488 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.006 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.77368 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 -0.0157201239 _diffrn_orient_matrix_ub_12 0.0402738592 _diffrn_orient_matrix_ub_13 -0.0095899001 _diffrn_orient_matrix_ub_21 0.0065974948 _diffrn_orient_matrix_ub_22 0.0198701846 _diffrn_orient_matrix_ub_23 0.0213877995 _diffrn_orient_matrix_ub_31 0.0356932954 _diffrn_orient_matrix_ub_32 0.0141045752 _diffrn_orient_matrix_ub_33 -0.0027169468 _diffrn_reflns_av_R_equivalents 0.07 _diffrn_reflns_av_unetI/netI 0.1638 _diffrn_reflns_number 99530 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 32.61 _diffrn_reflns_theta_full 31 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.931 _diffrn_measurement_device_type ; Oxford Diffraction Gemini diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 28124 _reflns_number_gt 12625 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.1185P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 28124 _refine_ls_number_parameters 931 _refine_ls_number_restraints 1429 _refine_ls_R_factor_all 0.1559 _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.2354 _refine_ls_wR_factor_gt 0.1598 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.007 _refine_diff_density_max 2.909 _refine_diff_density_min -1.043 _refine_diff_density_rms 0.189 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 C1 C 0.31811(10) 0.07361(17) 0.81346(15) 0.0199(6) Uani 1 1 d U . . H1A H 0.3439 0.0453 0.7993 0.03 Uiso 1 1 calc R . . H1B H 0.2907 0.0519 0.781 0.03 Uiso 1 1 calc R . . H1C H 0.3178 0.059 0.8655 0.03 Uiso 1 1 calc R . . N21 N 0.34713(7) 0.30010(14) 0.77931(12) 0.0146(5) Uani 1 1 d U . . C22 C 0.35124(9) 0.21219(18) 0.77365(14) 0.0171(6) Uani 1 1 d U . . H22 H 0.3723 0.1831 0.7506 0.02 Uiso 1 1 calc R . . N23 N 0.32113(8) 0.17119(15) 0.80532(12) 0.0167(5) Uani 1 1 d U . . C23A C 0.29631(9) 0.23461(17) 0.83266(13) 0.0143(5) Uani 1 1 d U . . C24 C 0.26015(9) 0.22743(19) 0.86824(14) 0.0186(6) Uani 1 1 d U . . O24 O 0.24303(7) 0.14398(13) 0.87600(10) 0.0214(5) Uani 1 1 d U . . C241 C 0.21158(10) 0.13912(18) 0.92430(15) 0.0209(6) Uani 1 1 d U . . H24A H 0.1841 0.1724 0.9023 0.025 Uiso 1 1 calc R . . H24B H 0.2246 0.1653 0.9736 0.025 Uiso 1 1 calc R . . C242 C 0.20092(10) 0.0421(2) 0.93264(17) 0.0259(7) Uani 1 1 d U . . H24C H 0.2283 0.0099 0.9566 0.031 Uiso 1 1 calc R . . H24D H 0.1897 0.0157 0.8828 0.031 Uiso 1 1 calc R . . C243 C 0.16552(11) 0.0322(2) 0.98049(18) 0.0319(8) Uani 1 1 d U . . H24E H 0.1772 0.0575 1.0306 0.038 Uiso 1 1 calc R . . H24F H 0.1386 0.0662 0.9572 0.038 Uiso 1 1 calc R . . C244 C 0.15294(13) -0.0647(3) 0.9883(2) 0.0438(10) Uani 1 1 d U . . H24G H 0.1405 -0.0894 0.9389 0.066 Uiso 1 1 calc R . . H24H H 0.1307 -0.0685 1.0195 0.066 Uiso 1 1 calc R . . H24I H 0.1795 -0.0985 1.0117 0.066 Uiso 1 1 calc R . . C25 C 0.24355(9) 0.30664(19) 0.89051(15) 0.0198(6) Uani 1 1 d U . . H25 H 0.2194 0.3047 0.9155 0.024 Uiso 1 1 calc R . . C26 C 0.26138(10) 0.3887(2) 0.87711(15) 0.0239(6) Uani 1 1 d U . . H26 H 0.2492 0.4412 0.8937 0.029 Uiso 1 1 calc R . . C27 C 0.29654(9) 0.39613(18) 0.84016(14) 0.0180(6) Uani 1 1 d U . . O27 O 0.31610(7) 0.47386(13) 0.82333(11) 0.0255(5) Uani 1 1 d U . . C271 C 0.30331(11) 0.55384(19) 0.85619(18) 0.0299(7) Uani 1 1 d U . . H27A H 0.3073 0.5463 0.9109 0.036 Uiso 1 1 calc R . . H27B H 0.2715 0.5671 0.8354 0.036 Uiso 1 1 calc R . . C272 C 0.33211(12) 0.6292(2) 0.8392(2) 0.0327(8) Uani 1 1 d U . . H27C H 0.3211 0.6854 0.8568 0.039 Uiso 1 1 calc R . . H27D H 0.3287 0.6337 0.7844 0.039 Uiso 1 1 calc R . . C273 C 0.38224(12) 0.6198(2) 0.8747(2) 0.0352(8) Uani 1 1 d U . . H27E H 0.394 0.5671 0.8529 0.042 Uiso 1 1 calc R . . H27F H 0.3981 0.6727 0.8611 0.042 Uiso 1 1 calc R . . C274 C 0.39296(14) 0.6104(3) 0.9591(2) 0.0447(10) Uani 1 1 d U . . H27G H 0.3801 0.6607 0.9814 0.067 Uiso 1 1 calc R . . H27H H 0.4254 0.6098 0.9772 0.067 Uiso 1 1 calc R . . H27I H 0.3803 0.5547 0.9731 0.067 Uiso 1 1 calc R . . C27A C 0.31303(9) 0.31712(18) 0.81714(14) 0.0166(6) Uani 1 1 d U . . C2 C 0.37039(9) 0.36392(17) 0.74044(14) 0.0149(5) Uani 1 1 d U . . H2A H 0.3491 0.4111 0.7185 0.018 Uiso 1 1 calc R . . H2B H 0.3799 0.3329 0.6988 0.018 Uiso 1 1 calc R . . C31 C 0.43666(9) 0.46626(17) 0.75693(14) 0.0169(6) Uani 1 1 d U . . C32 C 0.41075(9) 0.40730(16) 0.78903(13) 0.0135(5) Uani 1 1 d U . . C33 C 0.42389(10) 0.38908(19) 0.86573(14) 0.0205(6) Uani 1 1 d U . . H33 H 0.4066 0.349 0.888 0.025 Uiso 1 1 calc R . . C34 C 0.46087(11) 0.42736(18) 0.90949(16) 0.0229(7) Uani 1 1 d U . . H34 H 0.4684 0.4149 0.9614 0.027 Uiso 1 1 calc R . . C35 C 0.48749(10) 0.48464(18) 0.87766(15) 0.0223(7) Uani 1 1 d U . . H35 H 0.5139 0.5094 0.9071 0.027 Uiso 1 1 calc R . . C36 C 0.47472(10) 0.50470(19) 0.80253(15) 0.0210(6) Uani 1 1 d U . . H36 H 0.4921 0.5455 0.7811 0.025 Uiso 1 1 calc R . . C3 C 0.42470(9) 0.48926(17) 0.67479(13) 0.0150(5) Uani 1 1 d U . . H3A H 0.3942 0.4678 0.6534 0.018 Uiso 1 1 calc R . . H3B H 0.4249 0.5547 0.6688 0.018 Uiso 1 1 calc R . . N41 N 0.48899(7) 0.34403(15) 0.58159(11) 0.0147(5) Uani 1 1 d U . . C42 C 0.45447(9) 0.36396(17) 0.61238(14) 0.0163(6) Uani 1 1 d U . . H42 H 0.4317 0.3234 0.6183 0.02 Uiso 1 1 calc R . . N43 N 0.45651(7) 0.44858(14) 0.63356(11) 0.0114(4) Uani 1 1 d U . . C43A C 0.49474(8) 0.48675(17) 0.61630(13) 0.0126(5) Uani 1 1 d U . . C44 C 0.51267(9) 0.57292(18) 0.62514(14) 0.0166(6) Uani 1 1 d U . . O44 O 0.48972(7) 0.63347(13) 0.65865(10) 0.0205(5) Uani 1 1 d U . . C441 C 0.50873(10) 0.72124(17) 0.67169(15) 0.0202(6) Uani 1 1 d U . . H44A H 0.5057 0.7535 0.6238 0.024 Uiso 1 1 calc R . . H44B H 0.5408 0.7169 0.695 0.024 Uiso 1 1 calc R . . C442 C 0.48438(11) 0.77076(19) 0.72274(16) 0.0230(7) Uani 1 1 d U . . H44C H 0.4995 0.8286 0.7357 0.028 Uiso 1 1 calc R . . H44D H 0.4872 0.7364 0.7696 0.028 Uiso 1 1 calc R . . C443 C 0.43533(12) 0.7882(2) 0.69168(18) 0.0370(9) Uani 1 1 d U . . H44E H 0.4192 0.7309 0.6835 0.044 Uiso 1 1 calc R . . H44F H 0.4318 0.8187 0.6429 0.044 Uiso 1 1 calc R . . C444 C 0.41498(13) 0.8459(3) 0.7450(2) 0.0472(11) Uani 1 1 d U . . H44G H 0.4203 0.8178 0.7943 0.071 Uiso 1 1 calc R . . H44H H 0.3828 0.8518 0.7256 0.071 Uiso 1 1 calc R . . H44I H 0.4288 0.9049 0.7491 0.071 Uiso 1 1 calc R . . C45 C 0.55040(10) 0.58703(18) 0.59705(15) 0.0189(6) Uani 1 1 d U . . H45 H 0.5633 0.6447 0.601 0.023 Uiso 1 1 calc R . . C46 C 0.57039(9) 0.52003(18) 0.56311(14) 0.0178(6) Uani 1 1 d U . . H46 H 0.5964 0.5337 0.5449 0.021 Uiso 1 1 calc R . . C47 C 0.55368(9) 0.43389(18) 0.55488(14) 0.0176(6) Uani 1 1 d U . . O47 O 0.56925(7) 0.36426(13) 0.52147(11) 0.0222(5) Uani 1 1 d U . . C471 C 0.61251(10) 0.3718(2) 0.50237(16) 0.0251(7) Uani 1 1 d U . . H47A H 0.6147 0.4301 0.4783 0.03 Uiso 1 1 calc R . . H47B H 0.6156 0.3247 0.466 0.03 Uiso 1 1 calc R . . C472 C 0.64952(10) 0.3634(2) 0.56915(18) 0.0274(7) Uani 1 1 d U . . H47C H 0.6434 0.3124 0.5996 0.033 Uiso 1 1 calc R . . H47D H 0.6505 0.4178 0.5999 0.033 Uiso 1 1 calc R . . C473 C 0.69494(11) 0.3499(2) 0.5488(2) 0.0347(8) Uani 1 1 d U . . H47E H 0.6998 0.3974 0.5139 0.042 Uiso 1 1 calc R . . H47F H 0.6951 0.2922 0.523 0.042 Uiso 1 1 calc R . . C474 C 0.73309(12) 0.3517(2) 0.6181(2) 0.0417(10) Uani 1 1 d U . . H47G H 0.7345 0.4104 0.6416 0.062 Uiso 1 1 calc R . . H47H H 0.7614 0.3393 0.6033 0.062 Uiso 1 1 calc R . . H47I H 0.7278 0.3063 0.6537 0.062 Uiso 1 1 calc R . . C47A C 0.51527(9) 0.41973(17) 0.58318(13) 0.0137(5) Uani 1 1 d U . . C4 C 0.49751(10) 0.25491(17) 0.55451(16) 0.0223(6) Uani 1 1 d . . . H4A H 0.4743 0.2138 0.5632 0.033 Uiso 1 1 calc R . . H4B H 0.5267 0.2339 0.5813 0.033 Uiso 1 1 calc R . . H4C H 0.4972 0.2577 0.501 0.033 Uiso 1 1 calc R . . C5 C 0.82103(11) 0.5640(2) 0.79989(17) 0.0273(7) Uani 1 1 d U . . H5A H 0.8489 0.5408 0.7894 0.041 Uiso 1 1 calc R . . H5B H 0.7958 0.5398 0.7636 0.041 Uiso 1 1 calc R . . H5C H 0.8185 0.5465 0.8503 0.041 Uiso 1 1 calc R . . N61 N 0.84130(8) 0.79529(17) 0.76680(12) 0.0228(6) Uani 1 1 d U . . C62 C 0.84881(9) 0.7083(2) 0.76297(15) 0.0222(6) Uani 1 1 d U . . H62 H 0.8712 0.6829 0.7407 0.027 Uiso 1 1 calc R . . N63 N 0.82083(8) 0.66145(17) 0.79444(13) 0.0218(5) Uani 1 1 d U . . C63A C 0.79211(10) 0.72195(19) 0.81911(14) 0.0184(6) Uani 1 1 d U . . C64 C 0.75610(10) 0.70614(19) 0.85342(15) 0.0197(6) Uani 1 1 d U . . O64 O 0.74450(7) 0.62015(14) 0.86340(11) 0.0239(5) Uani 1 1 d U . . C641 C 0.71347(10) 0.6067(2) 0.91160(16) 0.0275(7) Uani 1 1 d U . . H64A H 0.6833 0.6267 0.8863 0.033 Uiso 1 1 calc R . . H64B H 0.7228 0.6417 0.958 0.033 Uiso 1 1 calc R . . C642 C 0.71263(12) 0.5089(2) 0.92983(18) 0.0374(8) Uani 1 1 d U . . H64C H 0.6914 0.5002 0.963 0.045 Uiso 1 1 calc R . . H64D H 0.7425 0.4921 0.9585 0.045 Uiso 1 1 calc R . . C643 C 0.70013(14) 0.4449(3) 0.8646(2) 0.0437(10) Uani 1 1 d U . . H64E H 0.7237 0.4458 0.8351 0.052 Uiso 1 1 calc R . . H64F H 0.672 0.4651 0.8317 0.052 Uiso 1 1 calc R . . C644 C 0.69417(15) 0.3503(3) 0.8900(2) 0.0523(12) Uani 1 1 d U . . H64G H 0.6717 0.3494 0.9209 0.078 Uiso 1 1 calc R . . H64H H 0.7226 0.3282 0.9192 0.078 Uiso 1 1 calc R . . H64I H 0.6844 0.3121 0.8463 0.078 Uiso 1 1 calc R . . C65 C 0.73510(10) 0.7817(2) 0.87311(15) 0.0251(7) Uani 1 1 d U . . H65 H 0.7112 0.7754 0.8984 0.03 Uiso 1 1 calc R . . C66 C 0.74866(10) 0.8674(2) 0.85627(16) 0.0250(7) Uani 1 1 d U . . H66 H 0.7333 0.9171 0.8705 0.03 Uiso 1 1 calc R . . C67 C 0.78308(10) 0.8828(2) 0.82015(16) 0.0228(6) Uani 1 1 d U . . O67 O 0.79935(8) 0.96171(14) 0.80163(11) 0.0309(5) Uani 1 1 d U . . C671 C 0.77802(12) 1.0404(2) 0.82197(18) 0.0332(8) Uani 1 1 d U . . H67A H 0.7789 1.0409 0.8763 0.04 Uiso 1 1 calc R . . H67B H 0.7465 1.0426 0.795 0.04 Uiso 1 1 calc R . . C672 C 0.80355(13) 1.1190(2) 0.8005(2) 0.0376(9) Uani 1 1 d U . . H67C H 0.8044 1.1148 0.7469 0.045 Uiso 1 1 calc R . . H67D H 0.8346 1.1172 0.8296 0.045 Uiso 1 1 calc R . . C673 C 0.78184(15) 1.2079(2) 0.8152(2) 0.0462(10) Uani 1 1 d U . . H67E H 0.78 1.2112 0.8684 0.055 Uiso 1 1 calc R . . H67F H 0.7511 1.2105 0.7848 0.055 Uiso 1 1 calc R . . C674 C 0.80876(17) 1.2885(3) 0.7957(2) 0.0581(13) Uani 1 1 d U . . H67G H 0.8075 1.2895 0.7418 0.087 Uiso 1 1 calc R . . H67H H 0.8399 1.2833 0.8224 0.087 Uiso 1 1 calc R . . H67I H 0.796 1.3436 0.8106 0.087 Uiso 1 1 calc R . . C67A C 0.80440(9) 0.8060(2) 0.80110(14) 0.0215(6) Uani 1 1 d U . . C6 C 0.86325(10) 0.8635(2) 0.72970(15) 0.0229(6) Uani 1 1 d U . . H6A H 0.8406 0.9074 0.706 0.028 Uiso 1 1 calc R . . H6B H 0.8754 0.8349 0.6896 0.028 Uiso 1 1 calc R . . C7 C 0.91907(10) 0.9946(2) 0.66954(15) 0.0227(6) Uani 1 1 d U . . H7A H 0.8898 0.9708 0.6441 0.027 Uiso 1 1 calc R . . H7B H 0.9185 1.0599 0.6624 0.027 Uiso 1 1 calc R . . C71 C 0.92659(10) 0.9739(2) 0.75269(15) 0.0222(6) Uani 1 1 d U . . C72 C 0.90041(10) 0.91189(19) 0.78124(15) 0.0207(6) Uani 1 1 d U . . C73 C 0.90938(11) 0.8954(2) 0.85834(15) 0.0290(7) Uani 1 1 d U . . H73 H 0.8917 0.8542 0.8787 0.035 Uiso 1 1 calc R . . C74 C 0.94433(12) 0.9399(2) 0.90495(17) 0.0320(8) Uani 1 1 d U . . H74 H 0.9508 0.9277 0.957 0.038 Uiso 1 1 calc R . . C75 C 0.96991(13) 1.0018(2) 0.87610(18) 0.0388(9) Uani 1 1 d U . . H75 H 0.9936 1.0321 0.9081 0.047 Uiso 1 1 calc R . . C76 C 0.96019(12) 1.0187(2) 0.79984(17) 0.0326(8) Uani 1 1 d U . . H76 H 0.9771 1.0619 0.78 0.039 Uiso 1 1 calc R . . C8 C 1.00485(11) 0.7637(2) 0.56877(17) 0.0281(7) Uani 1 1 d U . . H8A H 0.9844 0.7193 0.5819 0.042 Uiso 1 1 calc R . . H8B H 1.0354 0.7499 0.5948 0.042 Uiso 1 1 calc R . . H8C H 1.003 0.7626 0.5148 0.042 Uiso 1 1 calc R . . N81 N 0.99239(8) 0.85256(15) 0.59114(12) 0.0196(5) Uani 1 1 d U . . C82 C 0.95593(10) 0.8701(2) 0.61773(15) 0.0231(6) Uani 1 1 d U . . H82 H 0.9342 0.8272 0.6235 0.028 Uiso 1 1 calc R . . N83 N 0.95420(8) 0.95604(15) 0.63510(12) 0.0189(5) Uani 1 1 d U . . C83A C 0.99109(9) 0.99786(19) 0.61746(14) 0.0172(6) Uani 1 1 d U . . C84 C 1.00592(10) 1.08762(19) 0.62321(15) 0.0200(6) Uani 1 1 d U . . O84 O 0.98106(8) 1.14713(14) 0.65230(11) 0.0274(5) Uani 1 1 d U . . C841 C 1.00028(14) 1.2360(2) 0.66558(18) 0.0391(9) Uani 1 1 d U . . H84A H 0.9976 1.2676 0.6174 0.047 Uiso 1 1 calc R . . H84B H 1.0323 1.2312 0.689 0.047 Uiso 1 1 calc R . . C842 C 0.97710(16) 1.2871(3) 0.7149(2) 0.0498(10) Uani 1 1 d U . . H84C H 0.9777 1.2519 0.7608 0.06 Uiso 1 1 calc R . . H84D H 0.994 1.3426 0.7298 0.06 Uiso 1 1 calc R . . C843 C 0.93121(16) 1.3104(3) 0.6830(2) 0.0638(13) Uani 1 1 d U . . H84E H 0.9128 1.2558 0.679 0.077 Uiso 1 1 calc R . . H84F H 0.9295 1.3332 0.6318 0.077 Uiso 1 1 calc R . . C844 C 0.91010(15) 1.3836(3) 0.7298(2) 0.0617(14) Uani 1 1 d U . . H84G H 0.9291 1.4367 0.7369 0.093 Uiso 1 1 calc R . . H84H H 0.9082 1.359 0.7786 0.093 Uiso 1 1 calc R . . H84I H 0.8802 1.3997 0.7024 0.093 Uiso 1 1 calc R . . C85 C 1.04450(11) 1.1036(2) 0.59804(15) 0.0265(7) Uani 1 1 d U . . H85 H 1.0553 1.1629 0.6002 0.032 Uiso 1 1 calc R . . C86 C 1.06884(10) 1.03831(19) 0.56951(15) 0.0229(6) Uani 1 1 d U . . H86 H 1.095 1.0543 0.5527 0.028 Uiso 1 1 calc R . . C87 C 1.05483(10) 0.9500(2) 0.56570(15) 0.0226(6) Uani 1 1 d U . . O87 O 1.07490(7) 0.87991(14) 0.53977(11) 0.0251(5) Uani 1 1 d U . . C871 C 1.11781(10) 0.8950(2) 0.52278(17) 0.0251(7) Uani 1 1 d U . . H87A H 1.1384 0.9201 0.5668 0.03 Uiso 1 1 calc R . . H87B H 1.1152 0.9378 0.4811 0.03 Uiso 1 1 calc R . . C872 C 1.13526(11) 0.8084(2) 0.50162(17) 0.0318(8) Uani 1 1 d U . . H87C H 1.1148 0.7853 0.4565 0.038 Uiso 1 1 calc R . . H87D H 1.1356 0.7651 0.5425 0.038 Uiso 1 1 calc R . . C873 C 1.18182(12) 0.8152(3) 0.4862(2) 0.0400(9) Uani 1 1 d U . . H87E H 1.201 0.8463 0.5287 0.048 Uiso 1 1 calc R . . H87F H 1.1938 0.7543 0.4844 0.048 Uiso 1 1 calc R . . C874 C 1.18547(12) 0.8625(3) 0.4155(2) 0.0451(10) Uani 1 1 d U . . H87G H 1.1755 0.9242 0.4176 0.068 Uiso 1 1 calc R . . H87H H 1.1668 0.8324 0.3727 0.068 Uiso 1 1 calc R . . H87I H 1.2166 0.8618 0.41 0.068 Uiso 1 1 calc R . . C87A C 1.01536(9) 0.93322(18) 0.58950(14) 0.0172(6) Uani 1 1 d U . . O1 O 0.38776(9) 0.24381(17) 0.47872(12) 0.0422(7) Uani 1 1 d . . . O2 O 0.09975(10) 0.26434(17) 0.51183(13) 0.0502(8) Uani 1 1 d . . . Br1 Br 0.415530(10) 0.14190(2) 0.648888(16) 0.02465(7) Uani 1 1 d . . . Br2 Br 0.333438(10) 0.41255(2) 0.529308(15) 0.02301(7) Uani 1 1 d . . . Br3 Br 0.072847(11) 0.35406(2) 0.337662(17) 0.02776(7) Uani 1 1 d . . . Br4 Br 0.164991(11) 0.10347(2) 0.482715(17) 0.03158(8) Uani 1 1 d . . . 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 C1 0.0177(13) 0.0176(12) 0.0237(13) 0.0020(10) 0.0026(11) 0.0012(10) N21 0.0098(9) 0.0156(10) 0.0209(9) -0.0024(8) 0.0087(8) -0.0021(8) C22 0.0161(12) 0.0190(12) 0.0158(11) -0.0005(10) 0.0029(9) -0.0036(10) N23 0.0158(10) 0.0157(9) 0.0196(10) 0.0050(8) 0.0058(8) 0.0005(8) C23A 0.0136(11) 0.0165(11) 0.0138(10) 0.0030(9) 0.0051(9) -0.0002(9) C24 0.0152(12) 0.0240(12) 0.0169(11) -0.0002(10) 0.0041(9) -0.0050(10) O24 0.0165(9) 0.0266(10) 0.0231(9) 0.0017(8) 0.0091(7) -0.0050(8) C241 0.0227(13) 0.0209(12) 0.0210(12) 0.0074(10) 0.0090(10) -0.0015(11) C242 0.0190(14) 0.0283(14) 0.0310(14) 0.0038(12) 0.0064(11) -0.0066(12) C243 0.0189(15) 0.0400(17) 0.0369(16) 0.0099(14) 0.0063(12) -0.0022(13) C244 0.038(2) 0.055(2) 0.0368(18) -0.0009(17) 0.0040(16) -0.0196(17) C25 0.0099(11) 0.0310(14) 0.0199(11) -0.0003(11) 0.0062(9) 0.0017(10) C26 0.0283(14) 0.0281(13) 0.0166(11) -0.0017(11) 0.0079(10) 0.0063(12) C27 0.0152(12) 0.0200(12) 0.0200(11) 0.0008(10) 0.0063(9) 0.0043(10) O27 0.0335(11) 0.0175(9) 0.0286(9) -0.0015(8) 0.0134(8) 0.0009(8) C271 0.0334(16) 0.0156(12) 0.0406(16) -0.0062(12) 0.0077(13) 0.0086(12) C272 0.0385(17) 0.0179(13) 0.0416(16) -0.0014(13) 0.0081(14) 0.0027(13) C273 0.0283(16) 0.0273(15) 0.0500(18) -0.0084(14) 0.0084(14) -0.0009(13) C274 0.039(2) 0.0407(19) 0.048(2) -0.0174(17) -0.0055(17) 0.0011(17) C27A 0.0138(12) 0.0207(12) 0.0147(11) -0.0007(9) 0.0018(9) -0.0008(10) C2 0.0166(11) 0.0130(11) 0.0179(10) 0.0001(9) 0.0100(9) -0.0020(9) C31 0.0226(13) 0.0134(11) 0.0168(10) -0.0001(9) 0.0084(9) -0.0013(10) C32 0.0174(11) 0.0116(10) 0.0122(10) -0.0020(9) 0.0044(9) 0.0036(9) C33 0.0240(13) 0.0256(13) 0.0137(10) 0.0051(10) 0.0082(10) -0.0002(11) C34 0.0319(15) 0.0161(12) 0.0193(12) 0.0012(10) 0.0024(11) 0.0020(11) C35 0.0277(15) 0.0164(12) 0.0203(12) -0.0025(10) -0.0004(11) -0.0008(11) C36 0.0221(14) 0.0200(13) 0.0200(12) -0.0035(10) 0.0025(10) -0.0019(11) C3 0.0141(12) 0.0166(12) 0.0151(10) -0.0020(9) 0.0048(9) 0.0006(10) N41 0.0140(10) 0.0193(10) 0.0118(9) 0.0014(8) 0.0046(8) -0.0025(8) C42 0.0165(12) 0.0160(11) 0.0151(11) 0.0017(9) 0.0001(9) -0.0060(10) N43 0.0103(9) 0.0116(9) 0.0121(8) 0.0029(7) 0.0018(7) -0.0006(7) C43A 0.0107(11) 0.0181(11) 0.0091(9) 0.0025(9) 0.0023(8) -0.0063(9) C44 0.0163(12) 0.0208(12) 0.0123(10) -0.0014(9) 0.0021(9) -0.0017(10) O44 0.0200(10) 0.0216(9) 0.0210(9) -0.0039(7) 0.0067(7) -0.0094(8) C441 0.0300(14) 0.0113(11) 0.0198(12) -0.0084(10) 0.0062(11) -0.0111(10) C442 0.0281(15) 0.0150(12) 0.0236(13) -0.0028(10) 0.0002(11) -0.0046(11) C443 0.0348(18) 0.0403(17) 0.0282(15) -0.0197(14) -0.0112(14) -0.0010(15) C444 0.0291(19) 0.046(2) 0.057(2) -0.0151(18) -0.0125(17) 0.0164(16) C45 0.0193(13) 0.0166(11) 0.0197(12) 0.0041(10) 0.0014(10) -0.0034(10) C46 0.0139(12) 0.0232(12) 0.0147(11) 0.0059(10) -0.0003(9) -0.0023(10) C47 0.0200(12) 0.0191(12) 0.0159(11) 0.0038(9) 0.0087(9) 0.0022(10) O47 0.0157(9) 0.0221(10) 0.0319(10) 0.0024(8) 0.0121(8) 0.0004(8) C471 0.0161(12) 0.0329(15) 0.0290(13) 0.0057(12) 0.0107(11) 0.0037(11) C472 0.0168(13) 0.0291(15) 0.0367(15) 0.0013(13) 0.0068(12) -0.0021(12) C473 0.0142(13) 0.0357(17) 0.0559(19) 0.0047(15) 0.0111(13) 0.0062(13) C474 0.0147(15) 0.043(2) 0.065(2) 0.0126(18) 0.0038(15) 0.0076(14) C47A 0.0180(11) 0.0122(10) 0.0133(10) 0.0001(9) 0.0086(9) -0.0019(9) C4 0.0266(14) 0.0132(12) 0.0304(13) -0.0031(11) 0.0134(11) 0.0023(11) C5 0.0167(14) 0.0320(15) 0.0322(15) -0.0002(13) 0.0028(12) 0.0033(12) N61 0.0210(11) 0.0319(12) 0.0170(10) 0.0010(9) 0.0075(9) -0.0051(10) C62 0.0062(11) 0.0382(15) 0.0225(12) -0.0061(12) 0.0034(10) -0.0044(11) N63 0.0118(11) 0.0307(12) 0.0235(11) -0.0003(10) 0.0048(9) 0.0039(9) C63A 0.0174(12) 0.0221(12) 0.0154(11) -0.0032(10) 0.0026(9) -0.0017(10) C64 0.0149(12) 0.0264(13) 0.0161(11) 0.0060(10) -0.0003(10) 0.0025(10) O64 0.0137(9) 0.0338(11) 0.0246(9) 0.0074(9) 0.0048(8) -0.0027(8) C641 0.0208(14) 0.0409(16) 0.0229(12) 0.0087(12) 0.0092(11) -0.0050(13) C642 0.0369(18) 0.0487(17) 0.0278(14) 0.0128(13) 0.0097(13) -0.0079(15) C643 0.041(2) 0.0491(19) 0.0389(18) 0.0081(16) 0.0034(16) -0.0067(17) C644 0.046(2) 0.039(2) 0.065(3) 0.0105(19) -0.005(2) -0.0068(18) C65 0.0217(14) 0.0354(15) 0.0197(12) 0.0090(11) 0.0076(11) 0.0034(12) C66 0.0212(13) 0.0312(15) 0.0246(13) -0.0017(12) 0.0095(11) 0.0011(12) C67 0.0230(13) 0.0244(12) 0.0220(12) -0.0038(11) 0.0067(10) -0.0031(11) O67 0.0376(12) 0.0285(11) 0.0303(10) -0.0024(9) 0.0156(9) -0.0074(10) C671 0.0391(18) 0.0283(15) 0.0315(15) 0.0069(13) 0.0060(14) -0.0039(13) C672 0.044(2) 0.0304(15) 0.0355(16) 0.0031(14) 0.0021(15) -0.0121(14) C673 0.055(2) 0.0355(17) 0.0424(19) -0.0004(16) -0.0027(18) -0.0091(17) C674 0.079(3) 0.049(2) 0.040(2) 0.0036(19) -0.001(2) -0.018(2) C67A 0.0150(12) 0.0361(14) 0.0171(11) -0.0026(11) 0.0118(9) -0.0015(11) C6 0.0202(13) 0.0364(15) 0.0151(11) 0.0011(11) 0.0105(9) -0.0086(11) C7 0.0200(13) 0.0266(14) 0.0226(12) 0.0022(11) 0.0071(10) -0.0005(11) C71 0.0219(13) 0.0261(13) 0.0184(11) -0.0053(11) 0.0040(10) -0.0007(11) C72 0.0206(13) 0.0229(13) 0.0189(11) -0.0046(10) 0.0049(10) -0.0040(10) C73 0.0352(16) 0.0376(16) 0.0144(11) -0.0087(12) 0.0060(11) -0.0076(13) C74 0.0282(16) 0.0450(18) 0.0196(13) -0.0015(13) -0.0026(12) -0.0047(14) C75 0.046(2) 0.0393(17) 0.0268(15) -0.0091(14) -0.0035(14) -0.0158(15) C76 0.0342(17) 0.0378(17) 0.0235(13) 0.0016(13) 0.0010(13) -0.0096(14) C8 0.0255(15) 0.0266(14) 0.0363(15) 0.0069(12) 0.0159(12) -0.0021(12) N81 0.0166(11) 0.0216(11) 0.0229(10) -0.0023(9) 0.0095(9) -0.0025(9) C82 0.0184(13) 0.0323(14) 0.0205(12) -0.0030(11) 0.0082(10) -0.0076(11) N83 0.0155(11) 0.0209(11) 0.0204(10) -0.0007(9) 0.0038(8) -0.0003(9) C83A 0.0184(12) 0.0219(12) 0.0128(10) 0.0034(9) 0.0068(9) -0.0055(10) C84 0.0180(13) 0.0203(12) 0.0200(12) 0.0032(10) 0.0000(10) -0.0017(10) O84 0.0314(11) 0.0271(10) 0.0253(10) -0.0006(8) 0.0096(9) -0.0005(9) C841 0.068(2) 0.0232(15) 0.0272(14) 0.0004(12) 0.0140(15) -0.0072(15) C842 0.070(2) 0.045(2) 0.0334(17) -0.0024(16) 0.0082(17) -0.0032(18) C843 0.055(2) 0.094(3) 0.0397(19) -0.025(2) 0.0033(18) -0.024(2) C844 0.039(2) 0.104(4) 0.042(2) -0.002(2) 0.0079(18) 0.014(2) C85 0.0342(16) 0.0267(14) 0.0179(12) 0.0080(11) 0.0041(11) -0.0097(12) C86 0.0219(14) 0.0267(13) 0.0198(12) 0.0103(11) 0.0035(10) -0.0086(11) C87 0.0160(12) 0.0347(14) 0.0183(11) 0.0053(11) 0.0065(10) 0.0007(11) O87 0.0191(10) 0.0305(11) 0.0291(9) 0.0026(9) 0.0128(8) -0.0017(8) C871 0.0199(13) 0.0286(14) 0.0297(13) 0.0070(12) 0.0118(11) -0.0025(11) C872 0.0264(15) 0.0434(17) 0.0293(14) -0.0006(13) 0.0144(12) -0.0009(14) C873 0.0291(17) 0.048(2) 0.0452(18) 0.0019(16) 0.0129(14) 0.0039(15) C874 0.0271(18) 0.062(2) 0.0510(19) 0.0112(18) 0.0186(15) 0.0061(17) C87A 0.0185(12) 0.0220(12) 0.0123(10) 0.0056(9) 0.0057(9) 0.0001(10) O1 0.0447(15) 0.0530(15) 0.0290(11) -0.0128(11) 0.0079(11) 0.0104(13) O2 0.0746(19) 0.0428(15) 0.0391(13) -0.0121(11) 0.0257(13) -0.0112(14) Br1 0.02403(14) 0.02354(14) 0.03002(14) -0.00234(11) 0.01393(11) 0.00114(11) Br2 0.01857(14) 0.02935(14) 0.02065(12) 0.00591(11) 0.00306(10) -0.00628(11) Br3 0.02657(15) 0.02812(15) 0.03321(14) -0.00040(12) 0.01680(12) 0.00229(12) Br4 0.02240(15) 0.04831(19) 0.02356(13) 0.01021(13) 0.00379(11) -0.01476(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N23 1.480(3) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? N21 C22 1.334(3) . ? N21 C27A 1.395(3) . ? N21 C2 1.467(3) . ? C22 N23 1.340(4) . ? C22 H22 0.95 . ? N23 C23A 1.379(3) . ? C23A C27A 1.395(4) . ? C23A C24 1.404(4) . ? C24 O24 1.379(3) . ? C24 C25 1.390(4) . ? O24 C241 1.442(3) . ? C241 C242 1.510(4) . ? C241 H24A 0.99 . ? C241 H24B 0.99 . ? C242 C243 1.540(4) . ? C242 H24C 0.99 . ? C242 H24D 0.99 . ? C243 C244 1.521(5) . ? C243 H24E 0.99 . ? C243 H24F 0.99 . ? C244 H24G 0.98 . ? C244 H24H 0.98 . ? C244 H24I 0.98 . ? C25 C26 1.392(4) . ? C25 H25 0.95 . ? C26 C27 1.393(4) . ? C26 H26 0.95 . ? C27 O27 1.378(3) . ? C27 C27A 1.391(4) . ? O27 C271 1.436(3) . ? C271 C272 1.509(5) . ? C271 H27A 0.99 . ? C271 H27B 0.99 . ? C272 C273 1.546(5) . ? C272 H27C 0.99 . ? C272 H27D 0.99 . ? C273 C274 1.518(5) . ? C273 H27E 0.99 . ? C273 H27F 0.99 . ? C274 H27G 0.98 . ? C274 H27H 0.98 . ? C274 H27I 0.98 . ? C2 C32 1.513(4) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C31 C32 1.400(4) . ? C31 C36 1.410(4) . ? C31 C3 1.513(3) . ? C32 C33 1.406(3) . ? C33 C34 1.371(4) . ? C33 H33 0.95 . ? C34 C35 1.396(4) . ? C34 H34 0.95 . ? C35 C36 1.384(4) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C3 N43 1.486(3) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? N41 C42 1.334(4) . ? N41 C47A 1.392(3) . ? N41 C4 1.472(3) . ? C42 N43 1.328(3) . ? C42 H42 0.95 . ? N43 C43A 1.401(3) . ? C43A C47A 1.393(4) . ? C43A C44 1.404(4) . ? C44 O44 1.372(3) . ? C44 C45 1.379(4) . ? O44 C441 1.443(3) . ? C441 C442 1.510(4) . ? C441 H44A 0.99 . ? C441 H44B 0.99 . ? C442 C443 1.516(5) . ? C442 H44C 0.99 . ? C442 H44D 0.99 . ? C443 C444 1.534(5) . ? C443 H44E 0.99 . ? C443 H44F 0.99 . ? C444 H44G 0.98 . ? C444 H44H 0.98 . ? C444 H44I 0.98 . ? C45 C46 1.392(4) . ? C45 H45 0.95 . ? C46 C47 1.390(4) . ? C46 H46 0.95 . ? C47 O47 1.350(3) . ? C47 C47A 1.400(4) . ? O47 C471 1.446(4) . ? C471 C472 1.490(4) . ? C471 H47A 0.99 . ? C471 H47B 0.99 . ? C472 C473 1.530(5) . ? C472 H47C 0.99 . ? C472 H47D 0.99 . ? C473 C474 1.537(5) . ? C473 H47E 0.99 . ? C473 H47F 0.99 . ? C474 H47G 0.98 . ? C474 H47H 0.98 . ? C474 H47I 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 N63 1.468(4) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? N61 C62 1.333(4) . ? N61 C67A 1.415(4) . ? N61 C6 1.470(4) . ? C62 N63 1.331(4) . ? C62 H62 0.95 . ? N63 C63A 1.406(4) . ? C63A C67A 1.378(4) . ? C63A C64 1.401(4) . ? C64 O64 1.364(4) . ? C64 C65 1.391(4) . ? O64 C641 1.442(4) . ? C641 C642 1.510(5) . ? C641 H64A 0.99 . ? C641 H64B 0.99 . ? C642 C643 1.520(5) . ? C642 H64C 0.99 . ? C642 H64D 0.99 . ? C643 C644 1.520(5) . ? C643 H64E 0.99 . ? C643 H64F 0.99 . ? C644 H64G 0.98 . ? C644 H64H 0.98 . ? C644 H64I 0.98 . ? C65 C66 1.408(4) . ? C65 H65 0.95 . ? C66 C67 1.378(4) . ? C66 H66 0.95 . ? C67 O67 1.359(4) . ? C67 C67A 1.407(4) . ? O67 C671 1.438(4) . ? C671 C672 1.515(5) . ? C671 H67A 0.99 . ? C671 H67B 0.99 . ? C672 C673 1.543(5) . ? C672 H67C 0.99 . ? C672 H67D 0.99 . ? C673 C674 1.550(6) . ? C673 H67E 0.99 . ? C673 H67F 0.99 . ? C674 H67G 0.98 . ? C674 H67H 0.98 . ? C674 H67I 0.98 . ? C6 C72 1.507(4) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 N83 1.477(4) . ? C7 C71 1.525(4) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C71 C76 1.375(4) . ? C71 C72 1.402(4) . ? C72 C73 1.404(4) . ? C73 C74 1.394(4) . ? C73 H73 0.95 . ? C74 C75 1.392(5) . ? C74 H74 0.95 . ? C75 C76 1.390(4) . ? C75 H75 0.95 . ? C76 H76 0.95 . ? C8 N81 1.472(4) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? N81 C82 1.337(4) . ? N81 C87A 1.406(4) . ? C82 N83 1.334(4) . ? C82 H82 0.95 . ? N83 C83A 1.391(4) . ? C83A C87A 1.386(4) . ? C83A C84 1.421(4) . ? C84 O84 1.356(4) . ? C84 C85 1.378(4) . ? O84 C841 1.461(4) . ? C841 C842 1.478(5) . ? C841 H84A 0.99 . ? C841 H84B 0.99 . ? C842 C843 1.450(6) . ? C842 H84C 0.99 . ? C842 H84D 0.99 . ? C843 C844 1.613(7) . ? C843 H84E 0.99 . ? C843 H84F 0.99 . ? C844 H84G 0.98 . ? C844 H84H 0.98 . ? C844 H84I 0.98 . ? C85 C86 1.399(4) . ? C85 H85 0.95 . ? C86 C87 1.393(4) . ? C86 H86 0.95 . ? C87 O87 1.356(4) . ? C87 C87A 1.394(4) . ? O87 C871 1.433(4) . ? C871 C872 1.491(5) . ? C871 H87A 0.99 . ? C871 H87B 0.99 . ? C872 C873 1.517(5) . ? C872 H87C 0.99 . ? C872 H87D 0.99 . ? C873 C874 1.503(5) . ? C873 H87E 0.99 . ? C873 H87F 0.99 . ? C874 H87G 0.98 . ? C874 H87H 0.98 . ? C874 H87I 0.98 . ? 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 N23 C1 H1A 109.5 . . ? N23 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N23 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C22 N21 C27A 108.3(2) . . ? C22 N21 C2 123.2(2) . . ? C27A N21 C2 127.8(2) . . ? N21 C22 N23 109.7(2) . . ? N21 C22 H22 125.1 . . ? N23 C22 H22 125.1 . . ? C22 N23 C23A 108.8(2) . . ? C22 N23 C1 124.3(2) . . ? C23A N23 C1 126.8(2) . . ? N23 C23A C27A 106.7(2) . . ? N23 C23A C24 131.8(2) . . ? C27A C23A C24 121.6(2) . . ? O24 C24 C25 125.4(3) . . ? O24 C24 C23A 118.2(2) . . ? C25 C24 C23A 116.4(2) . . ? C24 O24 C241 115.3(2) . . ? O24 C241 C242 107.4(2) . . ? O24 C241 H24A 110.2 . . ? C242 C241 H24A 110.2 . . ? O24 C241 H24B 110.2 . . ? C242 C241 H24B 110.2 . . ? H24A C241 H24B 108.5 . . ? C241 C242 C243 110.2(3) . . ? C241 C242 H24C 109.6 . . ? C243 C242 H24C 109.6 . . ? C241 C242 H24D 109.6 . . ? C243 C242 H24D 109.6 . . ? H24C C242 H24D 108.1 . . ? C244 C243 C242 111.7(3) . . ? C244 C243 H24E 109.3 . . ? C242 C243 H24E 109.3 . . ? C244 C243 H24F 109.3 . . ? C242 C243 H24F 109.3 . . ? H24E C243 H24F 107.9 . . ? C243 C244 H24G 109.5 . . ? C243 C244 H24H 109.5 . . ? H24G C244 H24H 109.5 . . ? C243 C244 H24I 109.5 . . ? H24G C244 H24I 109.5 . . ? H24H C244 H24I 109.5 . . ? C24 C25 C26 121.7(3) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C25 C26 C27 122.0(3) . . ? C25 C26 H26 119 . . ? C27 C26 H26 119 . . ? O27 C27 C27A 117.0(2) . . ? O27 C27 C26 126.5(3) . . ? C27A C27 C26 116.5(3) . . ? C27 O27 C271 116.5(2) . . ? O27 C271 C272 108.6(3) . . ? O27 C271 H27A 110 . . ? C272 C271 H27A 110 . . ? O27 C271 H27B 110 . . ? C272 C271 H27B 110 . . ? H27A C271 H27B 108.4 . . ? C271 C272 C273 114.8(3) . . ? C271 C272 H27C 108.6 . . ? C273 C272 H27C 108.6 . . ? C271 C272 H27D 108.6 . . ? C273 C272 H27D 108.6 . . ? H27C C272 H27D 107.6 . . ? C274 C273 C272 115.0(3) . . ? C274 C273 H27E 108.5 . . ? C272 C273 H27E 108.5 . . ? C274 C273 H27F 108.5 . . ? C272 C273 H27F 108.5 . . ? H27E C273 H27F 107.5 . . ? C273 C274 H27G 109.5 . . ? C273 C274 H27H 109.5 . . ? H27G C274 H27H 109.5 . . ? C273 C274 H27I 109.5 . . ? H27G C274 H27I 109.5 . . ? H27H C274 H27I 109.5 . . ? C27 C27A N21 131.8(3) . . ? C27 C27A C23A 121.7(3) . . ? N21 C27A C23A 106.5(2) . . ? N21 C2 C32 114.7(2) . . ? N21 C2 H2A 108.6 . . ? C32 C2 H2A 108.6 . . ? N21 C2 H2B 108.6 . . ? C32 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? C32 C31 C36 118.9(2) . . ? C32 C31 C3 121.5(2) . . ? C36 C31 C3 119.6(2) . . ? C31 C32 C33 118.3(2) . . ? C31 C32 C2 119.5(2) . . ? C33 C32 C2 122.2(2) . . ? C34 C33 C32 122.1(3) . . ? C34 C33 H33 118.9 . . ? C32 C33 H33 118.9 . . ? C33 C34 C35 120.0(3) . . ? C33 C34 H34 120 . . ? C35 C34 H34 120 . . ? C36 C35 C34 118.8(3) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? C35 C36 C31 121.8(3) . . ? C35 C36 H36 119.1 . . ? C31 C36 H36 119.1 . . ? N43 C3 C31 111.3(2) . . ? N43 C3 H3A 109.4 . . ? C31 C3 H3A 109.4 . . ? N43 C3 H3B 109.4 . . ? C31 C3 H3B 109.4 . . ? H3A C3 H3B 108 . . ? C42 N41 C47A 108.4(2) . . ? C42 N41 C4 124.1(2) . . ? C47A N41 C4 127.5(2) . . ? N43 C42 N41 110.2(2) . . ? N43 C42 H42 124.9 . . ? N41 C42 H42 124.9 . . ? C42 N43 C43A 108.5(2) . . ? C42 N43 C3 123.2(2) . . ? C43A N43 C3 128.1(2) . . ? C47A C43A N43 106.2(2) . . ? C47A C43A C44 121.1(2) . . ? N43 C43A C44 132.7(2) . . ? O44 C44 C45 127.9(2) . . ? O44 C44 C43A 116.0(2) . . ? C45 C44 C43A 116.0(2) . . ? C44 O44 C441 117.0(2) . . ? O44 C441 C442 108.6(2) . . ? O44 C441 H44A 110 . . ? C442 C441 H44A 110 . . ? O44 C441 H44B 110 . . ? C442 C441 H44B 110 . . ? H44A C441 H44B 108.4 . . ? C441 C442 C443 115.7(2) . . ? C441 C442 H44C 108.4 . . ? C443 C442 H44C 108.4 . . ? C441 C442 H44D 108.4 . . ? C443 C442 H44D 108.4 . . ? H44C C442 H44D 107.4 . . ? C442 C443 C444 111.3(3) . . ? C442 C443 H44E 109.4 . . ? C444 C443 H44E 109.4 . . ? C442 C443 H44F 109.4 . . ? C444 C443 H44F 109.4 . . ? H44E C443 H44F 108 . . ? C443 C444 H44G 109.5 . . ? C443 C444 H44H 109.5 . . ? H44G C444 H44H 109.5 . . ? C443 C444 H44I 109.5 . . ? H44G C444 H44I 109.5 . . ? H44H C444 H44I 109.5 . . ? C44 C45 C46 122.6(3) . . ? C44 C45 H45 118.7 . . ? C46 C45 H45 118.7 . . ? C47 C46 C45 122.4(3) . . ? C47 C46 H46 118.8 . . ? C45 C46 H46 118.8 . . ? O47 C47 C46 127.9(3) . . ? O47 C47 C47A 117.1(2) . . ? C46 C47 C47A 114.9(2) . . ? C47 O47 C471 118.6(2) . . ? O47 C471 C472 112.0(2) . . ? O47 C471 H47A 109.2 . . ? C472 C471 H47A 109.2 . . ? O47 C471 H47B 109.2 . . ? C472 C471 H47B 109.2 . . ? H47A C471 H47B 107.9 . . ? C471 C472 C473 112.8(3) . . ? C471 C472 H47C 109 . . ? C473 C472 H47C 109 . . ? C471 C472 H47D 109 . . ? C473 C472 H47D 109 . . ? H47C C472 H47D 107.8 . . ? C472 C473 C474 111.8(3) . . ? C472 C473 H47E 109.3 . . ? C474 C473 H47E 109.3 . . ? C472 C473 H47F 109.3 . . ? C474 C473 H47F 109.3 . . ? H47E C473 H47F 107.9 . . ? C473 C474 H47G 109.5 . . ? C473 C474 H47H 109.5 . . ? H47G C474 H47H 109.5 . . ? C473 C474 H47I 109.5 . . ? H47G C474 H47I 109.5 . . ? H47H C474 H47I 109.5 . . ? N41 C47A C43A 106.7(2) . . ? N41 C47A C47 130.2(2) . . ? C43A C47A C47 122.9(2) . . ? N41 C4 H4A 109.5 . . ? N41 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N41 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N63 C5 H5A 109.5 . . ? N63 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N63 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C62 N61 C67A 107.3(2) . . ? C62 N61 C6 124.0(2) . . ? C67A N61 C6 127.8(3) . . ? N63 C62 N61 111.2(3) . . ? N63 C62 H62 124.4 . . ? N61 C62 H62 124.4 . . ? C62 N63 C63A 107.6(2) . . ? C62 N63 C5 124.3(3) . . ? C63A N63 C5 128.2(3) . . ? C67A C63A C64 123.0(3) . . ? C67A C63A N63 107.1(2) . . ? C64 C63A N63 129.9(3) . . ? O64 C64 C65 126.3(3) . . ? O64 C64 C63A 118.3(3) . . ? C65 C64 C63A 115.4(3) . . ? C64 O64 C641 116.1(2) . . ? O64 C641 C642 108.4(3) . . ? O64 C641 H64A 110 . . ? C642 C641 H64A 110 . . ? O64 C641 H64B 110 . . ? C642 C641 H64B 110 . . ? H64A C641 H64B 108.4 . . ? C641 C642 C643 117.1(3) . . ? C641 C642 H64C 108 . . ? C643 C642 H64C 108 . . ? C641 C642 H64D 108 . . ? C643 C642 H64D 108 . . ? H64C C642 H64D 107.3 . . ? C642 C643 C644 112.3(3) . . ? C642 C643 H64E 109.1 . . ? C644 C643 H64E 109.1 . . ? C642 C643 H64F 109.2 . . ? C644 C643 H64F 109.2 . . ? H64E C643 H64F 107.9 . . ? C643 C644 H64G 109.5 . . ? C643 C644 H64H 109.5 . . ? H64G C644 H64H 109.5 . . ? C643 C644 H64I 109.5 . . ? H64G C644 H64I 109.5 . . ? H64H C644 H64I 109.5 . . ? C64 C65 C66 121.1(3) . . ? C64 C65 H65 119.5 . . ? C66 C65 H65 119.5 . . ? C67 C66 C65 123.4(3) . . ? C67 C66 H66 118.3 . . ? C65 C66 H66 118.3 . . ? O67 C67 C66 128.7(3) . . ? O67 C67 C67A 116.2(3) . . ? C66 C67 C67A 115.1(3) . . ? C67 O67 C671 116.3(2) . . ? O67 C671 C672 106.6(3) . . ? O67 C671 H67A 110.4 . . ? C672 C671 H67A 110.4 . . ? O67 C671 H67B 110.4 . . ? C672 C671 H67B 110.4 . . ? H67A C671 H67B 108.6 . . ? C671 C672 C673 111.4(3) . . ? C671 C672 H67C 109.3 . . ? C673 C672 H67C 109.3 . . ? C671 C672 H67D 109.3 . . ? C673 C672 H67D 109.3 . . ? H67C C672 H67D 108 . . ? C672 C673 C674 111.5(4) . . ? C672 C673 H67E 109.3 . . ? C674 C673 H67E 109.3 . . ? C672 C673 H67F 109.3 . . ? C674 C673 H67F 109.3 . . ? H67E C673 H67F 108 . . ? C673 C674 H67G 109.5 . . ? C673 C674 H67H 109.5 . . ? H67G C674 H67H 109.5 . . ? C673 C674 H67I 109.5 . . ? H67G C674 H67I 109.5 . . ? H67H C674 H67I 109.5 . . ? C63A C67A C67 121.9(3) . . ? C63A C67A N61 106.7(3) . . ? C67 C67A N61 131.4(3) . . ? N61 C6 C72 114.0(2) . . ? N61 C6 H6A 108.8 . . ? C72 C6 H6A 108.8 . . ? N61 C6 H6B 108.7 . . ? C72 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? N83 C7 C71 112.1(2) . . ? N83 C7 H7A 109.2 . . ? C71 C7 H7A 109.2 . . ? N83 C7 H7B 109.2 . . ? C71 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C76 C71 C72 120.3(3) . . ? C76 C71 C7 117.7(3) . . ? C72 C71 C7 122.0(3) . . ? C71 C72 C73 119.1(3) . . ? C71 C72 C6 120.3(2) . . ? C73 C72 C6 120.6(3) . . ? C74 C73 C72 119.7(3) . . ? C74 C73 H73 120.1 . . ? C72 C73 H73 120.1 . . ? C75 C74 C73 120.7(3) . . ? C75 C74 H74 119.6 . . ? C73 C74 H74 119.6 . . ? C76 C75 C74 119.0(3) . . ? C76 C75 H75 120.5 . . ? C74 C75 H75 120.5 . . ? C71 C76 C75 121.1(3) . . ? C71 C76 H76 119.4 . . ? C75 C76 H76 119.4 . . ? N81 C8 H8A 109.5 . . ? N81 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N81 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C82 N81 C87A 107.4(2) . . ? C82 N81 C8 124.5(2) . . ? C87A N81 C8 128.1(2) . . ? N83 C82 N81 110.9(3) . . ? N83 C82 H82 124.6 . . ? N81 C82 H82 124.6 . . ? C82 N83 C83A 107.9(2) . . ? C82 N83 C7 123.5(2) . . ? C83A N83 C7 128.6(2) . . ? C87A C83A N83 107.2(2) . . ? C87A C83A C84 120.3(3) . . ? N83 C83A C84 132.5(3) . . ? O84 C84 C85 127.6(3) . . ? O84 C84 C83A 117.3(3) . . ? C85 C84 C83A 115.1(3) . . ? C84 O84 C841 115.4(3) . . ? O84 C841 C842 110.4(3) . . ? O84 C841 H84A 109.6 . . ? C842 C841 H84A 109.6 . . ? O84 C841 H84B 109.6 . . ? C842 C841 H84B 109.6 . . ? H84A C841 H84B 108.1 . . ? C843 C842 C841 115.5(3) . . ? C843 C842 H84C 108.4 . . ? C841 C842 H84C 108.4 . . ? C843 C842 H84D 108.4 . . ? C841 C842 H84D 108.4 . . ? H84C C842 H84D 107.5 . . ? C842 C843 C844 114.5(3) . . ? C842 C843 H84E 108.6 . . ? C844 C843 H84E 108.6 . . ? C842 C843 H84F 108.6 . . ? C844 C843 H84F 108.6 . . ? H84E C843 H84F 107.6 . . ? C843 C844 H84G 109.5 . . ? C843 C844 H84H 109.5 . . ? H84G C844 H84H 109.5 . . ? C843 C844 H84I 109.5 . . ? H84G C844 H84I 109.5 . . ? H84H C844 H84I 109.5 . . ? C84 C85 C86 124.5(3) . . ? C84 C85 H85 117.8 . . ? C86 C85 H85 117.8 . . ? C87 C86 C85 120.3(3) . . ? C87 C86 H86 119.9 . . ? C85 C86 H86 119.9 . . ? O87 C87 C86 126.9(3) . . ? O87 C87 C87A 117.2(3) . . ? C86 C87 C87A 115.9(3) . . ? C87 O87 C871 117.3(2) . . ? O87 C871 C872 108.3(2) . . ? O87 C871 H87A 110 . . ? C872 C871 H87A 110 . . ? O87 C871 H87B 110 . . ? C872 C871 H87B 110 . . ? H87A C871 H87B 108.4 . . ? C871 C872 C873 113.1(3) . . ? C871 C872 H87C 109 . . ? C873 C872 H87C 109 . . ? C871 C872 H87D 108.9 . . ? C873 C872 H87D 109 . . ? H87C C872 H87D 107.8 . . ? C874 C873 C872 115.8(3) . . ? C874 C873 H87E 108.3 . . ? C872 C873 H87E 108.3 . . ? C874 C873 H87F 108.3 . . ? C872 C873 H87F 108.3 . . ? H87E C873 H87F 107.4 . . ? C873 C874 H87G 109.5 . . ? C873 C874 H87H 109.5 . . ? H87G C874 H87H 109.5 . . ? C873 C874 H87I 109.5 . . ? H87G C874 H87I 109.5 . . ? H87H C874 H87I 109.5 . . ? C83A C87A C87 123.9(3) . . ? C83A C87A N81 106.6(2) . . ? C87 C87A N81 129.4(3) . . ? #===END data_ps91g _database_code_depnum_ccdc_archive 'CCDC 726627' _audit_creation_date 2009-07-14T08:48:34-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C40 H54 Br2 N4 O4 Pd' _chemical_formula_moiety 'C40 H54 Br2 N4 O4 Pd' _chemical_formula_weight 921.09 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.3106(9) _cell_length_b 19.9122(8) _cell_length_c 12.1672(7) _cell_angle_alpha 90 _cell_angle_beta 107.964(6) _cell_angle_gamma 90 _cell_volume 3989.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3521 _cell_measurement_theta_min 2.5471 _cell_measurement_theta_max 27.4471 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.095 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.513 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.86091 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 -0.0543958756 _diffrn_orient_matrix_ub_12 0.0036423924 _diffrn_orient_matrix_ub_13 -0.0301759356 _diffrn_orient_matrix_ub_21 -0.0271605593 _diffrn_orient_matrix_ub_22 0.0028711166 _diffrn_orient_matrix_ub_23 0.030651227 _diffrn_orient_matrix_ub_31 0.0077960744 _diffrn_orient_matrix_ub_32 0.0353130263 _diffrn_orient_matrix_ub_33 0.000563204 _diffrn_reflns_av_R_equivalents 0.1443 _diffrn_reflns_av_unetI/netI 0.1896 _diffrn_reflns_number 33059 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 7017 _reflns_number_gt 3209 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0430P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7017 _refine_ls_number_parameters 478 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.1961 _refine_ls_R_factor_gt 0.0773 _refine_ls_wR_factor_ref 0.1506 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 0.96 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.12 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.29086(5) 0.37286(4) 0.95062(7) 0.0286(2) Uani 1 1 d . . . Br1 Br 0.40978(6) 0.38211(5) 1.12752(9) 0.0342(3) Uani 1 1 d . . . Br2 Br 0.18690(7) 0.37237(7) 1.05210(10) 0.0472(3) Uani 1 1 d . . . C1 C 0.3763(7) 0.2473(5) 0.8315(10) 0.038(3) Uani 1 1 d . . . H1A H 0.428 0.2237 0.8644 0.057 Uiso 1 1 calc R . . H1B H 0.3461 0.2265 0.7578 0.057 Uiso 1 1 calc R . . H1C H 0.3443 0.2445 0.8852 0.057 Uiso 1 1 calc R . . N21 N 0.4001(5) 0.4270(4) 0.8245(7) 0.021(2) Uani 1 1 d . . . C22 C 0.3668(6) 0.3714(5) 0.8592(8) 0.025(2) Uani 1 1 d . . . N23 N 0.3923(5) 0.3187(4) 0.8121(8) 0.031(2) Uani 1 1 d . . . C23A C 0.4445(6) 0.3395(5) 0.7515(9) 0.023(3) Uani 1 1 d . . . C24 C 0.4851(6) 0.2992(5) 0.6909(10) 0.036(3) Uani 1 1 d . . . H24 H 0.4792 0.2518 0.686 0.043 Uiso 1 1 calc R . . C25 C 0.5339(7) 0.3337(5) 0.6396(10) 0.035(3) Uani 1 1 d . . . O25 O 0.5775(4) 0.3057(3) 0.5746(7) 0.041(2) Uani 1 1 d . . . C251 C 0.5788(7) 0.2327(5) 0.5722(11) 0.048(3) Uani 1 1 d . . . H25A H 0.5229 0.2149 0.5417 0.058 Uiso 1 1 calc R . . H25B H 0.6037 0.2147 0.6511 0.058 Uiso 1 1 calc R . . C252 C 0.6282(7) 0.2122(5) 0.4947(11) 0.052(4) Uani 1 1 d . . . H25C H 0.6819 0.2345 0.5209 0.063 Uiso 1 1 calc R . . H25D H 0.6002 0.227 0.4146 0.063 Uiso 1 1 calc R . . C253 C 0.6397(8) 0.1368(5) 0.4970(11) 0.057(4) Uani 1 1 d . . . H25E H 0.5859 0.1152 0.4646 0.069 Uiso 1 1 calc R . . H25F H 0.6624 0.122 0.5783 0.069 Uiso 1 1 calc R . . C254 C 0.6961(8) 0.1126(8) 0.4286(12) 0.085(5) Uani 1 1 d . . . H25G H 0.701 0.0636 0.4338 0.128 Uiso 1 1 calc R . . H25H H 0.7498 0.133 0.4612 0.128 Uiso 1 1 calc R . . H25I H 0.6732 0.1259 0.3475 0.128 Uiso 1 1 calc R . . C26 C 0.5425(6) 0.4065(5) 0.6511(10) 0.029(3) Uani 1 1 d . . . O26 O 0.5964(4) 0.4344(3) 0.6019(7) 0.040(2) Uani 1 1 d . . . C261 C 0.6066(7) 0.5052(5) 0.6134(10) 0.037(3) Uani 1 1 d . . . H26A H 0.6255 0.5174 0.6963 0.045 Uiso 1 1 calc R . . H26B H 0.554 0.5277 0.5771 0.045 Uiso 1 1 calc R . . C262 C 0.6675(6) 0.5285(5) 0.5567(9) 0.031(3) Uani 1 1 d . . . H26C H 0.6511 0.5125 0.4757 0.038 Uiso 1 1 calc R . . H26D H 0.7212 0.5087 0.5975 0.038 Uiso 1 1 calc R . . C263 C 0.6745(6) 0.6052(5) 0.5586(9) 0.032(3) Uani 1 1 d . . . H26E H 0.6198 0.625 0.5255 0.038 Uiso 1 1 calc R . . H26F H 0.6966 0.6207 0.6396 0.038 Uiso 1 1 calc R . . C264 C 0.7294(6) 0.6299(6) 0.4901(9) 0.041(3) Uani 1 1 d . . . H26G H 0.7313 0.6791 0.4918 0.062 Uiso 1 1 calc R . . H26H H 0.7078 0.6145 0.4099 0.062 Uiso 1 1 calc R . . H26I H 0.7843 0.6119 0.5246 0.062 Uiso 1 1 calc R . . C27 C 0.5016(6) 0.4429(5) 0.7102(10) 0.029(3) Uani 1 1 d . . . H27 H 0.5078 0.4902 0.7185 0.035 Uiso 1 1 calc R . . C27A C 0.4503(7) 0.4078(5) 0.7578(10) 0.034(3) Uani 1 1 d . . . C2 C 0.3875(6) 0.4970(4) 0.8534(9) 0.030(3) Uani 1 1 d . . . H2A H 0.4408 0.5199 0.8809 0.036 Uiso 1 1 calc R . . H2B H 0.3634 0.4974 0.9173 0.036 Uiso 1 1 calc R . . C31 C 0.2477(7) 0.5371(5) 0.7203(9) 0.035(3) Uani 1 1 d . . . C32 C 0.3332(7) 0.5356(5) 0.7531(10) 0.040(3) Uani 1 1 d . . . C33 C 0.3708(7) 0.5798(5) 0.6954(10) 0.035(3) Uani 1 1 d . . . H33 H 0.4284 0.5808 0.7187 0.042 Uiso 1 1 calc R . . C34 C 0.3289(7) 0.6220(6) 0.6067(9) 0.039(3) Uani 1 1 d . . . H34 H 0.3575 0.6501 0.5694 0.047 Uiso 1 1 calc R . . C35 C 0.2466(8) 0.6228(6) 0.5737(11) 0.054(3) Uani 1 1 d . . . H35 H 0.2167 0.6503 0.5113 0.065 Uiso 1 1 calc R . . C36 C 0.2066(8) 0.5827(6) 0.6325(12) 0.061(4) Uani 1 1 d . . . H36 H 0.1492 0.5861 0.613 0.073 Uiso 1 1 calc R . . C3 C 0.1995(6) 0.4966(5) 0.7771(10) 0.034(3) Uani 1 1 d . . . H3A H 0.2299 0.4941 0.8606 0.041 Uiso 1 1 calc R . . H3B H 0.1482 0.5209 0.7696 0.041 Uiso 1 1 calc RD . . N41 N 0.1661(5) 0.3182(4) 0.7411(7) 0.027(2) Uani 1 1 d . A . C42 C 0.2058(6) 0.3720(6) 0.8029(9) 0.035(3) Uani 1 1 d . . . N43 N 0.1789(5) 0.4275(4) 0.7339(8) 0.034(2) Uani 1 1 d . . . C43A C 0.1225(7) 0.4068(6) 0.6286(11) 0.038(3) Uani 1 1 d . A . C44 C 0.0824(6) 0.4427(6) 0.5299(11) 0.043(3) Uani 1 1 d . . . H44 H 0.0861 0.4903 0.5269 0.052 Uiso 1 1 calc R . . C45 C 0.0367(7) 0.4060(7) 0.4364(11) 0.045(3) Uani 1 1 d U A . O45 O -0.0042(5) 0.4381(4) 0.3341(7) 0.055(2) Uani 1 1 d DU . . C451 C 0.0442(14) 0.4324(13) 0.2578(18) 0.067(4) Uiso 0.5 1 d PDU A 1 H45A H 0.0534 0.3845 0.244 0.08 Uiso 0.5 1 calc PR A 1 H45B H 0.0976 0.4542 0.2927 0.08 Uiso 0.5 1 calc PR A 1 C452 C -0.0004(15) 0.4663(10) 0.146(2) 0.073(6) Uiso 0.5 1 d PDU A 1 H45C H -0.0244 0.5085 0.1632 0.088 Uiso 0.5 1 calc PR A 1 H45D H 0.0393 0.4784 0.1054 0.088 Uiso 0.5 1 calc PR A 1 C453 C -0.0660(14) 0.4251(14) 0.0663(16) 0.124(9) Uiso 0.5 1 d PDU A 1 H45E H -0.1164 0.4336 0.0864 0.149 Uiso 0.5 1 calc PR A 1 H45F H -0.0752 0.4426 -0.0129 0.149 Uiso 0.5 1 calc PR A 1 C454 C -0.0562(16) 0.3525(14) 0.062(3) 0.198(16) Uiso 0.5 1 d PDU A 1 H45G H -0.1065 0.3326 0.0117 0.297 Uiso 0.5 1 calc PRD A 1 H45H H -0.044 0.3338 0.1398 0.297 Uiso 0.5 1 calc PR A 1 H45I H -0.0115 0.3424 0.0309 0.297 Uiso 0.5 1 calc PR A 1 C455 C 0.0337(13) 0.4943(9) 0.291(2) 0.068(4) Uani 0.5 1 d PDU A 2 H45J H -0.0089 0.5177 0.2301 0.081 Uiso 0.5 1 calc PR A 2 H45K H 0.0551 0.5266 0.3556 0.081 Uiso 0.5 1 calc PR A 2 C456 C 0.1006(15) 0.4762(11) 0.245(2) 0.084(6) Uani 0.5 1 d PDU A 2 H45L H 0.079 0.4462 0.1774 0.101 Uiso 0.5 1 calc PR A 2 H45M H 0.1425 0.451 0.3044 0.101 Uiso 0.5 1 calc PR A 2 C457 C 0.1397(12) 0.5363(10) 0.208(2) 0.092(6) Uani 0.5 1 d PDU A 2 H45N H 0.144 0.5732 0.2646 0.11 Uiso 0.5 1 calc PR A 2 H45O H 0.1953 0.5244 0.2088 0.11 Uiso 0.5 1 calc PR A 2 C458 C 0.0913(17) 0.5601(14) 0.090(2) 0.097(7) Uani 0.5 1 d PDU A 2 H45P H 0.1186 0.5987 0.0679 0.146 Uiso 0.5 1 calc PR A 2 H45Q H 0.0368 0.5733 0.0896 0.146 Uiso 0.5 1 calc PR A 2 H45R H 0.0871 0.5237 0.0338 0.146 Uiso 0.5 1 calc PR A 2 C46 C 0.0304(7) 0.3369(7) 0.4395(12) 0.049(4) Uani 1 1 d . . . O46 O -0.0144(5) 0.3067(5) 0.3402(8) 0.076(3) Uani 1 1 d . A . C461 C -0.0295(9) 0.2376(8) 0.3400(13) 0.093(5) Uani 1 1 d U . . H46A H -0.0584 0.2274 0.3966 0.111 Uiso 1 1 calc R A . H46B H 0.0227 0.213 0.3634 0.111 Uiso 1 1 calc R . . C462 C -0.0802(8) 0.2146(8) 0.2211(14) 0.105(5) Uani 1 1 d U A . H46C H -0.0524 0.2248 0.1631 0.126 Uiso 1 1 calc R . . H46D H -0.0903 0.1657 0.2207 0.126 Uiso 1 1 calc R . . C463 C -0.1581(9) 0.2528(10) 0.1957(16) 0.117(6) Uani 1 1 d U . . H46E H -0.1853 0.2517 0.1112 0.14 Uiso 1 1 calc R A . H46F H -0.145 0.3003 0.2178 0.14 Uiso 1 1 calc R . . C464 C -0.2170(11) 0.2286(10) 0.2541(18) 0.147(8) Uani 1 1 d . A . H46G H -0.265 0.2577 0.2331 0.22 Uiso 1 1 calc R . . H46H H -0.1914 0.2297 0.338 0.22 Uiso 1 1 calc R . . H46I H -0.2333 0.1825 0.2296 0.22 Uiso 1 1 calc R . . C47 C 0.0697(7) 0.3016(6) 0.5403(10) 0.045(3) Uani 1 1 d . A . H47 H 0.0644 0.2543 0.5454 0.054 Uiso 1 1 calc R . . C47A C 0.1177(7) 0.3399(6) 0.6345(11) 0.035(3) Uani 1 1 d . . . C4 C 0.1683(7) 0.2499(5) 0.7849(10) 0.042(3) Uani 1 1 d . . . H4A H 0.1131 0.2315 0.7625 0.064 Uiso 1 1 calc R A . H4B H 0.1909 0.2503 0.8693 0.064 Uiso 1 1 calc R . . H4C H 0.2025 0.222 0.7523 0.064 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 0.0369(5) 0.0248(4) 0.0288(5) -0.0013(5) 0.0166(4) -0.0002(5) Br1 0.0454(7) 0.0289(6) 0.0292(7) -0.0037(6) 0.0128(5) -0.0018(6) Br2 0.0487(7) 0.0554(8) 0.0475(8) -0.0003(8) 0.0298(6) -0.0014(8) C1 0.055(8) 0.029(6) 0.044(8) -0.014(6) 0.034(6) 0.001(6) N21 0.031(5) 0.016(5) 0.023(6) 0.001(4) 0.019(4) 0.002(4) C22 0.043(6) 0.024(6) 0.013(5) 0.004(5) 0.014(5) -0.005(6) N23 0.049(6) 0.018(5) 0.034(6) 0.000(4) 0.023(5) -0.005(5) C23A 0.028(7) 0.023(6) 0.026(7) -0.005(5) 0.019(5) -0.003(5) C24 0.043(7) 0.028(6) 0.038(8) 0.004(6) 0.015(6) -0.006(6) C25 0.048(8) 0.015(6) 0.051(9) -0.011(6) 0.029(7) 0.008(6) O25 0.070(6) 0.019(4) 0.055(6) -0.001(4) 0.050(5) -0.006(4) C251 0.074(9) 0.017(6) 0.069(10) -0.007(6) 0.044(8) -0.005(6) C252 0.078(10) 0.035(7) 0.055(9) -0.013(6) 0.036(7) -0.001(7) C253 0.086(10) 0.036(8) 0.057(9) 0.004(7) 0.032(7) 0.013(8) C254 0.078(10) 0.095(12) 0.084(12) -0.002(10) 0.026(9) 0.032(10) C26 0.039(7) 0.020(6) 0.033(8) 0.001(5) 0.020(6) -0.002(5) O26 0.055(5) 0.012(4) 0.065(6) -0.001(4) 0.036(5) -0.004(4) C261 0.049(8) 0.028(6) 0.043(8) -0.010(6) 0.027(6) -0.007(6) C262 0.038(7) 0.031(6) 0.025(7) -0.011(5) 0.010(5) 0.000(6) C263 0.044(7) 0.026(6) 0.031(7) -0.002(5) 0.019(5) -0.008(5) C264 0.049(7) 0.040(6) 0.039(7) -0.008(7) 0.018(6) 0.007(7) C27 0.039(7) 0.013(5) 0.045(8) 0.000(5) 0.027(6) -0.008(5) C27A 0.047(8) 0.023(6) 0.028(8) -0.001(6) 0.008(6) 0.007(6) C2 0.047(7) 0.009(5) 0.039(8) -0.008(5) 0.020(6) 0.003(5) C31 0.040(7) 0.039(7) 0.033(8) -0.006(6) 0.020(6) 0.007(6) C32 0.069(9) 0.035(7) 0.028(7) 0.003(6) 0.033(7) 0.011(7) C33 0.035(7) 0.035(7) 0.038(8) -0.001(6) 0.014(6) 0.012(6) C34 0.057(8) 0.026(6) 0.037(7) 0.004(6) 0.016(6) -0.001(7) C35 0.070(9) 0.040(7) 0.054(9) 0.014(7) 0.022(7) -0.008(9) C36 0.048(9) 0.055(9) 0.075(11) 0.007(8) 0.012(8) 0.017(7) C3 0.036(7) 0.016(6) 0.057(9) 0.003(6) 0.022(6) 0.007(5) N41 0.036(6) 0.032(5) 0.016(6) -0.002(5) 0.010(4) -0.006(5) C42 0.035(6) 0.033(6) 0.042(7) -0.007(7) 0.018(5) 0.000(7) N43 0.028(6) 0.027(5) 0.046(7) -0.001(5) 0.012(5) 0.003(5) C43A 0.033(7) 0.046(8) 0.035(9) 0.014(7) 0.011(6) 0.015(7) C44 0.027(7) 0.044(7) 0.060(10) -0.006(7) 0.015(6) 0.003(6) C45 0.044(7) 0.056(7) 0.045(7) 0.013(6) 0.029(6) 0.022(6) O45 0.055(4) 0.062(4) 0.050(5) 0.013(4) 0.021(4) 0.017(4) C455 0.069(7) 0.077(7) 0.063(7) 0.032(6) 0.029(6) 0.034(6) C456 0.073(13) 0.101(14) 0.087(14) 0.016(12) 0.039(10) 0.009(11) C457 0.074(14) 0.100(15) 0.094(16) 0.024(13) 0.017(11) -0.003(12) C458 0.083(15) 0.100(16) 0.098(17) 0.022(13) 0.010(12) 0.001(14) C46 0.038(8) 0.058(9) 0.045(10) -0.010(8) 0.005(7) 0.009(7) O46 0.064(7) 0.096(8) 0.045(7) -0.026(6) -0.015(5) 0.002(6) C461 0.066(9) 0.127(13) 0.079(11) -0.059(10) 0.014(7) -0.017(10) C462 0.066(9) 0.158(13) 0.088(10) -0.052(10) 0.018(8) -0.017(9) C463 0.062(9) 0.165(15) 0.117(13) -0.057(12) 0.017(9) -0.029(9) C464 0.124(17) 0.19(2) 0.15(2) 0.010(17) 0.079(15) -0.017(16) C47 0.051(8) 0.051(8) 0.035(9) -0.011(7) 0.017(7) -0.006(7) C47A 0.034(7) 0.041(8) 0.039(9) -0.004(7) 0.025(6) 0.004(6) C4 0.055(8) 0.033(7) 0.036(8) 0.014(6) 0.008(6) -0.010(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C42 1.941(10) . ? Pd1 C22 1.967(9) . ? Pd1 Br2 2.4767(13) . ? Pd1 Br1 2.4842(13) . ? C1 N23 1.480(11) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? N21 C22 1.374(11) . ? N21 C27A 1.411(13) . ? N21 C2 1.471(11) . ? C22 N23 1.334(12) . ? N23 C23A 1.395(12) . ? C23A C27A 1.365(12) . ? C23A C24 1.414(14) . ? C24 C25 1.379(14) . ? C24 H24 0.95 . ? C25 O25 1.368(12) . ? C25 C26 1.460(12) . ? O25 C251 1.454(11) . ? C251 C252 1.511(15) . ? C251 H25A 0.99 . ? C251 H25B 0.99 . ? C252 C253 1.514(14) . ? C252 H25C 0.99 . ? C252 H25D 0.99 . ? C253 C254 1.542(16) . ? C253 H25E 0.99 . ? C253 H25F 0.99 . ? C254 H25G 0.98 . ? C254 H25H 0.98 . ? C254 H25I 0.98 . ? C26 C27 1.363(13) . ? C26 O26 1.371(11) . ? O26 C261 1.422(11) . ? C261 C262 1.500(13) . ? C261 H26A 0.99 . ? C261 H26B 0.99 . ? C262 C263 1.533(12) . ? C262 H26C 0.99 . ? C262 H26D 0.99 . ? C263 C264 1.525(13) . ? C263 H26E 0.99 . ? C263 H26F 0.99 . ? C264 H26G 0.98 . ? C264 H26H 0.98 . ? C264 H26I 0.98 . ? C27 C27A 1.389(14) . ? C27 H27 0.95 . ? C2 C32 1.501(14) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C31 C32 1.409(14) . ? C31 C36 1.415(15) . ? C31 C3 1.477(14) . ? C32 C33 1.405(14) . ? C33 C34 1.383(14) . ? C33 H33 0.95 . ? C34 C35 1.357(14) . ? C34 H34 0.95 . ? C35 C36 1.390(16) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C3 N43 1.478(12) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? N41 C42 1.366(12) . ? N41 C47A 1.378(13) . ? N41 C4 1.456(12) . ? C42 N43 1.379(12) . ? N43 C43A 1.412(13) . ? C43A C47A 1.338(13) . ? C43A C44 1.387(15) . ? C44 C45 1.378(16) . ? C44 H44 0.95 . ? C45 O45 1.385(13) . ? C45 C46 1.383(15) . ? O45 C451 1.43(3) . ? O45 C455 1.471(9) . ? C451 C452 1.503(17) . ? C451 H45A 0.99 . ? C451 H45B 0.99 . ? C452 C453 1.490(16) . ? C452 H45C 0.99 . ? C452 H45D 0.99 . ? C453 C454 1.459(18) . ? C453 H45E 0.99 . ? C453 H45F 0.99 . ? C454 H45G 0.98 . ? C454 H45H 0.98 . ? C454 H45I 0.98 . ? C455 C456 1.483(17) . ? C455 H45J 0.99 . ? C455 H45K 0.99 . ? C456 C457 1.507(17) . ? C456 H45L 0.99 . ? C456 H45M 0.99 . ? C457 C458 1.506(18) . ? C457 H45N 0.99 . ? C457 H45O 0.99 . ? C458 H45P 0.98 . ? C458 H45Q 0.98 . ? C458 H45R 0.98 . ? C46 O46 1.358(13) . ? C46 C47 1.395(15) . ? O46 C461 1.400(16) . ? C461 C462 1.513(18) . ? C461 H46A 0.99 . ? C461 H46B 0.99 . ? C462 C463 1.496(19) . ? C462 H46C 0.99 . ? C462 H46D 0.99 . ? C463 C464 1.49(2) . ? C463 H46E 0.99 . ? C463 H46F 0.99 . ? C464 H46G 0.98 . ? C464 H46H 0.98 . ? C464 H46I 0.98 . ? C47 C47A 1.414(15) . ? C47 H47 0.95 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? 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 C42 Pd1 C22 85.7(4) . . ? C42 Pd1 Br2 90.1(3) . . ? C22 Pd1 Br2 175.6(3) . . ? C42 Pd1 Br1 172.9(3) . . ? C22 Pd1 Br1 88.4(3) . . ? Br2 Pd1 Br1 95.95(5) . . ? N23 C1 H1A 109.5 . . ? N23 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N23 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C22 N21 C27A 110.4(8) . . ? C22 N21 C2 125.7(8) . . ? C27A N21 C2 123.9(8) . . ? N23 C22 N21 106.1(8) . . ? N23 C22 Pd1 128.5(7) . . ? N21 C22 Pd1 125.4(7) . . ? C22 N23 C23A 110.3(8) . . ? C22 N23 C1 125.7(9) . . ? C23A N23 C1 123.5(9) . . ? C27A C23A N23 108.3(10) . . ? C27A C23A C24 123.7(10) . . ? N23 C23A C24 128.0(9) . . ? C25 C24 C23A 115.2(9) . . ? C25 C24 H24 122.4 . . ? C23A C24 H24 122.4 . . ? O25 C25 C24 125.6(9) . . ? O25 C25 C26 113.7(10) . . ? C24 C25 C26 120.6(10) . . ? C25 O25 C251 115.7(8) . . ? O25 C251 C252 107.3(8) . . ? O25 C251 H25A 110.2 . . ? C252 C251 H25A 110.2 . . ? O25 C251 H25B 110.2 . . ? C252 C251 H25B 110.2 . . ? H25A C251 H25B 108.5 . . ? C251 C252 C253 110.6(10) . . ? C251 C252 H25C 109.5 . . ? C253 C252 H25C 109.5 . . ? C251 C252 H25D 109.5 . . ? C253 C252 H25D 109.5 . . ? H25C C252 H25D 108.1 . . ? C252 C253 C254 113.6(10) . . ? C252 C253 H25E 108.8 . . ? C254 C253 H25E 108.8 . . ? C252 C253 H25F 108.8 . . ? C254 C253 H25F 108.8 . . ? H25E C253 H25F 107.7 . . ? C253 C254 H25G 109.5 . . ? C253 C254 H25H 109.5 . . ? H25G C254 H25H 109.5 . . ? C253 C254 H25I 109.5 . . ? H25G C254 H25I 109.5 . . ? H25H C254 H25I 109.5 . . ? C27 C26 O26 123.3(9) . . ? C27 C26 C25 121.6(10) . . ? O26 C26 C25 115.0(10) . . ? C26 O26 C261 116.1(8) . . ? O26 C261 C262 110.2(8) . . ? O26 C261 H26A 109.6 . . ? C262 C261 H26A 109.6 . . ? O26 C261 H26B 109.6 . . ? C262 C261 H26B 109.6 . . ? H26A C261 H26B 108.1 . . ? C261 C262 C263 111.4(8) . . ? C261 C262 H26C 109.3 . . ? C263 C262 H26C 109.3 . . ? C261 C262 H26D 109.3 . . ? C263 C262 H26D 109.3 . . ? H26C C262 H26D 108 . . ? C264 C263 C262 111.9(8) . . ? C264 C263 H26E 109.2 . . ? C262 C263 H26E 109.2 . . ? C264 C263 H26F 109.2 . . ? C262 C263 H26F 109.2 . . ? H26E C263 H26F 107.9 . . ? C263 C264 H26G 109.5 . . ? C263 C264 H26H 109.5 . . ? H26G C264 H26H 109.5 . . ? C263 C264 H26I 109.5 . . ? H26G C264 H26I 109.5 . . ? H26H C264 H26I 109.5 . . ? C26 C27 C27A 117.1(9) . . ? C26 C27 H27 121.4 . . ? C27A C27 H27 121.5 . . ? C23A C27A C27 121.6(11) . . ? C23A C27A N21 104.8(10) . . ? C27 C27A N21 133.5(9) . . ? N21 C2 C32 113.1(8) . . ? N21 C2 H2A 109 . . ? C32 C2 H2A 109 . . ? N21 C2 H2B 109 . . ? C32 C2 H2B 109 . . ? H2A C2 H2B 107.8 . . ? C32 C31 C36 117.9(11) . . ? C32 C31 C3 123.5(10) . . ? C36 C31 C3 118.6(11) . . ? C33 C32 C31 116.9(10) . . ? C33 C32 C2 117.2(11) . . ? C31 C32 C2 125.5(10) . . ? C34 C33 C32 124.0(11) . . ? C34 C33 H33 118 . . ? C32 C33 H33 118 . . ? C35 C34 C33 119.2(11) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? C34 C35 C36 119.0(12) . . ? C34 C35 H35 120.5 . . ? C36 C35 H35 120.5 . . ? C35 C36 C31 122.9(12) . . ? C35 C36 H36 118.6 . . ? C31 C36 H36 118.6 . . ? N43 C3 C31 116.8(9) . . ? N43 C3 H3A 108.1 . . ? C31 C3 H3A 108.1 . . ? N43 C3 H3B 108.1 . . ? C31 C3 H3B 108.1 . . ? H3A C3 H3B 107.3 . . ? C42 N41 C47A 109.2(9) . . ? C42 N41 C4 125.3(9) . . ? C47A N41 C4 125.2(9) . . ? N41 C42 N43 106.0(8) . . ? N41 C42 Pd1 128.8(8) . . ? N43 C42 Pd1 125.0(8) . . ? C42 N43 C43A 109.1(8) . . ? C42 N43 C3 122.1(9) . . ? C43A N43 C3 128.2(9) . . ? C47A C43A C44 122.5(13) . . ? C47A C43A N43 106.2(11) . . ? C44 C43A N43 131.1(11) . . ? C45 C44 C43A 116.6(12) . . ? C45 C44 H44 121.7 . . ? C43A C44 H44 121.7 . . ? C44 C45 O45 120.1(12) . . ? C44 C45 C46 122.4(13) . . ? O45 C45 C46 117.5(13) . . ? C45 O45 C451 107.8(11) . . ? C45 O45 C455 120.5(14) . . ? O45 C451 C452 108(2) . . ? O45 C451 H45A 110 . . ? C452 C451 H45A 110 . . ? O45 C451 H45B 110 . . ? C452 C451 H45B 110.1 . . ? H45A C451 H45B 108.4 . . ? C453 C452 C451 114.7(14) . . ? C453 C452 H45C 108.7 . . ? C451 C452 H45C 108.6 . . ? C453 C452 H45D 108.4 . . ? C451 C452 H45D 108.6 . . ? H45C C452 H45D 107.6 . . ? C454 C453 C452 119.7(15) . . ? C454 C453 H45E 107.3 . . ? C452 C453 H45E 107.2 . . ? C454 C453 H45F 107.6 . . ? C452 C453 H45F 107.5 . . ? H45E C453 H45F 107 . . ? C453 C454 H45G 109.5 . . ? C453 C454 H45H 109.6 . . ? H45G C454 H45H 109.5 . . ? C453 C454 H45I 109.3 . . ? H45G C454 H45I 109.5 . . ? H45H C454 H45I 109.5 . . ? C456 C455 O45 115.9(16) . . ? C456 C455 H45J 108.3 . . ? O45 C455 H45J 108.3 . . ? C456 C455 H45K 108.3 . . ? O45 C455 H45K 108.3 . . ? H45J C455 H45K 107.4 . . ? C455 C456 C457 113.2(15) . . ? C455 C456 H45L 108.9 . . ? C457 C456 H45L 108.9 . . ? C455 C456 H45M 109 . . ? C457 C456 H45M 108.9 . . ? H45L C456 H45M 107.8 . . ? C458 C457 C456 111.4(16) . . ? C458 C457 H45N 109.4 . . ? C456 C457 H45N 109.4 . . ? C458 C457 H45O 109.3 . . ? C456 C457 H45O 109.4 . . ? H45N C457 H45O 108 . . ? C457 C458 H45P 109.5 . . ? C457 C458 H45Q 109.5 . . ? H45P C458 H45Q 109.5 . . ? C457 C458 H45R 109.5 . . ? H45P C458 H45R 109.5 . . ? H45Q C458 H45R 109.5 . . ? O46 C46 C45 116.4(13) . . ? O46 C46 C47 123.3(12) . . ? C45 C46 C47 120.3(13) . . ? C46 O46 C461 119.4(11) . . ? O46 C461 C462 110.6(14) . . ? O46 C461 H46A 109.5 . . ? C462 C461 H46A 109.5 . . ? O46 C461 H46B 109.5 . . ? C462 C461 H46B 109.5 . . ? H46A C461 H46B 108.1 . . ? C463 C462 C461 105.3(13) . . ? C463 C462 H46C 110.7 . . ? C461 C462 H46C 110.7 . . ? C463 C462 H46D 110.7 . . ? C461 C462 H46D 110.7 . . ? H46C C462 H46D 108.8 . . ? C462 C463 C464 116.2(18) . . ? C462 C463 H46E 108.2 . . ? C464 C463 H46E 108.2 . . ? C462 C463 H46F 108.2 . . ? C464 C463 H46F 108.2 . . ? H46E C463 H46F 107.4 . . ? C463 C464 H46G 109.5 . . ? C463 C464 H46H 109.5 . . ? H46G C464 H46H 109.5 . . ? C463 C464 H46I 109.5 . . ? H46G C464 H46I 109.5 . . ? H46H C464 H46I 109.5 . . ? C46 C47 C47A 116.5(11) . . ? C46 C47 H47 121.7 . . ? C47A C47 H47 121.7 . . ? C43A C47A N41 109.4(11) . . ? C43A C47A C47 121.6(13) . . ? N41 C47A C47 129.0(11) . . ? N41 C4 H4A 109.5 . . ? N41 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N41 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? #===END data_ps93f4 _database_code_depnum_ccdc_archive 'CCDC 726628' _audit_creation_date 2009-07-14T12:20:34-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C40.84 H54.84 Br2 Cl2.53 N4 O4 Pd' _chemical_formula_moiety 'C40 H54 Br2 N4 O4 Pd, 0.84(C H Cl3)' _chemical_formula_weight 1021.72 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2/c 1' _symmetry_space_group_name_Hall -p_2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 20.4781(5) _cell_length_b 9.9160(2) _cell_length_c 25.6217(7) _cell_angle_alpha 90 _cell_angle_beta 113.190(3) _cell_angle_gamma 90 _cell_volume 4782.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 10784 _cell_measurement_theta_min 2.6153 _cell_measurement_theta_max 27.9929 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour pale_yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.095 _exptl_crystal_size_min 0.085 _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2076 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.241 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.88981 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 0.0197690825 _diffrn_orient_matrix_ub_12 0.0304385822 _diffrn_orient_matrix_ub_13 0.0265427466 _diffrn_orient_matrix_ub_21 0.012921515 _diffrn_orient_matrix_ub_22 -0.0641396033 _diffrn_orient_matrix_ub_23 0.0116976383 _diffrn_orient_matrix_ub_31 0.0292345035 _diffrn_orient_matrix_ub_32 0.0076625078 _diffrn_orient_matrix_ub_33 -0.0079220113 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_av_unetI/netI 0.0847 _diffrn_reflns_number 44053 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 28.03 _diffrn_reflns_theta_full 27.0 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.919 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 10634 _reflns_number_gt 5718 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0711P)^2^+21.2762P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10634 _refine_ls_number_parameters 495 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.134 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.2248 _refine_ls_wR_factor_gt 0.2043 _refine_ls_goodness_of_fit_ref 1.12 _refine_ls_restrained_S_all 1.131 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.772 _refine_diff_density_min -0.59 _refine_diff_density_rms 0.109 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.24287(3) 0.61684(7) 0.48336(3) 0.0446(2) Uani 1 1 d . . . Br1 Br 0.26544(5) 0.39586(11) 0.52963(4) 0.0646(3) Uani 1 1 d . . . Br2 Br 0.22457(6) 0.84677(10) 0.44760(5) 0.0708(3) Uani 1 1 d . . . C1 C 0.1302(5) 0.7516(10) 0.5454(4) 0.058(2) Uani 1 1 d . . . H1A H 0.1192 0.8444 0.5351 0.088 Uiso 1 1 calc R . . H1B H 0.1809 0.74 0.5621 0.088 Uiso 1 1 calc R . . H1C H 0.1105 0.7255 0.5722 0.088 Uiso 1 1 calc R . . N21 N 0.0953(3) 0.5364(7) 0.4255(3) 0.0435(15) Uani 1 1 d . . . C22 C 0.1409(4) 0.6079(8) 0.4711(3) 0.0460(19) Uani 1 1 d . . . N23 N 0.1005(3) 0.6685(7) 0.4953(3) 0.0424(15) Uani 1 1 d . . . C23A C 0.0288(4) 0.6396(8) 0.4645(3) 0.0429(19) Uani 1 1 d . . . C24 C -0.0319(4) 0.6800(8) 0.4729(4) 0.047(2) Uani 1 1 d . . . O24 O -0.0220(3) 0.7588(6) 0.5193(2) 0.0546(15) Uani 1 1 d . . . C241 C -0.0829(5) 0.8203(10) 0.5230(4) 0.063(3) Uani 1 1 d D . . H24A H -0.1175 0.7519 0.5215 0.076 Uiso 1 1 calc R . . H24B H -0.1048 0.8816 0.4913 0.076 Uiso 1 1 calc R . . C242 C -0.0598(5) 0.8960(10) 0.5780(4) 0.076(3) Uani 1 1 d D . . H24C H -0.1016 0.9329 0.5818 0.091 Uiso 1 1 calc R . . H24D H -0.0379 0.8331 0.609 0.091 Uiso 1 1 calc R . . C243 C -0.0102(6) 1.0053(10) 0.5834(4) 0.084(3) Uani 1 1 d D . . H24E H -0.0306 1.0646 0.5509 0.101 Uiso 1 1 calc R . . H24F H 0.0331 0.9677 0.5826 0.101 Uiso 1 1 calc R . . C244 C 0.0086(8) 1.0887(12) 0.6374(5) 0.112(5) Uani 1 1 d D . . H24G H -0.0337 1.1298 0.6378 0.168 Uiso 1 1 calc R . . H24H H 0.042 1.1575 0.6384 0.168 Uiso 1 1 calc R . . H24I H 0.0292 1.0312 0.6699 0.168 Uiso 1 1 calc R . . C25 C -0.0960(4) 0.6345(9) 0.4338(4) 0.057(2) Uani 1 1 d . . . H25 H -0.1376 0.6601 0.4376 0.068 Uiso 1 1 calc R . . C26 C -0.1002(4) 0.5496(9) 0.3879(4) 0.054(2) Uani 1 1 d . . . H26 H -0.1445 0.5211 0.3623 0.065 Uiso 1 1 calc R . . C27 C -0.0400(4) 0.5084(8) 0.3805(4) 0.048(2) Uani 1 1 d . . . O27 O -0.0393(3) 0.4270(6) 0.3374(3) 0.0581(16) Uani 1 1 d . . . C271 C -0.1042(5) 0.3641(10) 0.3014(4) 0.063(3) Uani 1 1 d D . . H27A H -0.1381 0.4324 0.28 0.075 Uiso 1 1 calc R . . H27B H -0.1243 0.3153 0.3244 0.075 Uiso 1 1 calc R . . C272 C -0.0910(5) 0.2705(9) 0.2622(4) 0.064(3) Uani 1 1 d D . . H27C H -0.0527 0.2097 0.2837 0.076 Uiso 1 1 calc R . . H27D H -0.0758 0.3214 0.2366 0.076 Uiso 1 1 calc R . . C273 C -0.1557(6) 0.1889(13) 0.2278(5) 0.100(4) Uani 1 1 d D . . H27E H -0.1694 0.1349 0.2535 0.12 Uiso 1 1 calc R . . H27F H -0.1946 0.25 0.208 0.12 Uiso 1 1 calc R . . C274 C -0.1452(8) 0.0997(13) 0.1863(6) 0.118(5) Uani 1 1 d D . . H27G H -0.1502 0.1504 0.1531 0.178 Uiso 1 1 calc R . . H27H H -0.18 0.0289 0.1761 0.178 Uiso 1 1 calc R . . H27I H -0.0985 0.0611 0.2026 0.178 Uiso 1 1 calc R . . C27A C 0.0244(4) 0.5561(8) 0.4196(3) 0.0412(18) Uani 1 1 d . . . C2 C 0.1212(4) 0.4558(8) 0.3880(4) 0.0459(19) Uani 1 1 d . . . H2A H 0.0835 0.3958 0.3647 0.055 Uiso 1 1 calc R . . H2B H 0.1609 0.4005 0.4116 0.055 Uiso 1 1 calc R . . C31 C 0.2135(4) 0.5442(9) 0.3505(3) 0.048(2) Uani 1 1 d . . . C32 C 0.1440(4) 0.5416(8) 0.3500(3) 0.0426(18) Uani 1 1 d . . . C33 C 0.0919(5) 0.6280(9) 0.3113(4) 0.056(2) Uani 1 1 d . . . H33 H 0.0461 0.6287 0.3105 0.068 Uiso 1 1 calc R . . C34 C 0.1078(5) 0.7088(10) 0.2757(4) 0.066(3) Uani 1 1 d . . . H34 H 0.0727 0.764 0.2506 0.079 Uiso 1 1 calc R . . C35 C 0.1743(6) 0.7111(11) 0.2759(4) 0.067(3) Uani 1 1 d . . . H35 H 0.1842 0.7668 0.2508 0.08 Uiso 1 1 calc R . . C36 C 0.2263(5) 0.6320(10) 0.3129(4) 0.060(2) Uani 1 1 d . . . H36 H 0.2718 0.6364 0.3131 0.072 Uiso 1 1 calc R . . C3 C 0.2748(4) 0.4618(9) 0.3884(4) 0.048(2) Uani 1 1 d . . . H3A H 0.2588 0.4037 0.4115 0.057 Uiso 1 1 calc R . . H3B H 0.2908 0.4044 0.3651 0.057 Uiso 1 1 calc R . . N41 N 0.3973(3) 0.6722(7) 0.4971(3) 0.0497(17) Uani 1 1 d . . . C42 C 0.3341(4) 0.6100(9) 0.4720(4) 0.051(2) Uani 1 1 d . . . N43 N 0.3355(3) 0.5431(7) 0.4263(3) 0.0451(16) Uani 1 1 d . . . C43A C 0.4010(4) 0.5641(9) 0.4218(4) 0.049(2) Uani 1 1 d . . . C44 C 0.4281(5) 0.5193(10) 0.3824(4) 0.057(2) Uani 1 1 d . . . O44 O 0.3853(4) 0.4415(8) 0.3394(3) 0.083(2) Uani 1 1 d U B . C441 C 0.4114(7) 0.3942(16) 0.2996(5) 0.116(3) Uani 1 1 d DU . . H44A H 0.4316 0.3047 0.3096 0.139 Uiso 1 1 calc R A 1 H44B H 0.4475 0.4544 0.2972 0.139 Uiso 1 1 calc R A 1 C442 C 0.3472(13) 0.392(3) 0.2445(9) 0.139(5) Uiso 0.5 1 d PDU B 1 H44C H 0.3249 0.4799 0.2372 0.166 Uiso 0.5 1 calc PR B 1 H44D H 0.313 0.3268 0.2469 0.166 Uiso 0.5 1 calc PR B 1 C443 C 0.3698(17) 0.353(4) 0.1961(9) 0.165(7) Uiso 0.5 1 d PDU B 1 H44E H 0.4144 0.3037 0.2104 0.198 Uiso 0.5 1 calc PR B 1 H44F H 0.3749 0.4321 0.1758 0.198 Uiso 0.5 1 calc PR B 1 C444 C 0.308(2) 0.262(4) 0.1573(15) 0.222(13) Uiso 0.5 1 d PDU B 1 H44G H 0.3124 0.2475 0.1218 0.334 Uiso 0.5 1 calc PR B 1 H44H H 0.2634 0.3054 0.1505 0.334 Uiso 0.5 1 calc PR B 1 H44I H 0.3096 0.1768 0.1757 0.334 Uiso 0.5 1 calc PR B 1 C445 C 0.3576(13) 0.288(2) 0.2617(10) 0.119(5) Uiso 0.5 1 d PDU B 2 H44J H 0.382 0.2211 0.2483 0.143 Uiso 0.5 1 calc PR B 2 H44K H 0.3343 0.2423 0.2832 0.143 Uiso 0.5 1 calc PR B 2 C446 C 0.3034(12) 0.363(3) 0.2120(10) 0.148(6) Uiso 0.5 1 d PDU B 2 H44L H 0.2651 0.3025 0.1901 0.178 Uiso 0.5 1 calc PR B 2 H44M H 0.2834 0.4367 0.2256 0.178 Uiso 0.5 1 calc PR B 2 C447 C 0.340(2) 0.417(4) 0.1748(14) 0.188(11) Uiso 0.5 1 d PDU B 2 H44N H 0.3076 0.4761 0.1467 0.282 Uiso 0.5 1 calc PR B 2 H44O H 0.3523 0.343 0.1565 0.282 Uiso 0.5 1 calc PR B 2 H44P H 0.3815 0.4655 0.1979 0.282 Uiso 0.5 1 calc PR B 2 C45 C 0.4949(5) 0.5603(12) 0.3911(4) 0.073(3) Uani 1 1 d . . . H45 H 0.5145 0.5327 0.3658 0.087 Uiso 1 1 calc R . . C46 C 0.5358(5) 0.6439(11) 0.4376(4) 0.070(3) Uani 1 1 d . . . H46 H 0.5812 0.6704 0.4419 0.083 Uiso 1 1 calc R . . C47 C 0.5092(4) 0.6856(10) 0.4761(4) 0.057(2) Uani 1 1 d . . . O47 O 0.5436(3) 0.7673(7) 0.5224(3) 0.0729(18) Uani 1 1 d U . . C471 C 0.6086(5) 0.8277(12) 0.5279(5) 0.085(3) Uani 1 1 d DU . . H47A H 0.6005 0.8921 0.4974 0.103 Uiso 1 1 calc R . . H47B H 0.6411 0.7592 0.5254 0.103 Uiso 1 1 calc R . . C472 C 0.6403(6) 0.8981(12) 0.5844(6) 0.108(3) Uani 1 1 d DU . . H47C H 0.6459 0.8335 0.6143 0.13 Uiso 1 1 calc R . . H47D H 0.687 0.9315 0.5899 0.13 Uiso 1 1 calc R . . C473 C 0.5977(7) 1.0080(13) 0.5890(6) 0.122(4) Uani 1 1 d DU . . H47E H 0.5512 0.9751 0.5845 0.147 Uiso 1 1 calc R . . H47F H 0.5915 1.0729 0.559 0.147 Uiso 1 1 calc R . . C474 C 0.6335(8) 1.0766(16) 0.6469(7) 0.146(6) Uani 1 1 d DU . . H47G H 0.6053 1.1522 0.649 0.219 Uiso 1 1 calc R . . H47H H 0.6799 1.1073 0.6516 0.219 Uiso 1 1 calc R . . H47I H 0.6376 1.0134 0.6764 0.219 Uiso 1 1 calc R . . C47A C 0.4405(4) 0.6454(9) 0.4672(4) 0.050(2) Uani 1 1 d . . . C4 C 0.4152(5) 0.7558(11) 0.5476(4) 0.072(3) Uani 1 1 d . . . H4A H 0.4642 0.7423 0.572 0.108 Uiso 1 1 calc R . . H4B H 0.3858 0.7313 0.5674 0.108 Uiso 1 1 calc R . . H4C H 0.4076 0.849 0.5367 0.108 Uiso 1 1 calc R . . C01 C 0.3062(7) 0.1323(11) 0.6355(6) 0.59(8) Uani 0.843(15) 1 d PD C 1 H01 H 0.2964 0.2247 0.6208 0.711 Uiso 0.843(15) 1 calc PR C 1 Cl1 Cl 0.2877(7) 0.0222(11) 0.5795(6) 0.355(9) Uani 0.843(15) 1 d PRD C 1 Cl2 Cl 0.2494(11) 0.091(2) 0.6660(7) 0.61(2) Uani 0.843(15) 1 d PD C 1 Cl3 Cl 0.3934(10) 0.119(3) 0.6794(9) 0.71(3) Uani 0.843(15) 1 d PD C 1 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 0.0321(3) 0.0499(4) 0.0527(4) -0.0031(3) 0.0175(3) -0.0020(3) Br1 0.0455(5) 0.0717(7) 0.0804(7) 0.0222(5) 0.0288(5) 0.0075(5) Br2 0.0639(6) 0.0567(6) 0.0948(8) 0.0066(5) 0.0344(6) 0.0010(5) C1 0.050(5) 0.066(6) 0.065(6) -0.016(5) 0.028(5) -0.005(5) N21 0.036(4) 0.046(4) 0.049(4) -0.004(3) 0.017(3) -0.002(3) C22 0.039(4) 0.043(5) 0.056(5) -0.005(4) 0.019(4) -0.007(4) N23 0.035(3) 0.045(4) 0.048(4) -0.007(3) 0.017(3) -0.004(3) C23A 0.033(4) 0.040(4) 0.057(5) 0.009(4) 0.019(4) 0.000(3) C24 0.046(5) 0.044(5) 0.057(5) 0.004(4) 0.028(4) 0.008(4) O24 0.042(3) 0.060(4) 0.065(4) -0.006(3) 0.024(3) 0.002(3) C241 0.051(5) 0.067(6) 0.079(7) -0.013(5) 0.034(5) 0.004(5) C242 0.079(7) 0.068(7) 0.099(8) -0.006(6) 0.055(6) 0.014(6) C243 0.101(9) 0.069(7) 0.089(8) -0.005(6) 0.045(7) -0.003(7) C244 0.166(14) 0.073(8) 0.088(9) -0.027(7) 0.042(9) 0.009(8) C25 0.034(4) 0.069(6) 0.071(6) -0.009(5) 0.025(4) -0.001(4) C26 0.029(4) 0.065(6) 0.064(6) -0.008(5) 0.012(4) -0.006(4) C27 0.043(5) 0.040(5) 0.060(5) -0.002(4) 0.018(4) -0.001(4) O27 0.037(3) 0.069(4) 0.065(4) -0.018(3) 0.016(3) -0.011(3) C271 0.045(5) 0.072(7) 0.063(6) 0.000(5) 0.011(4) -0.017(5) C272 0.063(6) 0.062(6) 0.061(6) -0.009(5) 0.019(5) -0.004(5) C273 0.092(9) 0.105(10) 0.092(9) -0.046(8) 0.025(7) -0.027(8) C274 0.119(11) 0.088(10) 0.137(12) -0.031(9) 0.039(10) -0.013(8) C27A 0.035(4) 0.037(4) 0.054(5) 0.003(4) 0.020(4) 0.000(3) C2 0.039(4) 0.041(4) 0.059(5) -0.004(4) 0.021(4) 0.002(4) C31 0.048(5) 0.052(5) 0.045(5) -0.005(4) 0.020(4) -0.004(4) C32 0.042(4) 0.041(4) 0.045(4) -0.005(4) 0.018(4) -0.010(4) C33 0.046(5) 0.067(6) 0.048(5) -0.002(5) 0.010(4) 0.006(5) C34 0.065(7) 0.059(6) 0.061(6) 0.019(5) 0.011(5) 0.003(5) C35 0.072(7) 0.073(7) 0.059(6) 0.011(5) 0.031(5) -0.008(6) C36 0.049(5) 0.073(7) 0.063(6) 0.002(5) 0.027(5) -0.007(5) C3 0.038(4) 0.052(5) 0.060(5) -0.003(4) 0.027(4) 0.000(4) N41 0.038(4) 0.059(4) 0.051(4) -0.002(4) 0.017(3) -0.007(3) C42 0.042(5) 0.051(5) 0.057(5) 0.010(4) 0.016(4) 0.005(4) N43 0.033(4) 0.051(4) 0.051(4) -0.002(3) 0.017(3) -0.001(3) C43A 0.040(5) 0.049(5) 0.061(5) 0.009(4) 0.022(4) 0.003(4) C44 0.048(5) 0.073(6) 0.057(5) 0.000(5) 0.028(4) 0.008(5) O44 0.076(4) 0.111(5) 0.083(5) -0.023(4) 0.052(4) -0.009(4) C441 0.111(6) 0.134(6) 0.113(5) -0.026(5) 0.056(5) -0.004(5) C45 0.069(7) 0.093(8) 0.074(7) 0.003(6) 0.047(6) 0.003(6) C46 0.045(5) 0.097(8) 0.073(7) 0.008(6) 0.029(5) -0.007(5) C47 0.035(5) 0.067(6) 0.068(6) 0.001(5) 0.021(4) -0.003(4) O47 0.043(3) 0.086(5) 0.093(5) 0.000(4) 0.031(3) -0.013(3) C471 0.051(5) 0.087(6) 0.118(6) -0.007(5) 0.034(5) -0.023(4) C472 0.075(6) 0.090(6) 0.148(7) -0.020(6) 0.031(6) -0.027(5) C473 0.095(7) 0.094(8) 0.164(9) -0.024(7) 0.036(7) -0.024(6) C474 0.128(11) 0.124(11) 0.176(12) -0.051(9) 0.049(10) -0.022(9) C47A 0.042(5) 0.052(5) 0.062(5) 0.010(4) 0.026(4) 0.001(4) C4 0.047(5) 0.094(8) 0.072(7) -0.013(6) 0.020(5) -0.005(5) C01 1.4(2) 0.24(5) 0.15(3) 0.09(3) 0.28(8) 0.17(10) Cl1 0.44(2) 0.169(9) 0.54(3) 0.021(12) 0.277(19) -0.003(10) Cl2 0.80(4) 0.83(5) 0.34(2) 0.22(3) 0.38(3) 0.47(4) Cl3 0.92(6) 0.58(5) 0.34(3) 0.03(3) -0.06(3) -0.24(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C22 1.988(8) . ? Pd1 C42 2.003(8) . ? Pd1 Br2 2.4306(12) . ? Pd1 Br1 2.4472(12) . ? C1 N23 1.442(10) . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? N21 C22 1.372(10) . ? N21 C27A 1.413(9) . ? N21 C2 1.498(10) . ? C22 N23 1.354(10) . ? N23 C23A 1.394(9) . ? C23A C27A 1.392(11) . ? C23A C24 1.400(10) . ? C24 O24 1.371(10) . ? C24 C25 1.376(12) . ? O24 C241 1.424(9) . ? C241 C242 1.500(11) . ? C241 H24A 0.97 . ? C241 H24B 0.97 . ? C242 C243 1.454(11) . ? C242 H24C 0.97 . ? C242 H24D 0.97 . ? C243 C244 1.525(11) . ? C243 H24E 0.97 . ? C243 H24F 0.97 . ? C244 H24G 0.96 . ? C244 H24H 0.96 . ? C244 H24I 0.96 . ? C25 C26 1.422(12) . ? C25 H25 0.93 . ? C26 C27 1.381(11) . ? C26 H26 0.93 . ? C27 O27 1.373(10) . ? C27 C27A 1.388(11) . ? O27 C271 1.428(9) . ? C271 C272 1.470(10) . ? C271 H27A 0.97 . ? C271 H27B 0.97 . ? C272 C273 1.506(11) . ? C272 H27C 0.97 . ? C272 H27D 0.97 . ? C273 C274 1.463(12) . ? C273 H27E 0.97 . ? C273 H27F 0.97 . ? C274 H27G 0.96 . ? C274 H27H 0.96 . ? C274 H27I 0.96 . ? C2 C32 1.499(11) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C31 C36 1.398(12) . ? C31 C32 1.419(11) . ? C31 C3 1.492(11) . ? C32 C33 1.423(11) . ? C33 C34 1.345(12) . ? C33 H33 0.93 . ? C34 C35 1.360(13) . ? C34 H34 0.93 . ? C35 C36 1.361(13) . ? C35 H35 0.93 . ? C36 H36 0.93 . ? C3 N43 1.479(10) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? N41 C42 1.345(10) . ? N41 C47A 1.406(10) . ? N41 C4 1.457(11) . ? C42 N43 1.356(10) . ? N43 C43A 1.406(10) . ? C43A C47A 1.383(12) . ? C43A C44 1.401(11) . ? C44 O44 1.349(11) . ? C44 C45 1.360(13) . ? O44 C441 1.403(13) . ? C441 C442 1.504(17) . ? C441 C445 1.558(17) . ? C441 H44A 0.97 . ? C441 H44B 0.97 . ? C442 C443 1.535(18) . ? C442 H44C 0.97 . ? C442 H44D 0.97 . ? C443 C444 1.554(19) . ? C443 H44E 0.97 . ? C443 H44F 0.97 . ? C444 H44G 0.96 . ? C444 H44H 0.96 . ? C444 H44I 0.96 . ? C445 C446 1.514(18) . ? C445 H44J 0.97 . ? C445 H44K 0.97 . ? C446 C447 1.513(19) . ? C446 H44L 0.97 . ? C446 H44M 0.97 . ? C447 H44N 0.96 . ? C447 H44O 0.96 . ? C447 H44P 0.96 . ? C45 C46 1.422(14) . ? C45 H45 0.93 . ? C46 C47 1.366(13) . ? C46 H46 0.93 . ? C47 O47 1.378(11) . ? C47 C47A 1.392(11) . ? O47 C471 1.416(11) . ? C471 C472 1.505(12) . ? C471 H47A 0.97 . ? C471 H47B 0.97 . ? C472 C473 1.429(13) . ? C472 H47C 0.97 . ? C472 H47D 0.97 . ? C473 C474 1.531(14) . ? C473 H47E 0.97 . ? C473 H47F 0.97 . ? C474 H47G 0.96 . ? C474 H47H 0.96 . ? C474 H47I 0.96 . ? C4 H4A 0.96 . ? C4 H4B 0.96 . ? C4 H4C 0.96 . ? C01 Cl2 1.688(15) . ? C01 Cl3 1.700(15) . ? C01 Cl1 1.7221 . ? C01 H01 0.98 . ? 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 C22 Pd1 C42 163.4(3) . . ? C22 Pd1 Br2 89.2(2) . . ? C42 Pd1 Br2 89.5(2) . . ? C22 Pd1 Br1 91.3(2) . . ? C42 Pd1 Br1 91.8(2) . . ? Br2 Pd1 Br1 173.81(5) . . ? N23 C1 H1A 109.5 . . ? N23 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N23 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C22 N21 C27A 110.2(6) . . ? C22 N21 C2 121.9(6) . . ? C27A N21 C2 127.9(6) . . ? N23 C22 N21 106.6(6) . . ? N23 C22 Pd1 134.6(6) . . ? N21 C22 Pd1 118.5(6) . . ? C22 N23 C23A 110.3(6) . . ? C22 N23 C1 122.6(7) . . ? C23A N23 C1 127.1(7) . . ? C27A C23A N23 107.6(6) . . ? C27A C23A C24 121.6(7) . . ? N23 C23A C24 130.8(8) . . ? O24 C24 C25 126.2(7) . . ? O24 C24 C23A 117.4(7) . . ? C25 C24 C23A 116.5(8) . . ? C24 O24 C241 117.8(6) . . ? O24 C241 C242 108.4(7) . . ? O24 C241 H24A 110 . . ? C242 C241 H24A 110 . . ? O24 C241 H24B 110 . . ? C242 C241 H24B 110 . . ? H24A C241 H24B 108.4 . . ? C243 C242 C241 114.4(8) . . ? C243 C242 H24C 108.7 . . ? C241 C242 H24C 108.7 . . ? C243 C242 H24D 108.7 . . ? C241 C242 H24D 108.7 . . ? H24C C242 H24D 107.6 . . ? C242 C243 C244 114.1(9) . . ? C242 C243 H24E 108.7 . . ? C244 C243 H24E 108.7 . . ? C242 C243 H24F 108.7 . . ? C244 C243 H24F 108.7 . . ? H24E C243 H24F 107.6 . . ? C243 C244 H24G 109.5 . . ? C243 C244 H24H 109.5 . . ? H24G C244 H24H 109.5 . . ? C243 C244 H24I 109.5 . . ? H24G C244 H24I 109.5 . . ? H24H C244 H24I 109.5 . . ? C24 C25 C26 121.7(7) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C27 C26 C25 121.5(8) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? O27 C27 C26 125.2(7) . . ? O27 C27 C27A 118.3(7) . . ? C26 C27 C27A 116.5(8) . . ? C27 O27 C271 118.3(6) . . ? O27 C271 C272 110.0(7) . . ? O27 C271 H27A 109.7 . . ? C272 C271 H27A 109.7 . . ? O27 C271 H27B 109.7 . . ? C272 C271 H27B 109.7 . . ? H27A C271 H27B 108.2 . . ? C271 C272 C273 112.5(8) . . ? C271 C272 H27C 109.1 . . ? C273 C272 H27C 109.1 . . ? C271 C272 H27D 109.1 . . ? C273 C272 H27D 109.1 . . ? H27C C272 H27D 107.8 . . ? C274 C273 C272 113.7(10) . . ? C274 C273 H27E 108.8 . . ? C272 C273 H27E 108.8 . . ? C274 C273 H27F 108.8 . . ? C272 C273 H27F 108.8 . . ? H27E C273 H27F 107.7 . . ? C273 C274 H27G 109.5 . . ? C273 C274 H27H 109.5 . . ? H27G C274 H27H 109.5 . . ? C273 C274 H27I 109.5 . . ? H27G C274 H27I 109.5 . . ? H27H C274 H27I 109.5 . . ? C27 C27A C23A 122.3(7) . . ? C27 C27A N21 132.4(7) . . ? C23A C27A N21 105.3(6) . . ? N21 C2 C32 113.1(7) . . ? N21 C2 H2A 109 . . ? C32 C2 H2A 109 . . ? N21 C2 H2B 109 . . ? C32 C2 H2B 109 . . ? H2A C2 H2B 107.8 . . ? C36 C31 C32 117.7(8) . . ? C36 C31 C3 116.9(7) . . ? C32 C31 C3 125.4(7) . . ? C31 C32 C33 118.0(7) . . ? C31 C32 C2 125.0(7) . . ? C33 C32 C2 117.1(7) . . ? C34 C33 C32 121.1(8) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C33 C34 C35 121.0(9) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C34 C35 C36 120.1(9) . . ? C34 C35 H35 120 . . ? C36 C35 H35 120 . . ? C35 C36 C31 122.1(8) . . ? C35 C36 H36 119 . . ? C31 C36 H36 119 . . ? N43 C3 C31 113.7(7) . . ? N43 C3 H3A 108.8 . . ? C31 C3 H3A 108.8 . . ? N43 C3 H3B 108.8 . . ? C31 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C42 N41 C47A 110.2(7) . . ? C42 N41 C4 123.0(7) . . ? C47A N41 C4 126.8(7) . . ? N41 C42 N43 107.1(7) . . ? N41 C42 Pd1 133.7(7) . . ? N43 C42 Pd1 118.7(6) . . ? C42 N43 C43A 110.0(7) . . ? C42 N43 C3 122.4(6) . . ? C43A N43 C3 127.6(7) . . ? C47A C43A C44 121.6(8) . . ? C47A C43A N43 106.2(7) . . ? C44 C43A N43 132.2(8) . . ? O44 C44 C45 126.3(8) . . ? O44 C44 C43A 117.3(8) . . ? C45 C44 C43A 116.4(9) . . ? C44 O44 C441 118.4(8) . . ? O44 C441 C442 104.2(13) . . ? O44 C441 C445 107.5(15) . . ? O44 C441 H44A 110.9 . . ? C442 C441 H44A 110.9 . . ? O44 C441 H44B 110.9 . . ? C442 C441 H44B 110.9 . . ? H44A C441 H44B 108.9 . . ? C441 C442 C443 109.4(17) . . ? C441 C442 H44C 109.8 . . ? C443 C442 H44C 109.8 . . ? C441 C442 H44D 109.8 . . ? C443 C442 H44D 109.8 . . ? H44C C442 H44D 108.2 . . ? C442 C443 C444 103.4(16) . . ? C442 C443 H44E 111.1 . . ? C444 C443 H44E 111.1 . . ? C442 C443 H44F 111.1 . . ? C444 C443 H44F 111.1 . . ? H44E C443 H44F 109 . . ? C443 C444 H44G 109.5 . . ? C443 C444 H44H 109.5 . . ? H44G C444 H44H 109.5 . . ? C443 C444 H44I 109.5 . . ? H44G C444 H44I 109.5 . . ? H44H C444 H44I 109.5 . . ? C446 C445 C441 107.3(15) . . ? C446 C445 H44J 110.3 . . ? C441 C445 H44J 110.3 . . ? C446 C445 H44K 110.3 . . ? C441 C445 H44K 110.3 . . ? H44J C445 H44K 108.5 . . ? C447 C446 C445 109.0(17) . . ? C447 C446 H44L 109.9 . . ? C445 C446 H44L 109.9 . . ? C447 C446 H44M 109.9 . . ? C445 C446 H44M 109.9 . . ? H44L C446 H44M 108.3 . . ? C446 C447 H44N 109.5 . . ? C446 C447 H44O 109.5 . . ? H44N C447 H44O 109.5 . . ? C446 C447 H44P 109.5 . . ? H44N C447 H44P 109.5 . . ? H44O C447 H44P 109.5 . . ? C44 C45 C46 122.3(9) . . ? C44 C45 H45 118.8 . . ? C46 C45 H45 118.8 . . ? C47 C46 C45 120.7(9) . . ? C47 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C46 C47 O47 125.8(8) . . ? C46 C47 C47A 117.4(9) . . ? O47 C47 C47A 116.8(8) . . ? C47 O47 C471 118.4(7) . . ? O47 C471 C472 108.9(9) . . ? O47 C471 H47A 109.9 . . ? C472 C471 H47A 109.9 . . ? O47 C471 H47B 109.9 . . ? C472 C471 H47B 109.9 . . ? H47A C471 H47B 108.3 . . ? C473 C472 C471 112.8(10) . . ? C473 C472 H47C 109 . . ? C471 C472 H47C 109 . . ? C473 C472 H47D 109 . . ? C471 C472 H47D 109 . . ? H47C C472 H47D 107.8 . . ? C472 C473 C474 110.2(11) . . ? C472 C473 H47E 109.6 . . ? C474 C473 H47E 109.6 . . ? C472 C473 H47F 109.6 . . ? C474 C473 H47F 109.6 . . ? H47E C473 H47F 108.1 . . ? C473 C474 H47G 109.5 . . ? C473 C474 H47H 109.5 . . ? H47G C474 H47H 109.5 . . ? C473 C474 H47I 109.5 . . ? H47G C474 H47I 109.5 . . ? H47H C474 H47I 109.5 . . ? C43A C47A C47 121.6(8) . . ? C43A C47A N41 106.4(7) . . ? C47 C47A N41 132.0(9) . . ? N41 C4 H4A 109.5 . . ? N41 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N41 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Cl2 C01 Cl3 114.2(10) . . ? Cl2 C01 Cl1 105.5(8) . . ? Cl3 C01 Cl1 109.4(9) . . ? Cl2 C01 H01 109.2 . . ? Cl3 C01 H01 109.2 . . ? Cl1 C01 H01 109.2 . . ? #===END #===END data_ps97 _database_code_depnum_ccdc_archive 'CCDC 726629' _audit_creation_date 2009-07-14T09:05:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C55 H69 Br2 N4 O4 Pd' _chemical_formula_moiety 'C40 H54 Br2 N4 O4 Pd, 2.5(C6 H6)' _chemical_formula_weight 1116.36 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' 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 27.2399(9) _cell_length_b 20.8844(4) _cell_length_c 20.5822(4) _cell_angle_alpha 90 _cell_angle_beta 90.149(2) _cell_angle_gamma 90 _cell_volume 11708.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5884 _cell_measurement_theta_min 2.6537 _cell_measurement_theta_max 67.0692 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4600 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.489 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.83269 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 -0.0312483853 _diffrn_orient_matrix_ub_12 -0.0299497138 _diffrn_orient_matrix_ub_13 0.0544742582 _diffrn_orient_matrix_ub_21 -0.044582388 _diffrn_orient_matrix_ub_22 0.04039439 _diffrn_orient_matrix_ub_23 -0.0216581 _diffrn_orient_matrix_ub_31 -0.0161952573 _diffrn_orient_matrix_ub_32 -0.0540486765 _diffrn_orient_matrix_ub_33 -0.0464855023 _diffrn_reflns_av_R_equivalents 0.1055 _diffrn_reflns_av_unetI/netI 0.1172 _diffrn_reflns_number 67877 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 67.74 _diffrn_reflns_theta_full 67.74 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type ; Oxford Diffraction Gemini diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 10449 _reflns_number_gt 3743 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.1026P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10449 _refine_ls_number_parameters 608 _refine_ls_number_restraints 202 _refine_ls_R_factor_all 0.1541 _refine_ls_R_factor_gt 0.073 _refine_ls_wR_factor_ref 0.2103 _refine_ls_wR_factor_gt 0.1813 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.897 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.006 _refine_diff_density_max 2.451 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.125 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.178956(19) 0.62420(2) 0.790804(19) 0.05482(13) Uani 1 1 d . . . Br1 Br 0.15184(3) 0.53859(3) 0.86548(3) 0.0726(2) Uani 1 1 d . . . Br2 Br 0.15451(3) 0.70966(3) 0.86719(3) 0.0693(2) Uani 1 1 d . . . C1 C 0.2824(3) 0.5363(3) 0.7824(4) 0.091(3) Uani 1 1 d . . . H1A H 0.3099 0.5547 0.7579 0.136 Uiso 1 1 calc R . . H1B H 0.2933 0.4968 0.8039 0.136 Uiso 1 1 calc R . . H1C H 0.2713 0.5671 0.8152 0.136 Uiso 1 1 calc R . . N21 N 0.2422(2) 0.5218(2) 0.7382(3) 0.0629(17) Uani 1 1 d . . . C22 C 0.1990(2) 0.5531(3) 0.7306(3) 0.0549(18) Uani 1 1 d . . . N23 N 0.1697(2) 0.5240(2) 0.6865(2) 0.0533(14) Uani 1 1 d . . . C23A C 0.1938(2) 0.4684(2) 0.6645(3) 0.0547(16) Uani 1 1 d U . . C24 C 0.1793(3) 0.4194(3) 0.6214(3) 0.0612(16) Uani 1 1 d U . . O24 O 0.13242(17) 0.4207(2) 0.5972(2) 0.0696(13) Uani 1 1 d U . . C241 C 0.1187(2) 0.3743(3) 0.5502(3) 0.074(2) Uani 1 1 d D B . H24A H 0.1216 0.3306 0.5685 0.089 Uiso 1 1 calc R . . H24B H 0.14 0.3774 0.5115 0.089 Uiso 1 1 calc R . . C242 C 0.0655(3) 0.3885(4) 0.5322(4) 0.117(2) Uani 1 1 d DU . . H24C H 0.0635 0.4282 0.5059 0.14 Uiso 0.5 1 calc PR A 1 H24D H 0.0455 0.3944 0.5718 0.14 Uiso 0.5 1 calc PR A 1 H24E H 0.0479 0.3623 0.5647 0.14 Uiso 0.5 1 d PR A 2 H24F H 0.061 0.4333 0.547 0.14 Uiso 0.5 1 d PR A 2 C243 C 0.0466(4) 0.3313(6) 0.4929(8) 0.122(3) Uiso 0.5 1 d PDU B 1 H24G H 0.0478 0.2924 0.5203 0.146 Uiso 0.5 1 calc PR B 1 H24H H 0.0684 0.3243 0.4551 0.146 Uiso 0.5 1 calc PR B 1 C244 C -0.0074(5) 0.3421(9) 0.4684(10) 0.157(6) Uiso 0.5 1 d PDU B 1 H24I H -0.0149 0.388 0.4688 0.235 Uiso 0.5 1 calc PR B 1 H24J H -0.0302 0.3194 0.497 0.235 Uiso 0.5 1 calc PR B 1 H24K H -0.0107 0.3256 0.424 0.235 Uiso 0.5 1 calc PR B 1 C245 C 0.0421(5) 0.3732(8) 0.4712(7) 0.137(3) Uiso 0.5 1 d PDU B 2 H24L H 0.0415 0.3261 0.4661 0.165 Uiso 0.5 1 calc PR B 2 H24M H 0.0622 0.391 0.4355 0.165 Uiso 0.5 1 calc PR B 2 C246 C -0.0089(4) 0.3978(9) 0.4646(10) 0.161(7) Uiso 0.5 1 d PDU B 2 H24N H -0.0162 0.4263 0.5012 0.242 Uiso 0.5 1 calc PR B 2 H24O H -0.0319 0.3618 0.4646 0.242 Uiso 0.5 1 calc PR B 2 H24P H -0.012 0.4216 0.4238 0.242 Uiso 0.5 1 calc PR B 2 C25 C 0.2133(2) 0.3709(3) 0.6130(3) 0.0620(18) Uani 1 1 d . . . H25 H 0.2042 0.3356 0.5865 0.074 Uiso 1 1 calc R . . C26 C 0.2593(2) 0.3705(3) 0.6404(3) 0.0621(18) Uani 1 1 d . . . H26 H 0.2817 0.3372 0.6298 0.074 Uiso 1 1 calc R . . C27 C 0.2732(3) 0.4179(3) 0.6830(3) 0.0571(19) Uani 1 1 d . . . O27 O 0.31694(17) 0.42113(19) 0.7149(2) 0.0670(14) Uani 1 1 d . . . C271 C 0.3534(2) 0.3717(3) 0.7011(3) 0.070(2) Uani 1 1 d . D . H27A H 0.3605 0.3703 0.654 0.084 Uiso 1 1 calc R . . H27B H 0.3409 0.3292 0.7146 0.084 Uiso 1 1 calc R . . C272 C 0.4002(3) 0.3885(3) 0.7395(4) 0.099(2) Uani 1 1 d DU . . H27C H 0.3923 0.3855 0.7864 0.119 Uiso 0.5 1 calc PR C 1 H27D H 0.425 0.3551 0.7302 0.119 Uiso 0.5 1 calc PR C 1 H27E H 0.4135 0.4293 0.7225 0.119 Uiso 0.5 1 d PR C 2 H27F H 0.3921 0.3948 0.786 0.119 Uiso 0.5 1 d PR C 2 C273 C 0.4232(5) 0.4513(6) 0.7281(6) 0.103(3) Uiso 0.5 1 d PDU D 1 H27G H 0.3992 0.485 0.7399 0.124 Uiso 0.5 1 calc PR D 1 H27H H 0.4516 0.4556 0.758 0.124 Uiso 0.5 1 calc PR D 1 C274 C 0.4400(6) 0.4635(7) 0.6629(6) 0.130(5) Uiso 0.5 1 d PDU D 1 H27I H 0.4657 0.4326 0.6516 0.195 Uiso 0.5 1 calc PR D 1 H27J H 0.4533 0.507 0.6602 0.195 Uiso 0.5 1 calc PR D 1 H27K H 0.4124 0.459 0.6325 0.195 Uiso 0.5 1 calc PR D 1 C275 C 0.4424(5) 0.3419(8) 0.7367(6) 0.127(3) Uiso 0.5 1 d PDU D 2 H27L H 0.4318 0.2989 0.7514 0.153 Uiso 0.5 1 calc PR D 2 H27M H 0.4697 0.3565 0.7649 0.153 Uiso 0.5 1 calc PR D 2 C276 C 0.4589(6) 0.3395(9) 0.6653(7) 0.166(6) Uiso 0.5 1 d PDU D 2 H27N H 0.4326 0.3212 0.6385 0.25 Uiso 0.5 1 calc PR D 2 H27O H 0.4884 0.3128 0.6616 0.25 Uiso 0.5 1 calc PR D 2 H27P H 0.4663 0.3829 0.6502 0.25 Uiso 0.5 1 calc PR D 2 C27A C 0.2399(2) 0.4678(3) 0.6945(3) 0.0589(19) Uani 1 1 d . . . C2 C 0.1232(2) 0.5505(3) 0.6642(3) 0.059(2) Uani 1 1 d . . . H2A H 0.1083 0.5766 0.6991 0.071 Uiso 1 1 calc R . . H2B H 0.1002 0.5153 0.6534 0.071 Uiso 1 1 calc R . . C31 C 0.1303(2) 0.6591(3) 0.6035(3) 0.0558(19) Uani 1 1 d . . . C32 C 0.1318(3) 0.5915(3) 0.6047(3) 0.076(2) Uani 1 1 d . . . C33 C 0.1374(3) 0.5616(3) 0.5465(3) 0.080(2) Uani 1 1 d . . . H33 H 0.1359 0.5161 0.5466 0.096 Uiso 1 1 calc R . . C34 C 0.1450(3) 0.5911(3) 0.4875(4) 0.097(3) Uani 1 1 d . . . H34 H 0.1506 0.5673 0.4489 0.116 Uiso 1 1 calc R . . C35 C 0.1441(3) 0.6568(3) 0.4876(3) 0.077(3) Uani 1 1 d . . . H35 H 0.1466 0.6785 0.4472 0.092 Uiso 1 1 calc R . . C36 C 0.1396(3) 0.6933(3) 0.5438(3) 0.091(3) Uani 1 1 d . . . H36 H 0.1426 0.7386 0.543 0.109 Uiso 1 1 calc R . . C3 C 0.1259(2) 0.7007(3) 0.6643(3) 0.060(2) Uani 1 1 d . . . H3A H 0.1034 0.7367 0.6546 0.072 Uiso 1 1 calc R . . H3B H 0.1107 0.6749 0.6992 0.072 Uiso 1 1 calc R . . N41 N 0.24308(17) 0.7292(2) 0.7375(2) 0.0515(15) Uani 1 1 d . . . C42 C 0.2025(2) 0.6967(3) 0.7311(3) 0.060(2) Uani 1 1 d . . . N43 N 0.17216(18) 0.7268(2) 0.6886(2) 0.0480(14) Uani 1 1 d . . . C43A C 0.1983(2) 0.7811(3) 0.6680(3) 0.0538(18) Uani 1 1 d . . . C44 C 0.1834(3) 0.8324(3) 0.6275(3) 0.060(2) Uani 1 1 d . . . O44 O 0.13650(16) 0.83242(19) 0.6024(2) 0.0640(14) Uani 1 1 d . . . C441 C 0.1225(3) 0.8813(3) 0.5609(3) 0.080(2) Uani 1 1 d . F . H44A H 0.1448 0.8824 0.523 0.096 Uiso 1 1 calc R . . H44B H 0.125 0.9229 0.5838 0.096 Uiso 1 1 calc R . . C442 C 0.0711(3) 0.8715(4) 0.5382(4) 0.117(2) Uani 1 1 d DU . . H44C H 0.0601 0.9114 0.5166 0.14 Uiso 0.5 1 calc PR E 1 H44D H 0.0714 0.8375 0.5047 0.14 Uiso 0.5 1 calc PR E 1 H44E H 0.0493 0.8629 0.5756 0.14 Uiso 0.5 1 d PR E 2 H44F H 0.0697 0.8344 0.5082 0.14 Uiso 0.5 1 d PR E 2 C443 C 0.0347(5) 0.8544(8) 0.5863(7) 0.133(4) Uiso 0.5 1 d PDU F 1 H44G H 0.0272 0.8919 0.6141 0.16 Uiso 0.5 1 calc PR F 1 H44H H 0.0472 0.8195 0.6143 0.16 Uiso 0.5 1 calc PR F 1 C444 C -0.0129(5) 0.8321(10) 0.5497(10) 0.197(9) Uiso 0.5 1 d PDU F 1 H44I H -0.0354 0.8119 0.5806 0.296 Uiso 0.5 1 calc PR F 1 H44J H -0.004 0.8012 0.5158 0.296 Uiso 0.5 1 calc PR F 1 H44K H -0.029 0.8692 0.5297 0.296 Uiso 0.5 1 calc PR F 1 C445 C 0.0538(5) 0.9337(7) 0.5068(9) 0.132(4) Uiso 0.5 1 d PDU F 2 H44L H 0.0516 0.9678 0.54 0.158 Uiso 0.5 1 calc PR F 2 H44M H 0.0776 0.9474 0.4734 0.158 Uiso 0.5 1 calc PR F 2 C446 C 0.0039(5) 0.9232(9) 0.4758(9) 0.186(9) Uiso 0.5 1 d PDU F 2 H44N H -0.0079 0.8802 0.4863 0.279 Uiso 0.5 1 calc PR F 2 H44O H 0.0067 0.9277 0.4285 0.279 Uiso 0.5 1 calc PR F 2 H44P H -0.0193 0.9551 0.4924 0.279 Uiso 0.5 1 calc PR F 2 C45 C 0.2190(2) 0.8777(3) 0.6164(3) 0.0568(15) Uani 1 1 d U . . H45 H 0.2118 0.9112 0.5866 0.068 Uiso 1 1 calc R . . C46 C 0.2650(2) 0.8773(3) 0.6464(3) 0.0585(14) Uani 1 1 d U . . H46 H 0.2876 0.9106 0.637 0.07 Uiso 1 1 calc R . . C47 C 0.2786(2) 0.8296(3) 0.6896(3) 0.0556(15) Uani 1 1 d U . . O47 O 0.32230(16) 0.8237(2) 0.7198(2) 0.0671(14) Uani 1 1 d . . . C471 C 0.3578(2) 0.8709(3) 0.7087(3) 0.0630(19) Uani 1 1 d . H . H47A H 0.3445 0.9132 0.7216 0.076 Uiso 1 1 calc R . . H47B H 0.3656 0.8725 0.6618 0.076 Uiso 1 1 calc R . . C472 C 0.4030(3) 0.8574(4) 0.7463(4) 0.085(2) Uani 1 1 d U . . H47C H 0.3945 0.8567 0.793 0.102 Uiso 0.5 1 calc PR G 1 H47D H 0.4147 0.8141 0.7345 0.102 Uiso 0.5 1 calc PR G 1 H47E H 0.3939 0.8514 0.7924 0.102 Uiso 0.5 1 d PR G 2 H47F H 0.4255 0.8945 0.7439 0.102 Uiso 0.5 1 d PR G 2 C473 C 0.4401(5) 0.8991(7) 0.7376(7) 0.088(3) Uani 0.5 1 d PU H 1 H47G H 0.4655 0.8886 0.7703 0.105 Uiso 0.5 1 calc PR H 1 H47H H 0.4273 0.9421 0.7488 0.105 Uiso 0.5 1 calc PR H 1 C474 C 0.4667(6) 0.9056(8) 0.6712(7) 0.095(4) Uani 0.5 1 d PU H 1 H47I H 0.5023 0.9033 0.678 0.142 Uiso 0.5 1 calc PR H 1 H47J H 0.4583 0.9469 0.6514 0.142 Uiso 0.5 1 calc PR H 1 H47K H 0.4564 0.8708 0.6423 0.142 Uiso 0.5 1 calc PR H 1 C475 C 0.4286(6) 0.8038(8) 0.7265(8) 0.099(3) Uiso 0.5 1 d PU H 2 H47L H 0.4068 0.766 0.7277 0.118 Uiso 0.5 1 calc PR H 2 H47M H 0.4564 0.7961 0.7566 0.118 Uiso 0.5 1 calc PR H 2 C476 C 0.4476(8) 0.8129(10) 0.6595(11) 0.163(8) Uiso 0.5 1 d PU H 2 H47N H 0.4614 0.856 0.6553 0.244 Uiso 0.5 1 calc PR H 2 H47O H 0.4207 0.8075 0.6283 0.244 Uiso 0.5 1 calc PR H 2 H47P H 0.4732 0.7811 0.6508 0.244 Uiso 0.5 1 calc PR H 2 C47A C 0.2426(2) 0.7813(3) 0.6997(3) 0.0534(16) Uani 1 1 d U . . C4 C 0.2823(2) 0.7123(3) 0.7832(3) 0.064(2) Uani 1 1 d . . . H4A H 0.2695 0.6826 0.8159 0.095 Uiso 1 1 calc R . . H4B H 0.2943 0.7511 0.8048 0.095 Uiso 1 1 calc R . . H4C H 0.3093 0.6919 0.7596 0.095 Uiso 1 1 calc R . . C101 C 0.3032(3) 0.6855(3) 0.5869(4) 0.173(5) Uani 1 1 d D . . H101 H 0.2962 0.7275 0.5717 0.207 Uiso 1 1 calc R . . C102 C 0.3461(3) 0.6744(4) 0.6232(4) 0.216(7) Uani 1 1 d D . . H102 H 0.3653 0.7088 0.6394 0.259 Uiso 1 1 calc R . . C103 C 0.3592(3) 0.6119(4) 0.6342(4) 0.154(5) Uani 1 1 d D . . H103 H 0.3905 0.6031 0.6524 0.185 Uiso 1 1 calc R . . C104 C 0.3284(3) 0.5615(4) 0.6200(4) 0.150(4) Uani 1 1 d D . . H104 H 0.3369 0.5191 0.6323 0.18 Uiso 1 1 calc R . . C105 C 0.2843(3) 0.5739(4) 0.5871(4) 0.150(4) Uani 1 1 d D . . H105 H 0.2636 0.5394 0.5744 0.179 Uiso 1 1 calc R . . C106 C 0.2711(3) 0.6360(4) 0.5730(4) 0.150(4) Uani 1 1 d D . . H106 H 0.24 0.6448 0.5539 0.181 Uiso 1 1 calc R . . C201 C 0.2976(3) 0.4369(3) 0.4700(4) 0.119(2) Uani 1 1 d DU . . H201 H 0.2891 0.4808 0.4652 0.143 Uiso 1 1 calc R . . C202 C 0.3440(3) 0.4185(4) 0.4962(4) 0.125(2) Uani 1 1 d DU . . H202 H 0.3673 0.4509 0.5063 0.15 Uiso 1 1 calc R . . C203 C 0.3562(3) 0.3560(3) 0.5072(4) 0.122(2) Uani 1 1 d DU . . H203 H 0.3864 0.3448 0.5274 0.147 Uiso 1 1 calc R . . C204 C 0.3229(3) 0.3097(4) 0.4879(4) 0.117(2) Uani 1 1 d DU . . H204 H 0.3311 0.2658 0.493 0.141 Uiso 1 1 calc R . . C205 C 0.2787(3) 0.3261(3) 0.4617(4) 0.113(2) Uani 1 1 d DU . . H205 H 0.2563 0.2932 0.4499 0.136 Uiso 1 1 calc R . . C206 C 0.2655(3) 0.3893(3) 0.4519(3) 0.111(2) Uani 1 1 d DU . . H206 H 0.2347 0.3997 0.433 0.133 Uiso 1 1 calc R . . C301 C 0.0165(3) 0.6913(4) 0.7736(4) 0.242(8) Uani 1 1 d D . . H301 H 0.0285 0.7304 0.791 0.29 Uiso 1 1 calc R . . C302 C 0.0326(3) 0.6351(4) 0.7962(5) 0.175(6) Uani 1 1 d D . . H302 H 0.0575 0.6361 0.8286 0.209 Uiso 1 1 calc R . . C303 C 0.0163(3) 0.5764(4) 0.7766(4) 0.214(7) Uani 1 1 d D . . H303 H 0.0263 0.538 0.7976 0.257 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 0.0882(3) 0.0355(2) 0.0407(2) 0.0012(2) 0.0081(2) 0.0002(3) Br1 0.1198(6) 0.0420(4) 0.0562(4) 0.0071(3) 0.0161(4) 0.0018(4) Br2 0.1087(6) 0.0454(4) 0.0539(4) -0.0043(3) 0.0159(4) 0.0017(4) C1 0.109(6) 0.055(4) 0.108(6) -0.046(4) -0.038(5) 0.018(4) N21 0.084(4) 0.042(3) 0.063(3) 0.005(3) 0.001(3) 0.003(3) C22 0.070(4) 0.039(3) 0.055(4) 0.012(3) 0.006(3) 0.000(3) N23 0.085(4) 0.033(3) 0.042(3) -0.007(2) 0.003(3) -0.012(3) C23A 0.095(4) 0.031(3) 0.038(3) -0.012(2) 0.013(3) -0.010(3) C24 0.090(3) 0.038(3) 0.056(3) -0.002(2) 0.012(3) -0.008(3) O24 0.096(3) 0.046(2) 0.067(3) -0.007(2) 0.001(2) 0.000(2) C241 0.096(5) 0.064(4) 0.063(4) -0.016(4) -0.013(4) -0.020(4) C242 0.118(4) 0.123(4) 0.109(4) -0.032(4) -0.007(4) -0.023(4) C25 0.074(4) 0.043(3) 0.069(4) -0.030(3) 0.015(3) -0.002(4) C26 0.079(4) 0.034(3) 0.074(4) -0.001(3) 0.029(3) 0.007(4) C27 0.095(5) 0.036(3) 0.040(3) -0.005(3) 0.003(3) 0.000(3) O27 0.099(3) 0.041(2) 0.060(3) -0.002(2) -0.002(3) 0.003(3) C271 0.090(5) 0.044(3) 0.078(4) -0.013(4) 0.021(4) -0.001(4) C272 0.104(4) 0.106(4) 0.087(4) 0.005(4) 0.007(4) 0.026(4) C27A 0.089(5) 0.036(3) 0.051(3) -0.010(3) 0.023(3) -0.017(3) C2 0.078(5) 0.030(3) 0.070(4) -0.004(3) 0.001(4) -0.007(3) C31 0.064(4) 0.054(4) 0.050(3) 0.013(3) 0.000(3) 0.000(3) C32 0.127(6) 0.049(4) 0.052(4) 0.007(3) -0.002(4) -0.009(4) C33 0.113(6) 0.052(4) 0.076(5) -0.010(4) 0.009(5) -0.028(4) C34 0.165(8) 0.053(4) 0.072(5) -0.028(4) 0.027(5) -0.010(5) C35 0.140(7) 0.061(4) 0.030(3) -0.012(3) -0.008(4) -0.004(5) C36 0.173(8) 0.046(4) 0.055(4) 0.000(3) -0.005(5) -0.013(5) C3 0.069(4) 0.075(5) 0.035(3) -0.006(3) -0.002(3) -0.001(4) N41 0.060(3) 0.044(3) 0.050(3) 0.003(2) 0.016(3) 0.010(2) C42 0.078(5) 0.061(4) 0.041(3) -0.015(3) 0.014(3) 0.010(4) N43 0.068(3) 0.043(3) 0.032(2) 0.008(2) -0.002(2) 0.000(3) C43A 0.092(5) 0.032(3) 0.037(3) 0.001(3) 0.006(3) 0.008(3) C44 0.092(5) 0.045(4) 0.044(3) 0.004(3) 0.007(3) 0.004(4) O44 0.088(3) 0.047(2) 0.057(3) 0.002(2) -0.005(3) 0.007(2) C441 0.092(5) 0.070(4) 0.077(4) 0.040(4) 0.000(4) 0.007(5) C442 0.110(4) 0.127(4) 0.113(4) 0.029(4) 0.001(4) 0.015(4) C45 0.076(3) 0.039(3) 0.055(3) -0.003(3) 0.008(3) 0.007(3) C46 0.078(3) 0.037(2) 0.060(3) -0.001(3) 0.015(3) -0.003(3) C47 0.078(3) 0.038(3) 0.051(3) 0.009(2) 0.008(3) 0.000(3) O47 0.081(3) 0.052(3) 0.069(3) 0.011(2) 0.003(3) 0.000(3) C471 0.063(4) 0.070(4) 0.056(3) -0.018(4) 0.006(3) -0.018(4) C472 0.085(4) 0.103(4) 0.067(3) -0.011(3) 0.012(3) -0.005(3) C473 0.087(6) 0.100(6) 0.076(5) -0.021(5) 0.012(5) -0.007(5) C474 0.085(8) 0.106(9) 0.092(7) -0.008(8) 0.016(6) -0.018(8) C47A 0.079(4) 0.040(3) 0.041(3) 0.003(2) 0.005(3) -0.001(3) C4 0.068(5) 0.063(4) 0.059(4) 0.004(3) -0.005(4) -0.002(4) C101 0.294(13) 0.050(5) 0.175(9) -0.049(5) 0.124(9) -0.042(7) C102 0.073(6) 0.52(2) 0.059(5) 0.083(9) 0.022(5) 0.059(10) C103 0.154(9) 0.235(14) 0.073(6) 0.039(7) -0.047(6) 0.021(9) C104 0.211(9) 0.139(7) 0.101(7) -0.051(5) 0.053(7) -0.123(7) C105 0.211(10) 0.130(8) 0.108(8) -0.019(7) 0.048(7) -0.097(8) C106 0.150(8) 0.199(12) 0.102(6) 0.016(8) 0.079(6) 0.038(8) C201 0.187(4) 0.097(4) 0.073(4) 0.026(4) 0.017(4) -0.003(3) C202 0.178(4) 0.120(4) 0.078(4) -0.004(4) 0.006(4) -0.034(4) C203 0.163(4) 0.130(4) 0.074(4) -0.009(4) -0.007(4) 0.003(4) C204 0.166(4) 0.110(4) 0.076(4) -0.006(4) 0.009(4) 0.009(3) C205 0.163(4) 0.114(4) 0.063(4) 0.007(4) 0.006(4) -0.013(4) C206 0.161(4) 0.120(4) 0.052(3) 0.021(4) 0.004(4) 0.000(4) C301 0.171(12) 0.412(19) 0.142(13) -0.027(14) 0.077(9) 0.028(14) C302 0.115(8) 0.291(16) 0.117(9) 0.019(11) -0.007(7) -0.056(10) C303 0.206(13) 0.238(13) 0.199(16) 0.043(12) 0.109(11) 0.014(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C22 2.010(6) . ? Pd1 C42 2.054(6) . ? Pd1 Br2 2.4712(8) . ? Pd1 Br1 2.4719(8) . ? C1 N21 1.454(8) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? N21 C22 1.355(8) . ? N21 C27A 1.444(7) . ? C22 N23 1.352(8) . ? N23 C23A 1.409(7) . ? N23 C2 1.455(8) . ? C23A C27A 1.398(9) . ? C23A C24 1.410(8) . ? C24 O24 1.370(8) . ? C24 C25 1.383(8) . ? O24 C241 1.420(7) . ? C241 C242 1.524(9) . ? C241 H24A 0.99 . ? C241 H24B 0.99 . ? C242 C245 1.442(13) . ? C242 C243 1.531(12) . ? C242 H24C 0.99 . ? C242 H24D 0.99 . ? C242 H24E 0.99 . ? C242 H24F 0.99 . ? C243 C244 1.570(14) . ? C243 H24G 0.99 . ? C243 H24H 0.99 . ? C244 H24I 0.98 . ? C244 H24J 0.98 . ? C244 H24K 0.98 . ? C245 C246 1.486(14) . ? C245 H24L 0.99 . ? C245 H24M 0.99 . ? C246 H24N 0.98 . ? C246 H24O 0.98 . ? C246 H24P 0.98 . ? C25 C26 1.375(9) . ? C25 H25 0.95 . ? C26 C27 1.376(8) . ? C26 H26 0.95 . ? C27 O27 1.361(8) . ? C27 C27A 1.401(8) . ? O27 C271 1.462(7) . ? C271 C272 1.539(9) . ? C271 H27A 0.99 . ? C271 H27B 0.99 . ? C272 C273 1.474(12) . ? C272 C275 1.508(13) . ? C272 H27C 0.99 . ? C272 H27D 0.99 . ? C272 H27E 0.99 . ? C272 H27F 0.99 . ? C273 C274 1.443(14) . ? C273 H27G 0.99 . ? C273 H27H 0.99 . ? C274 H27I 0.98 . ? C274 H27J 0.98 . ? C274 H27K 0.98 . ? C275 C276 1.539(14) . ? C275 H27L 0.99 . ? C275 H27M 0.99 . ? C276 H27N 0.98 . ? C276 H27O 0.98 . ? C276 H27P 0.98 . ? C2 C32 1.513(9) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C31 C32 1.411(8) . ? C31 C36 1.445(9) . ? C31 C3 1.528(8) . ? C32 C33 1.360(9) . ? C33 C34 1.379(10) . ? C33 H33 0.95 . ? C34 C35 1.373(9) . ? C34 H34 0.95 . ? C35 C36 1.390(9) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C3 N43 1.461(8) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? N41 C42 1.303(8) . ? N41 C47A 1.337(7) . ? N41 C4 1.465(7) . ? C42 N43 1.356(8) . ? N43 C43A 1.404(7) . ? C43A C47A 1.371(9) . ? C43A C44 1.415(8) . ? C44 O44 1.376(8) . ? C44 C45 1.375(8) . ? O44 C441 1.385(7) . ? C441 C442 1.490(10) . ? C441 H44A 0.99 . ? C441 H44B 0.99 . ? C442 C443 1.448(13) . ? C442 C445 1.524(13) . ? C442 H44C 0.99 . ? C442 H44D 0.99 . ? C442 H44E 0.99 . ? C442 H44F 0.99 . ? C443 C444 1.568(15) . ? C443 H44G 0.99 . ? C443 H44H 0.99 . ? C444 H44I 0.98 . ? C444 H44J 0.98 . ? C444 H44K 0.98 . ? C445 C446 1.515(14) . ? C445 H44L 0.99 . ? C445 H44M 0.99 . ? C446 H44N 0.98 . ? C446 H44O 0.98 . ? C446 H44P 0.98 . ? C45 C46 1.397(8) . ? C45 H45 0.95 . ? C46 C47 1.385(8) . ? C46 H46 0.95 . ? C47 O47 1.347(7) . ? C47 C47A 1.424(8) . ? O47 C471 1.400(7) . ? C471 C472 1.479(9) . ? C471 H47A 0.99 . ? C471 H47B 0.99 . ? C472 C473 1.347(16) . ? C472 C475 1.381(16) . ? C472 H47C 0.99 . ? C472 H47D 0.99 . ? C472 H47E 0.99 . ? C472 H47F 0.99 . ? C473 C474 1.55(2) . ? C473 H47G 0.99 . ? C473 H47H 0.99 . ? C474 H47I 0.98 . ? C474 H47J 0.98 . ? C474 H47K 0.98 . ? C475 C476 1.48(3) . ? C475 H47L 0.99 . ? C475 H47M 0.99 . ? C476 H47N 0.98 . ? C476 H47O 0.98 . ? C476 H47P 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C101 C106 1.385(9) . ? C101 C102 1.404(10) . ? C101 H101 0.95 . ? C102 C103 1.371(10) . ? C102 H102 0.95 . ? C103 C104 1.378(9) . ? C103 H103 0.95 . ? C104 C105 1.401(10) . ? C104 H104 0.95 . ? C105 C106 1.377(10) . ? C105 H105 0.95 . ? C106 H106 0.95 . ? C201 C206 1.374(9) . ? C201 C202 1.426(9) . ? C201 H201 0.95 . ? C202 C203 1.365(9) . ? C202 H202 0.95 . ? C203 C204 1.382(9) . ? C203 H203 0.95 . ? C204 C205 1.362(9) . ? C204 H204 0.95 . ? C205 C206 1.383(9) . ? C205 H205 0.95 . ? C206 H206 0.95 . ? C301 C301 1.320(14) 2_556 ? C301 C302 1.337(11) . ? C301 H301 0.95 . ? C302 C303 1.365(10) . ? C302 H302 0.95 . ? C303 C303 1.408(13) 2_556 ? C303 H303 0.95 . ? 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 C22 Pd1 C42 95.1(2) . . ? C22 Pd1 Br2 178.55(17) . . ? C42 Pd1 Br2 86.16(16) . . ? C22 Pd1 Br1 86.09(16) . . ? C42 Pd1 Br1 178.24(18) . . ? Br2 Pd1 Br1 92.60(3) . . ? N21 C1 H1A 109.5 . . ? N21 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N21 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C22 N21 C27A 105.6(5) . . ? C22 N21 C1 128.6(5) . . ? C27A N21 C1 125.7(5) . . ? N21 C22 N23 111.8(5) . . ? N21 C22 Pd1 121.5(5) . . ? N23 C22 Pd1 125.8(5) . . ? C22 N23 C23A 108.2(5) . . ? C22 N23 C2 123.6(5) . . ? C23A N23 C2 128.1(5) . . ? C27A C23A C24 121.3(6) . . ? C27A C23A N23 106.5(5) . . ? C24 C23A N23 132.1(6) . . ? O24 C24 C25 126.3(6) . . ? O24 C24 C23A 118.2(6) . . ? C25 C24 C23A 115.1(6) . . ? C24 O24 C241 118.6(5) . . ? O24 C241 C242 106.4(5) . . ? O24 C241 H24A 110.5 . . ? C242 C241 H24A 110.4 . . ? O24 C241 H24B 110.5 . . ? C242 C241 H24B 110.5 . . ? H24A C241 H24B 108.6 . . ? C245 C242 C241 125.9(8) . . ? C241 C242 C243 107.1(7) . . ? C241 C242 H24C 110.3 . . ? C243 C242 H24C 110.3 . . ? C241 C242 H24D 110.3 . . ? C243 C242 H24D 110.3 . . ? H24C C242 H24D 108.6 . . ? C245 C242 H24E 104.6 . . ? C241 C242 H24E 100.8 . . ? C245 C242 H24F 115 . . ? C241 C242 H24F 103.1 . . ? H24E C242 H24F 104.7 . . ? C242 C243 C244 111.7(11) . . ? C242 C243 H24G 109.3 . . ? C244 C243 H24G 109.3 . . ? C242 C243 H24H 109.3 . . ? C244 C243 H24H 109.3 . . ? H24G C243 H24H 107.9 . . ? C242 C245 C246 114.4(12) . . ? C242 C245 H24L 108.7 . . ? C246 C245 H24L 108.6 . . ? C242 C245 H24M 108.7 . . ? C246 C245 H24M 108.7 . . ? C245 C246 H24N 109.5 . . ? C245 C246 H24O 109.5 . . ? H24N C246 H24O 109.5 . . ? C245 C246 H24P 109.5 . . ? H24N C246 H24P 109.5 . . ? H24O C246 H24P 109.5 . . ? C26 C25 C24 124.3(6) . . ? C26 C25 H25 117.8 . . ? C24 C25 H25 117.8 . . ? C27 C26 C25 120.4(6) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? O27 C27 C26 125.6(6) . . ? O27 C27 C27A 116.6(5) . . ? C26 C27 C27A 117.8(6) . . ? C27 O27 C271 117.8(5) . . ? O27 C271 C272 107.5(5) . . ? O27 C271 H27A 110.2 . . ? C272 C271 H27A 110.2 . . ? O27 C271 H27B 110.2 . . ? C272 C271 H27B 110.2 . . ? H27A C271 H27B 108.5 . . ? C273 C272 C275 104.1(10) . . ? C273 C272 C271 118.3(8) . . ? C275 C272 C271 117.6(8) . . ? C273 C272 H27C 107.7 . . ? C271 C272 H27C 107.7 . . ? C273 C272 H27D 107.7 . . ? C271 C272 H27D 107.7 . . ? H27C C272 H27D 107.1 . . ? C275 C272 H27E 105.2 . . ? C271 C272 H27E 108.5 . . ? C275 C272 H27F 107.2 . . ? C271 C272 H27F 109.9 . . ? H27E C272 H27F 108.1 . . ? C274 C273 C272 116.1(11) . . ? C274 C273 H27G 108.3 . . ? C272 C273 H27G 108.2 . . ? C274 C273 H27H 108.2 . . ? C272 C273 H27H 108.3 . . ? H27G C273 H27H 107.4 . . ? C272 C275 C276 106.5(11) . . ? C272 C275 H27L 110.4 . . ? C276 C275 H27L 110.4 . . ? C272 C275 H27M 110.4 . . ? C276 C275 H27M 110.5 . . ? H27L C275 H27M 108.6 . . ? C275 C276 H27N 109.5 . . ? C275 C276 H27O 109.5 . . ? H27N C276 H27O 109.5 . . ? C275 C276 H27P 109.5 . . ? H27N C276 H27P 109.5 . . ? H27O C276 H27P 109.5 . . ? C23A C27A C27 120.9(5) . . ? C23A C27A N21 107.8(5) . . ? C27 C27A N21 131.2(6) . . ? N23 C2 C32 109.5(5) . . ? N23 C2 H2A 109.8 . . ? C32 C2 H2A 109.8 . . ? N23 C2 H2B 109.8 . . ? C32 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? C32 C31 C36 120.3(6) . . ? C32 C31 C3 123.8(6) . . ? C36 C31 C3 115.4(5) . . ? C33 C32 C31 116.6(6) . . ? C33 C32 C2 118.0(6) . . ? C31 C32 C2 125.2(6) . . ? C32 C33 C34 126.0(7) . . ? C32 C33 H33 117 . . ? C34 C33 H33 117 . . ? C35 C34 C33 116.2(7) . . ? C35 C34 H34 121.9 . . ? C33 C34 H34 121.9 . . ? C34 C35 C36 123.5(6) . . ? C34 C35 H35 118.3 . . ? C36 C35 H35 118.3 . . ? C35 C36 C31 116.8(6) . . ? C35 C36 H36 121.6 . . ? C31 C36 H36 121.6 . . ? N43 C3 C31 115.1(5) . . ? N43 C3 H3A 108.5 . . ? C31 C3 H3A 108.5 . . ? N43 C3 H3B 108.5 . . ? C31 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C42 N41 C47A 110.9(5) . . ? C42 N41 C4 123.8(5) . . ? C47A N41 C4 125.2(5) . . ? N41 C42 N43 109.8(5) . . ? N41 C42 Pd1 126.1(5) . . ? N43 C42 Pd1 122.5(5) . . ? C42 N43 C43A 105.2(5) . . ? C42 N43 C3 124.9(5) . . ? C43A N43 C3 129.4(5) . . ? C47A C43A N43 107.7(5) . . ? C47A C43A C44 121.9(6) . . ? N43 C43A C44 130.1(6) . . ? O44 C44 C45 126.2(5) . . ? O44 C44 C43A 119.0(6) . . ? C45 C44 C43A 114.7(6) . . ? C44 O44 C441 119.1(5) . . ? O44 C441 C442 110.5(6) . . ? O44 C441 H44A 109.5 . . ? C442 C441 H44A 109.5 . . ? O44 C441 H44B 109.5 . . ? C442 C441 H44B 109.6 . . ? H44A C441 H44B 108.1 . . ? C443 C442 C441 117.6(8) . . ? C443 C442 C445 106.7(10) . . ? C441 C442 C445 107.8(7) . . ? C443 C442 H44C 107.9 . . ? C441 C442 H44C 107.9 . . ? C443 C442 H44D 107.9 . . ? C441 C442 H44D 107.9 . . ? C445 C442 H44D 108.6 . . ? H44C C442 H44D 107.2 . . ? C441 C442 H44E 110.1 . . ? C445 C442 H44E 107.4 . . ? C441 C442 H44F 109.7 . . ? C445 C442 H44F 113 . . ? H44E C442 H44F 108.8 . . ? C442 C443 C444 108.1(11) . . ? C442 C443 H44G 110.1 . . ? C444 C443 H44G 110.1 . . ? C442 C443 H44H 110.1 . . ? C444 C443 H44H 110.1 . . ? H44E C443 H44H 104.2 . . ? H44G C443 H44H 108.4 . . ? C446 C445 C442 109.4(11) . . ? C446 C445 H44L 109.8 . . ? C442 C445 H44L 109.8 . . ? C446 C445 H44M 109.8 . . ? C442 C445 H44M 109.8 . . ? H44L C445 H44M 108.2 . . ? C445 C446 H44N 109.5 . . ? C445 C446 H44O 109.5 . . ? H44N C446 H44O 109.5 . . ? C445 C446 H44P 109.5 . . ? H44N C446 H44P 109.5 . . ? H44O C446 H44P 109.5 . . ? C44 C45 C46 123.6(6) . . ? C44 C45 H45 118.2 . . ? C46 C45 H45 118.2 . . ? C47 C46 C45 121.9(6) . . ? C47 C46 H46 119.1 . . ? C45 C46 H46 119.1 . . ? O47 C47 C46 126.7(6) . . ? O47 C47 C47A 118.4(5) . . ? C46 C47 C47A 114.8(6) . . ? C47 O47 C471 118.0(5) . . ? O47 C471 C472 110.8(6) . . ? O47 C471 H47A 109.5 . . ? C472 C471 H47A 109.5 . . ? O47 C471 H47B 109.5 . . ? C472 C471 H47B 109.5 . . ? H47A C471 H47B 108.1 . . ? C473 C472 C471 115.6(9) . . ? C475 C472 C471 114.9(9) . . ? C473 C472 H47C 108.4 . . ? C471 C472 H47C 108.4 . . ? C473 C472 H47D 108.4 . . ? C471 C472 H47D 108.4 . . ? H47C C472 H47D 107.4 . . ? C475 C472 H47E 107.9 . . ? C471 C472 H47E 108.4 . . ? C475 C472 H47F 107.8 . . ? C471 C472 H47F 109.9 . . ? H47E C472 H47F 107.6 . . ? C472 C473 C474 121.7(13) . . ? C472 C473 H47G 106.9 . . ? C474 C473 H47G 106.9 . . ? H47F C473 H47G 112.9 . . ? C472 C473 H47H 106.9 . . ? C474 C473 H47H 106.9 . . ? H47G C473 H47H 106.7 . . ? C472 C475 C476 110.3(15) . . ? C472 C475 H47L 109.6 . . ? C476 C475 H47L 109.6 . . ? C472 C475 H47M 109.6 . . ? C476 C475 H47M 109.6 . . ? H47L C475 H47M 108.1 . . ? C475 C476 H47N 109.5 . . ? C475 C476 H47O 109.5 . . ? H47N C476 H47O 109.5 . . ? C475 C476 H47P 109.5 . . ? H47N C476 H47P 109.5 . . ? H47O C476 H47P 109.5 . . ? N41 C47A C43A 106.4(5) . . ? N41 C47A C47 131.0(6) . . ? C43A C47A C47 122.6(5) . . ? N41 C4 H4A 109.5 . . ? N41 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N41 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C106 C101 C102 120.7(7) . . ? C106 C101 H101 119.7 . . ? C102 C101 H101 119.7 . . ? C103 C102 C101 117.5(7) . . ? C103 C102 H102 121.3 . . ? C101 C102 H102 121.2 . . ? C102 C103 C104 122.3(7) . . ? C102 C103 H103 118.9 . . ? C104 C103 H103 118.9 . . ? C103 C104 C105 118.9(7) . . ? C103 C104 H104 120.5 . . ? C105 C104 H104 120.6 . . ? C106 C105 C104 119.9(7) . . ? C106 C105 H105 120.1 . . ? C104 C105 H105 120.1 . . ? C105 C106 C101 119.7(7) . . ? C105 C106 H106 120.1 . . ? C101 C106 H106 120.1 . . ? C206 C201 C202 118.1(7) . . ? C206 C201 H201 120.9 . . ? C202 C201 H201 121 . . ? C203 C202 C201 122.3(7) . . ? C203 C202 H202 118.9 . . ? C201 C202 H202 118.8 . . ? C202 C203 C204 117.6(7) . . ? C202 C203 H203 121.2 . . ? C204 C203 H203 121.2 . . ? C205 C204 C203 121.0(7) . . ? C205 C204 H204 119.5 . . ? C203 C204 H204 119.5 . . ? C204 C205 C206 121.8(7) . . ? C204 C205 H205 119.1 . . ? C206 C205 H205 119.1 . . ? C201 C206 C205 119.1(7) . . ? C201 C206 H206 120.5 . . ? C205 C206 H206 120.5 . . ? C301 C301 C302 118.5(5) 2_556 . ? C301 C301 H301 120.7 2_556 . ? C302 C301 H301 120.7 . . ? C301 C302 C303 125.5(9) . . ? C301 C302 H302 117.3 . . ? C303 C302 H302 117.3 . . ? C302 C303 C303 115.7(5) . 2_556 ? C302 C303 H303 122.2 . . ? C303 C303 H303 122.2 2_556 . ? 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 0.464 0.004 0.059 19 0 ' ' 2 0.964 0.504 0.059 19 0 ' ' 3 0.000 0.864 0.250 319 70 ' ' 4 0.500 0.364 0.250 319 70 ' ' 5 0.036 0.494 0.113 7 1 ' ' 6 0.536 0.994 0.113 7 1 ' ' 7 0.470 -0.005 0.393 8 0 ' ' 8 0.970 0.495 0.393 8 0 ' ' 9 0.042 0.505 0.443 18 -1 ' ' 10 0.542 1.005 0.443 18 -1 ' ' 11 0.463 0.996 0.560 18 -1 ' ' 12 0.963 0.496 0.560 18 -1 ' ' 13 0.000 0.136 0.750 319 72 ' ' 14 0.500 0.636 0.750 319 72 ' ' 15 0.036 0.506 0.613 8 0 ' ' 16 0.536 0.006 0.613 8 0 ' ' 17 0.470 0.005 0.893 8 0 ' ' 18 0.970 0.505 0.893 8 0 ' ' 19 0.042 0.495 0.943 18 -1 ' ' 20 0.542 -0.005 0.943 18 -1 ' ' _platon_squeeze_details ; ; #===END data_ps97x _database_code_depnum_ccdc_archive 'CCDC 726630' _audit_creation_date 2009-07-14T11:19:39-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C45 H67 Br2 Cl3 N4 O6 Pd S2' _chemical_formula_moiety 'C40 H54 Br2 N4 O4 Pd,2(C2 H6 O S), C H Cl3' _chemical_formula_weight 1196.72 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall -P_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1456(7) _cell_length_b 14.5636(6) _cell_length_c 16.8254(10) _cell_angle_alpha 68.016(4) _cell_angle_beta 86.629(5) _cell_angle_gamma 72.488(4) _cell_volume 2627.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9271 _cell_measurement_theta_min 2.8355 _cell_measurement_theta_max 66.9245 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2621 _exptl_crystal_size_mid 0.0469 _exptl_crystal_size_min 0.0205 _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.162 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.444 _exptl_absorpt_correction_T_max 0.872 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 0.0347610204 _diffrn_orient_matrix_ub_12 -0.1177943373 _diffrn_orient_matrix_ub_13 0.0526028659 _diffrn_orient_matrix_ub_21 0.0247013914 _diffrn_orient_matrix_ub_22 -0.0208355232 _diffrn_orient_matrix_ub_23 -0.0833653923 _diffrn_orient_matrix_ub_31 0.126322923 _diffrn_orient_matrix_ub_32 -0.0012851917 _diffrn_orient_matrix_ub_33 0.0084520724 _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_unetI/netI 0.0516 _diffrn_reflns_number 32223 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 67.23 _diffrn_reflns_theta_full 67.23 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type ; Oxford Diffraction Gemini diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 9288 _reflns_number_gt 6622 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution Sir92 _computing_molecular_graphics ORTEP2 _computing_publication_material WinGX _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.1245P)^2^+0.3208P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 9288 _refine_ls_number_parameters 676 _refine_ls_number_restraints 244 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.063 _refine_ls_wR_factor_ref 0.1862 _refine_ls_wR_factor_gt 0.1687 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.539 _refine_diff_density_min -0.843 _refine_diff_density_rms 0.127 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.605325(14) 0.522563(12) 0.330282(11) 0.03746(5) Uani 1 1 d U . . Br1 Br 0.39902(2) 0.60431(2) 0.280051(19) 0.05031(8) Uani 1 1 d U . . Br2 Br 0.63250(2) 0.686496(19) 0.323323(19) 0.05055(8) Uani 1 1 d U . . C11 C 0.6600(4) 0.2387(3) 0.5265(3) 0.0587(13) Uani 0.5 1 d PDU A 1 C12 C 0.7549(4) 0.2693(3) 0.5432(3) 0.0563(13) Uani 0.5 1 d PDU A 1 C13 C 0.8603(5) 0.1880(4) 0.5798(3) 0.0621(13) Uani 0.5 1 d PDU A 1 H13 H 0.9233 0.2062 0.5939 0.074 Uiso 0.5 1 calc PR A 1 C14 C 0.8759(5) 0.0835(4) 0.5957(4) 0.0649(14) Uani 0.5 1 d PDU A 1 H14 H 0.949 0.0329 0.6161 0.078 Uiso 0.5 1 calc PR A 1 C15 C 0.7800(4) 0.0554(4) 0.5805(4) 0.0681(14) Uani 0.5 1 d PDU A 1 H15 H 0.7869 -0.0152 0.5923 0.082 Uiso 0.5 1 calc PR A 1 C16 C 0.6775(4) 0.1307(3) 0.5488(4) 0.0628(13) Uani 0.5 1 d PDU A 1 H16 H 0.6134 0.1097 0.541 0.075 Uiso 0.5 1 calc PR A 1 C1 C 0.5425(4) 0.3153(4) 0.4868(3) 0.0478(15) Uani 0.5 1 d PD A 1 H1A H 0.5348 0.3831 0.4908 0.057 Uiso 0.5 1 calc PR A 1 H1B H 0.48 0.2889 0.5182 0.057 Uiso 0.5 1 calc PR A 1 C1' C 0.5014(5) 0.3376(4) 0.4742(3) 0.0406(15) Uani 0.5 1 d P A 2 H1'A H 0.5182 0.3982 0.4766 0.061 Uiso 0.5 1 calc PR A 2 H1'B H 0.5461 0.2748 0.5208 0.061 Uiso 0.5 1 calc PR A 2 H1'C H 0.4186 0.3458 0.4804 0.061 Uiso 0.5 1 calc PR A 2 N21 N 0.53255(16) 0.32870(14) 0.39287(13) 0.0385(6) Uani 1 1 d U . . C22 C 0.57799(19) 0.39341(17) 0.33069(16) 0.0398(4) Uani 1 1 d U A . N23 N 0.57524(17) 0.37287(14) 0.25893(13) 0.0412(6) Uani 1 1 d U . . C23A C 0.5233(2) 0.29511(17) 0.27490(17) 0.0427(6) Uani 1 1 d U A . C24 C 0.4901(2) 0.25420(18) 0.22075(17) 0.0464(7) Uani 1 1 d U . . O24 O 0.51357(16) 0.29202(14) 0.13631(12) 0.0552(6) Uani 1 1 d U A . C241 C 0.4790(3) 0.2510(2) 0.07954(18) 0.0612(8) Uani 1 1 d U . . H24A H 0.395 0.2596 0.0817 0.073 Uiso 1 1 calc R A . H24B H 0.521 0.1761 0.0971 0.073 Uiso 1 1 calc R . . C242 C 0.5072(3) 0.3098(3) -0.0102(2) 0.0818(10) Uani 1 1 d U A . H24C H 0.4598 0.3834 -0.0277 0.098 Uiso 1 1 calc R . . H24D H 0.4839 0.2818 -0.0497 0.098 Uiso 1 1 calc R . . C243 C 0.6341(4) 0.3059(4) -0.0221(3) 0.1019(13) Uani 1 1 d U . . H24E H 0.6413 0.3518 -0.0816 0.122 Uiso 1 1 calc R A . H24F H 0.6579 0.3337 0.0172 0.122 Uiso 1 1 calc R . . C244 C 0.7139(5) 0.2013(5) -0.0061(4) 0.145(2) Uani 1 1 d U A . H24G H 0.7272 0.1619 0.056 0.217 Uiso 1 1 calc R . . H24H H 0.7876 0.2069 -0.0311 0.217 Uiso 1 1 calc R . . H24I H 0.6801 0.1654 -0.0323 0.217 Uiso 1 1 calc R . . C25 C 0.4309(2) 0.18099(18) 0.25757(18) 0.0478(7) Uani 1 1 d U A . H25 H 0.4063 0.1515 0.2227 0.057 Uiso 1 1 calc R . . C26 C 0.4065(2) 0.14956(18) 0.34517(18) 0.0468(7) Uani 1 1 d U . . H26 H 0.3676 0.0984 0.3681 0.056 Uiso 1 1 calc R A . C27 C 0.4384(2) 0.19183(17) 0.39840(17) 0.0432(7) Uani 1 1 d U A . O27 O 0.41968(14) 0.16756(12) 0.48272(11) 0.0465(5) Uani 1 1 d U . . C271 C 0.3516(2) 0.09718(18) 0.52150(19) 0.0503(8) Uani 1 1 d . A . H27A H 0.3878 0.0297 0.5153 0.06 Uiso 1 1 calc R . . H27B H 0.2723 0.1272 0.494 0.06 Uiso 1 1 calc R . . C272 C 0.3488(2) 0.08327(19) 0.61448(19) 0.0526(9) Uani 1 1 d . . . H27C H 0.3171 0.1524 0.6185 0.063 Uiso 1 1 calc R A . H27D H 0.429 0.0531 0.6402 0.063 Uiso 1 1 calc R . . C273 C 0.2771(3) 0.0140(2) 0.6670(2) 0.0703(12) Uani 1 1 d . A . H27E H 0.1958 0.0455 0.6435 0.084 Uiso 1 1 calc R . . H27F H 0.3067 -0.0545 0.6618 0.084 Uiso 1 1 calc R . . C274 C 0.2813(3) -0.0009(3) 0.7608(3) 0.0907(16) Uani 1 1 d . . . H27G H 0.3621 -0.0268 0.7831 0.136 Uiso 1 1 calc R A . H27H H 0.2409 -0.0512 0.7931 0.136 Uiso 1 1 calc R . . H27I H 0.2436 0.0656 0.7668 0.136 Uiso 1 1 calc R . . C27A C 0.4973(2) 0.26674(17) 0.36003(16) 0.0406(7) Uani 1 1 d . A . C2' C 0.6479(3) 0.4137(3) 0.1840(3) 0.0331(12) Uani 0.5 1 d PD A 2 H2'A H 0.6134 0.418 0.1303 0.04 Uiso 0.5 1 calc PR A 2 H2'B H 0.6468 0.4845 0.1771 0.04 Uiso 0.5 1 calc PR A 2 C2 C 0.6040(5) 0.4276(5) 0.1762(4) 0.059(2) Uani 0.5 1 d P A 1 H2A H 0.6076 0.4953 0.1728 0.071 Uiso 0.5 1 calc PR A 1 H2B H 0.545 0.4379 0.1338 0.071 Uiso 0.5 1 calc PR A 1 H2C H 0.6794 0.3879 0.1643 0.071 Uiso 0.5 1 calc PR A 1 C31 C 0.8631(3) 0.3721(3) 0.2184(2) 0.0313(12) Uani 0.5 1 d PD A 2 C32 C 0.7705(3) 0.3448(2) 0.1982(2) 0.0289(11) Uani 0.5 1 d PD A 2 C33 C 0.7911(4) 0.2498(3) 0.1873(3) 0.0389(13) Uani 0.5 1 d PD A 2 H33 H 0.7284 0.2314 0.173 0.047 Uiso 0.5 1 calc PR A 2 C34 C 0.9020(3) 0.1839(3) 0.1973(3) 0.0398(14) Uani 0.5 1 d PD A 2 H34 H 0.9147 0.1187 0.1922 0.048 Uiso 0.5 1 calc PR A 2 C35 C 0.9944(4) 0.2105(3) 0.2146(3) 0.0469(16) Uani 0.5 1 d PD A 2 H35 H 1.0709 0.1664 0.2172 0.056 Uiso 0.5 1 calc PR A 2 C36 C 0.9755(4) 0.3036(3) 0.2286(3) 0.0372(13) Uani 0.5 1 d PD A 2 H36 H 1.0387 0.3199 0.2449 0.045 Uiso 0.5 1 calc PR A 2 C3' C 0.8509(4) 0.4686(3) 0.2347(3) 0.0392(15) Uani 0.5 1 d PD A 2 H3'A H 0.9093 0.5004 0.202 0.047 Uiso 0.5 1 calc PR A 2 H3'B H 0.7739 0.5178 0.21 0.047 Uiso 0.5 1 calc PR A 2 C3 C 0.8512(4) 0.5069(5) 0.2229(3) 0.0528(19) Uani 0.5 1 d P A 1 H3A H 0.8954 0.4545 0.2004 0.063 Uiso 0.5 1 calc PR A 1 H3B H 0.8814 0.5665 0.2023 0.063 Uiso 0.5 1 calc PR A 1 H3C H 0.7696 0.5297 0.2032 0.063 Uiso 0.5 1 calc PR A 1 N41 N 0.86216(16) 0.46044(15) 0.32027(13) 0.0399(6) Uani 1 1 d U . . C42 C 0.77204(19) 0.45857(17) 0.37039(15) 0.0393(4) Uani 1 1 d U A . N43 N 0.81383(16) 0.42287(15) 0.45302(13) 0.0428(6) Uani 1 1 d U . . C43A C 0.93480(19) 0.40194(17) 0.45483(16) 0.0402(7) Uani 1 1 d . A . C44 C 1.0164(2) 0.36693(17) 0.52349(17) 0.0448(7) Uani 1 1 d . . . O44 O 0.97605(15) 0.34687(13) 0.60318(11) 0.0487(6) Uani 1 1 d . A . C441 C 1.0593(2) 0.3026(2) 0.67595(18) 0.0563(9) Uani 1 1 d . . . H44A H 1.1041 0.3508 0.6716 0.068 Uiso 1 1 calc R A . H44B H 1.1139 0.2362 0.6768 0.068 Uiso 1 1 calc R . . C442 C 0.9957(3) 0.2846(3) 0.7557(2) 0.0687(11) Uani 1 1 d . A . H44C H 0.9442 0.3527 0.7538 0.082 Uiso 1 1 calc R . . H44D H 1.0528 0.2575 0.8049 0.082 Uiso 1 1 calc R . . C443 C 0.9245(4) 0.2126(3) 0.7735(3) 0.0891(16) Uani 1 1 d . . . H44E H 0.8814 0.215 0.8249 0.107 Uiso 1 1 calc R A . H44F H 0.8665 0.2409 0.7247 0.107 Uiso 1 1 calc R . . C444 C 0.9825(5) 0.1016(4) 0.7880(5) 0.155(3) Uani 1 1 d . A . H44G H 1.015 0.0959 0.7347 0.233 Uiso 1 1 calc R . . H44H H 0.9261 0.0628 0.8059 0.233 Uiso 1 1 calc R . . H44I H 1.0448 0.0727 0.8331 0.233 Uiso 1 1 calc R . . C45 C 1.1294(2) 0.35762(17) 0.50187(17) 0.0462(8) Uani 1 1 d . A . H45 H 1.1881 0.3331 0.5462 0.055 Uiso 1 1 calc R . . C46 C 1.1600(2) 0.38291(18) 0.41727(18) 0.0465(8) Uani 1 1 d . . . H46 H 1.2392 0.375 0.4059 0.056 Uiso 1 1 calc R A . C47 C 1.0807(2) 0.41888(18) 0.34927(17) 0.0437(7) Uani 1 1 d . A . O47 O 1.10050(13) 0.44926(13) 0.26451(12) 0.0481(6) Uani 1 1 d . . . C471 C 1.2194(2) 0.4384(2) 0.2428(2) 0.0547(9) Uani 1 1 d . A . H47A H 1.2659 0.3643 0.2658 0.066 Uiso 1 1 calc R . . H47B H 1.2529 0.4765 0.2677 0.066 Uiso 1 1 calc R . . C472 C 1.2200(3) 0.4824(3) 0.1464(2) 0.0734(13) Uani 1 1 d . . . H47C H 1.1763 0.5572 0.126 0.088 Uiso 1 1 calc R A . H47D H 1.301 0.4772 0.131 0.088 Uiso 1 1 calc R . . C473 C 1.1728(3) 0.4356(3) 0.0995(2) 0.0827(14) Uani 1 1 d . A . H47E H 1.0904 0.4437 0.1115 0.099 Uiso 1 1 calc R . . H47F H 1.2145 0.3604 0.1198 0.099 Uiso 1 1 calc R . . C474 C 1.1827(4) 0.4849(4) 0.0023(3) 0.115(2) Uani 1 1 d . . . H47G H 1.1488 0.5604 -0.0171 0.173 Uiso 1 1 calc R A . H47H H 1.1413 0.4575 -0.0274 0.173 Uiso 1 1 calc R . . H47I H 1.2644 0.4682 -0.0107 0.173 Uiso 1 1 calc R . . C47A C 0.96439(19) 0.42702(17) 0.37121(16) 0.0403(7) Uani 1 1 d . A . C4 C 0.7472(4) 0.3827(3) 0.5251(3) 0.0470(15) Uani 0.5 1 d PD A 1 H4A H 0.6653 0.426 0.5127 0.056 Uiso 0.5 1 calc PR A 1 H4B H 0.7765 0.3872 0.5768 0.056 Uiso 0.5 1 calc PR A 1 C4' C 0.7405(4) 0.4265(4) 0.5291(3) 0.0388(11) Uiso 0.5 1 d P A 2 H4'A H 0.7616 0.4698 0.5547 0.058 Uiso 0.5 1 calc PR A 2 H4'B H 0.7542 0.356 0.5721 0.058 Uiso 0.5 1 calc PR A 2 H4'C H 0.6585 0.4561 0.5095 0.058 Uiso 0.5 1 calc PR A 2 Cl11 Cl 0.0468(2) 0.28211(18) -0.01344(12) 0.1949(11) Uani 1 1 d . B 1 Cl12 Cl 0.25818(13) 0.21430(18) -0.08161(14) 0.1847(10) Uani 1 1 d . B 1 Cl13 Cl 0.1357(2) 0.07224(15) -0.00678(13) 0.2888(9) Uani 1 1 d . B 1 C01 C 0.1746(5) 0.1744(4) 0.0005(4) 0.132(2) Uani 1 1 d . B 1 H01 H 0.2168 0.1526 0.057 0.159 Uiso 1 1 calc R B 1 C201 C 0.3440(7) -0.1116(5) 0.2942(3) 0.093(2) Uiso 0.5 1 d PD C 1 H20A H 0.406 -0.0968 0.3173 0.14 Uiso 0.5 1 calc PR C 1 H20B H 0.3639 -0.1864 0.3077 0.14 Uiso 0.5 1 calc PR C 1 H20C H 0.2716 -0.0886 0.32 0.14 Uiso 0.5 1 calc PR C 1 C203 C 0.3170(5) -0.1242(4) 0.2332(5) 0.090(2) Uiso 0.5 1 d PD D 2 H20D H 0.2556 -0.1033 0.269 0.135 Uiso 0.5 1 calc PR D 2 H20E H 0.3642 -0.196 0.2645 0.135 Uiso 0.5 1 calc PR D 2 H20F H 0.2823 -0.1194 0.1801 0.135 Uiso 0.5 1 calc PR D 2 C202 C 0.4473(6) -0.0984(5) 0.1373(4) 0.138(4) Uiso 0.5 1 d PD C 1 H20G H 0.4329 -0.0679 0.0747 0.206 Uiso 0.5 1 calc PR C 1 H20H H 0.4629 -0.1738 0.1573 0.206 Uiso 0.5 1 calc PR C 1 H20I H 0.5143 -0.0831 0.1529 0.206 Uiso 0.5 1 calc PR C 1 C204 C 0.4881(5) -0.0643(6) 0.1258(4) 0.121(3) Uiso 0.5 1 d PD D 2 H20J H 0.4461 -0.0189 0.0703 0.181 Uiso 0.5 1 calc PR D 2 H20K H 0.5025 -0.137 0.1332 0.181 Uiso 0.5 1 calc PR D 2 H20L H 0.5621 -0.0507 0.1276 0.181 Uiso 0.5 1 calc PR D 2 S20 S 0.3272(4) -0.0465(2) 0.1846(2) 0.1631(18) Uani 0.5 1 d PD C 1 S20' S 0.40658(11) -0.03991(10) 0.20750(9) 0.0659(4) Uani 0.5 1 d PD D 2 O20 O 0.3184(3) 0.06862(17) 0.1644(2) 0.1305(12) Uani 1 1 d D . . C301 C 0.7937(6) 0.0205(5) 0.5568(7) 0.267(11) Uiso 0.5 1 d PD E 3 H30A H 0.754 0.0158 0.61 0.401 Uiso 0.5 1 calc PR E 3 H30B H 0.8633 -0.0393 0.5686 0.401 Uiso 0.5 1 calc PR E 3 H30C H 0.7419 0.0207 0.5141 0.401 Uiso 0.5 1 calc PR E 3 C302 C 0.9588(5) 0.1203(7) 0.5626(5) 0.219(8) Uiso 0.5 1 d PD E 3 H30D H 0.984 0.0543 0.6119 0.328 Uiso 0.5 1 calc PR E 3 H30E H 0.9488 0.178 0.5817 0.328 Uiso 0.5 1 calc PR E 3 H30F H 1.0172 0.1222 0.5198 0.328 Uiso 0.5 1 calc PR E 3 S30 S 0.8313(5) 0.1312(4) 0.5184(3) 0.313(5) Uani 0.5 1 d PD E 3 O30 O 0.8376(7) 0.1662(6) 0.4179(3) 0.164(3) Uiso 0.5 1 d PD E 3 C401 C 0.8535(6) 0.2666(12) 0.1910(4) 0.239(10) Uiso 0.5 1 d PD F 4 H40A H 0.8385 0.3375 0.1889 0.359 Uiso 0.5 1 calc PR F 4 H40B H 0.782 0.2471 0.202 0.359 Uiso 0.5 1 calc PR F 4 H40C H 0.8813 0.2632 0.136 0.359 Uiso 0.5 1 calc PR F 4 C402 C 0.9137(9) 0.1860(15) 0.3706(4) 0.464(7) Uiso 0.5 1 d PD F 4 H40D H 0.9819 0.174 0.4057 0.696 Uiso 0.5 1 calc PR F 4 H40E H 0.8772 0.1313 0.3991 0.696 Uiso 0.5 1 calc PR F 4 H40F H 0.8585 0.2537 0.3635 0.696 Uiso 0.5 1 calc PR F 4 S40 S 0.9550(6) 0.1838(7) 0.2705(4) 0.464(7) Uiso 0.5 1 d PD F 4 O40 O 1.0687(5) 0.2147(10) 0.2547(7) 0.366(11) Uiso 0.5 1 d PD F 4 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 0.03155(7) 0.03226(6) 0.04365(8) -0.00900(6) -0.00267(6) -0.00850(5) Br1 0.03587(10) 0.04594(11) 0.06281(14) -0.01717(10) -0.00683(10) -0.00576(9) Br2 0.04763(12) 0.03910(9) 0.06310(14) -0.01574(9) -0.00462(11) -0.01337(9) C11 0.0630(17) 0.0560(16) 0.060(2) -0.0172(17) 0.0011(18) -0.0278(15) C12 0.0660(18) 0.0520(16) 0.056(2) -0.0162(16) 0.0052(18) -0.0300(13) C13 0.0687(18) 0.0687(16) 0.052(2) -0.0127(17) -0.0028(18) -0.0372(15) C14 0.0667(18) 0.0621(17) 0.053(2) -0.0096(18) -0.0083(19) -0.0138(17) C15 0.0782(19) 0.0513(17) 0.065(2) -0.0017(19) 0.006(2) -0.0312(14) C16 0.0676(18) 0.0622(16) 0.063(2) -0.0110(17) -0.0049(18) -0.0407(14) C1 0.070(3) 0.044(2) 0.034(2) -0.0090(17) -0.006(2) -0.0292(19) C1' 0.051(2) 0.032(2) 0.027(2) 0.0013(17) -0.0084(19) -0.0105(19) N21 0.0346(8) 0.0341(8) 0.0429(9) -0.0070(7) -0.0014(7) -0.0138(6) C22 0.0334(4) 0.0379(2) 0.0455(8) -0.0116(3) -0.0039(5) -0.0111(2) N23 0.0404(9) 0.0376(8) 0.0429(9) -0.0113(7) 0.0012(8) -0.0125(7) C23A 0.0370(10) 0.0337(8) 0.0540(11) -0.0153(7) -0.0013(9) -0.0064(8) C24 0.0437(10) 0.0377(9) 0.0560(10) -0.0178(8) -0.0046(9) -0.0079(8) O24 0.0590(9) 0.0523(8) 0.0554(8) -0.0195(6) -0.0021(8) -0.0182(7) C241 0.0696(14) 0.0612(12) 0.0550(11) -0.0247(9) -0.0048(11) -0.0176(11) C242 0.1060(16) 0.0847(16) 0.0573(13) -0.0210(12) -0.0076(14) -0.0371(14) C243 0.1247(18) 0.120(2) 0.0640(18) -0.0176(17) 0.0071(17) -0.0637(16) C244 0.107(3) 0.172(4) 0.117(4) -0.019(3) 0.016(3) -0.037(3) C25 0.0437(11) 0.0375(9) 0.0649(11) -0.0254(8) -0.0046(10) -0.0066(8) C26 0.0400(10) 0.0318(9) 0.0644(12) -0.0139(8) -0.0002(10) -0.0097(8) C27 0.0365(10) 0.0320(9) 0.0558(11) -0.0104(8) -0.0030(9) -0.0093(8) O27 0.0456(8) 0.0397(7) 0.0500(8) -0.0075(6) 0.0015(7) -0.0187(6) C271 0.0363(11) 0.0366(10) 0.0749(16) -0.0137(10) -0.0014(11) -0.0149(8) C272 0.0426(12) 0.0357(11) 0.0691(16) -0.0102(11) 0.0064(12) -0.0100(10) C273 0.0563(15) 0.0500(14) 0.089(2) -0.0060(15) 0.0113(15) -0.0200(12) C274 0.069(2) 0.072(2) 0.088(3) 0.003(2) 0.0193(19) -0.0073(18) C27A 0.0359(10) 0.0274(9) 0.0515(13) -0.0082(8) -0.0027(10) -0.0070(8) C2' 0.0247(17) 0.0351(17) 0.040(2) -0.0109(15) 0.0040(16) -0.0142(14) C2 0.038(2) 0.071(3) 0.072(3) -0.027(2) 0.013(2) -0.023(2) C31 0.0314(18) 0.0339(18) 0.0240(18) -0.0054(14) 0.0014(15) -0.0106(15) C32 0.0302(18) 0.0256(15) 0.0310(18) -0.0104(13) 0.0072(15) -0.0097(14) C33 0.040(2) 0.0356(18) 0.044(2) -0.0122(16) 0.0115(18) -0.0201(15) C34 0.046(2) 0.0214(16) 0.049(2) -0.0127(15) 0.007(2) -0.0068(16) C35 0.042(2) 0.0195(16) 0.070(3) -0.0172(17) -0.004(2) 0.0051(17) C36 0.034(2) 0.0310(17) 0.045(2) -0.0131(15) -0.0014(18) -0.0082(16) C3' 0.0251(18) 0.0182(17) 0.060(3) 0.0002(18) 0.0001(19) -0.0056(14) C3 0.035(2) 0.064(3) 0.039(3) 0.005(2) -0.010(2) -0.016(2) N41 0.0294(8) 0.0425(8) 0.0441(9) -0.0129(7) -0.0002(7) -0.0092(7) C42 0.0333(3) 0.0385(4) 0.0442(9) -0.0119(5) -0.0014(4) -0.0121(3) N43 0.0375(9) 0.0386(8) 0.0473(10) -0.0079(7) 0.0004(8) -0.0145(7) C43A 0.0323(10) 0.0339(9) 0.0509(12) -0.0139(8) -0.0053(9) -0.0062(8) C44 0.0398(11) 0.0325(9) 0.0582(13) -0.0135(9) -0.0081(10) -0.0080(9) O44 0.0445(8) 0.0417(8) 0.0489(9) -0.0086(7) -0.0125(7) -0.0056(7) C441 0.0519(14) 0.0503(12) 0.0582(14) -0.0182(10) -0.0206(11) -0.0018(11) C442 0.0665(18) 0.0696(17) 0.0516(15) -0.0194(12) -0.0138(13) 0.0041(15) C443 0.096(2) 0.079(2) 0.065(2) -0.0016(18) 0.0019(19) -0.019(2) C444 0.096(3) 0.115(4) 0.216(7) -0.035(4) 0.021(4) -0.013(3) C45 0.0405(11) 0.0307(9) 0.0629(13) -0.0158(9) -0.0160(10) -0.0027(9) C46 0.0305(10) 0.0419(10) 0.0649(14) -0.0185(9) -0.0047(10) -0.0084(9) C47 0.0337(10) 0.0376(10) 0.0554(13) -0.0148(9) -0.0074(10) -0.0061(9) O47 0.0296(7) 0.0509(8) 0.0565(9) -0.0147(7) 0.0016(7) -0.0085(6) C471 0.0290(11) 0.0531(13) 0.0724(17) -0.0142(12) -0.0009(11) -0.0099(10) C472 0.0420(13) 0.083(2) 0.076(2) -0.0094(17) 0.0100(14) -0.0200(13) C473 0.074(2) 0.096(2) 0.0630(19) -0.0220(17) 0.0139(16) -0.0178(18) C474 0.110(3) 0.143(4) 0.070(2) -0.024(2) 0.016(2) -0.031(3) C47A 0.0296(10) 0.0323(9) 0.0530(12) -0.0118(8) -0.0076(9) -0.0044(8) C4 0.036(2) 0.064(2) 0.043(2) -0.0269(18) 0.0012(19) -0.009(2) Cl11 0.1868(18) 0.2390(18) 0.1350(11) -0.0824(11) 0.0139(12) -0.0158(16) Cl12 0.0882(8) 0.2502(19) 0.2020(16) -0.0812(14) -0.0090(10) -0.0331(10) Cl13 0.4971(19) 0.1593(11) 0.1891(12) 0.0501(9) -0.2027(11) -0.1757(11) C01 0.156(4) 0.123(3) 0.100(3) -0.004(3) -0.048(3) -0.053(3) S20 0.173(3) 0.0875(16) 0.197(3) -0.0450(18) -0.010(3) -0.0016(19) S20' 0.0834(6) 0.0534(5) 0.0617(7) 0.0029(5) -0.0392(5) -0.0449(4) O20 0.179(2) 0.0606(12) 0.144(2) -0.0214(12) -0.0789(17) -0.0296(14) S30 0.435(10) 0.255(7) 0.116(3) -0.022(4) -0.038(5) 0.030(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C42 1.994(2) . ? Pd1 C22 2.003(3) . ? Pd1 Br2 2.4664(4) . ? Pd1 Br1 2.4719(3) . ? C11 C16 1.423(7) . ? C11 C12 1.432(7) . ? C11 C1 1.524(6) . ? C12 C13 1.434(6) . ? C12 C4 1.537(7) . ? C13 C14 1.396(7) . ? C13 H13 0.95 . ? C14 C15 1.410(8) . ? C14 H14 0.95 . ? C15 C16 1.362(6) . ? C15 H15 0.95 . ? C16 H16 0.95 . ? C1 N21 1.526(6) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? C1' N21 1.440(6) . ? C1' H1'A 0.98 . ? C1' H1'B 0.98 . ? C1' H1'C 0.98 . ? N21 C22 1.339(3) . ? N21 C27A 1.391(4) . ? C22 N23 1.353(4) . ? N23 C23A 1.391(4) . ? N23 C2 1.405(6) . ? N23 C2' 1.532(5) . ? C23A C27A 1.380(4) . ? C23A C24 1.393(4) . ? C24 O24 1.365(3) . ? C24 C25 1.397(4) . ? O24 C241 1.439(4) . ? C241 C242 1.510(4) . ? C241 H24A 0.99 . ? C241 H24B 0.99 . ? C242 C243 1.529(6) . ? C242 H24C 0.99 . ? C242 H24D 0.99 . ? C243 C244 1.472(7) . ? C243 H24E 0.99 . ? C243 H24F 0.99 . ? C244 H24G 0.98 . ? C244 H24H 0.98 . ? C244 H24I 0.98 . ? C25 C26 1.412(4) . ? C25 H25 0.95 . ? C26 C27 1.388(5) . ? C26 H26 0.95 . ? C27 O27 1.351(3) . ? C27 C27A 1.417(4) . ? O27 C271 1.452(3) . ? C271 C272 1.500(5) . ? C271 H27A 0.99 . ? C271 H27B 0.99 . ? C272 C273 1.525(4) . ? C272 H27C 0.99 . ? C272 H27D 0.99 . ? C273 C274 1.512(6) . ? C273 H27E 0.99 . ? C273 H27F 0.99 . ? C274 H27G 0.98 . ? C274 H27H 0.98 . ? C274 H27I 0.98 . ? C2' C32 1.497(5) . ? C2' H2'A 0.99 . ? C2' H2'B 0.99 . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C31 C32 1.398(6) . ? C31 C36 1.403(5) . ? C31 C3' 1.493(6) . ? C32 C33 1.410(6) . ? C33 C34 1.375(5) . ? C33 H33 0.95 . ? C34 C35 1.371(7) . ? C34 H34 0.95 . ? C35 C36 1.412(6) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C3' N41 1.412(6) . ? C3' H3'A 0.99 . ? C3' H3'B 0.99 . ? C3 N41 1.516(6) . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? N41 C42 1.342(3) . ? N41 C47A 1.401(3) . ? C42 N43 1.358(3) . ? N43 C43A 1.408(3) . ? N43 C4 1.451(5) . ? N43 C4' 1.525(5) . ? C43A C47A 1.370(4) . ? C43A C44 1.402(4) . ? C44 O44 1.356(3) . ? C44 C45 1.378(4) . ? O44 C441 1.449(3) . ? C441 C442 1.484(4) . ? C441 H44A 0.99 . ? C441 H44B 0.99 . ? C442 C443 1.489(6) . ? C442 H44C 0.99 . ? C442 H44D 0.99 . ? C443 C444 1.487(7) . ? C443 H44E 0.99 . ? C443 H44F 0.99 . ? C444 H44G 0.98 . ? C444 H44H 0.98 . ? C444 H44I 0.98 . ? C45 C46 1.389(4) . ? C45 H45 0.95 . ? C46 C47 1.374(4) . ? C46 H46 0.95 . ? C47 O47 1.356(3) . ? C47 C47A 1.420(3) . ? O47 C471 1.445(3) . ? C471 C472 1.505(5) . ? C471 H47A 0.99 . ? C471 H47B 0.99 . ? C472 C473 1.453(7) . ? C472 H47C 0.99 . ? C472 H47D 0.99 . ? C473 C474 1.533(5) . ? C473 H47E 0.99 . ? C473 H47F 0.99 . ? C474 H47G 0.98 . ? C474 H47H 0.98 . ? C474 H47I 0.98 . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C4' H4'A 0.98 . ? C4' H4'B 0.98 . ? C4' H4'C 0.98 . ? Cl11 C01 1.796(6) . ? Cl12 C01 1.693(6) . ? Cl13 C01 1.738(7) . ? C01 H01 1 . ? C201 S20 1.721(6) . ? C201 H20A 0.98 . ? C201 H20B 0.98 . ? C201 H20C 0.98 . ? C203 S20' 1.797(6) . ? C203 H20D 0.98 . ? C203 H20E 0.98 . ? C203 H20F 0.98 . ? C202 S20 1.727(7) . ? C202 H20G 0.98 . ? C202 H20H 0.98 . ? C202 H20I 0.98 . ? C204 S20' 1.729(7) . ? C204 H20J 0.98 . ? C204 H20K 0.98 . ? C204 H20L 0.98 . ? S20 O20 1.552(4) . ? S20' O20 1.545(2) . ? C301 S30 1.690(9) . ? C301 H30A 0.98 . ? C301 H30B 0.98 . ? C301 H30C 0.98 . ? C302 S30 1.696(9) . ? C302 H30D 0.98 . ? C302 H30E 0.98 . ? C302 H30F 0.98 . ? S30 O30 1.578(7) . ? C401 S40 1.690(8) . ? C401 H40A 0.98 . ? C401 H40B 0.98 . ? C401 H40C 0.98 . ? C402 S40 1.737(11) . ? C402 H40D 0.9805 . ? C402 H40E 0.9805 . ? C402 H40F 0.9805 . ? S40 O40 1.555(11) . ? 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 C42 Pd1 C22 96.57(10) . . ? C42 Pd1 Br2 85.69(8) . . ? C22 Pd1 Br2 177.16(6) . . ? C42 Pd1 Br1 179.20(7) . . ? C22 Pd1 Br1 84.21(6) . . ? Br2 Pd1 Br1 93.522(12) . . ? C16 C11 C12 117.5(4) . . ? C16 C11 C1 119.0(5) . . ? C12 C11 C1 123.4(4) . . ? C11 C12 C13 116.7(4) . . ? C11 C12 C4 123.2(4) . . ? C13 C12 C4 120.1(5) . . ? C14 C13 C12 123.8(5) . . ? C14 C13 H13 118.1 . . ? C12 C13 H13 118.1 . . ? C13 C14 C15 118.1(4) . . ? C13 C14 H14 121 . . ? C15 C14 H14 121 . . ? C16 C15 C14 119.3(5) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C11 124.4(6) . . ? C15 C16 H16 117.8 . . ? C11 C16 H16 117.8 . . ? C11 C1 N21 108.8(4) . . ? C11 C1 H1A 109.9 . . ? N21 C1 H1A 109.9 . . ? C11 C1 H1B 109.9 . . ? N21 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N21 C1' H1'A 109.5 . . ? N21 C1' H1'B 109.5 . . ? H1'A C1' H1'B 109.5 . . ? N21 C1' H1'C 109.5 . . ? H1'A C1' H1'C 109.5 . . ? H1'B C1' H1'C 109.5 . . ? C22 N21 C27A 109.2(2) . . ? C22 N21 C1' 124.9(3) . . ? C27A N21 C1' 124.5(3) . . ? C22 N21 C1 122.3(3) . . ? C27A N21 C1 127.6(3) . . ? N21 C22 N23 107.9(2) . . ? N21 C22 Pd1 126.9(2) . . ? N23 C22 Pd1 123.28(16) . . ? C22 N23 C23A 109.5(2) . . ? C22 N23 C2 127.8(4) . . ? C23A N23 C2 122.2(4) . . ? C22 N23 C2' 120.2(3) . . ? C23A N23 C2' 128.5(3) . . ? C27A C23A N23 106.0(3) . . ? C27A C23A C24 122.1(2) . . ? N23 C23A C24 131.7(2) . . ? O24 C24 C23A 117.6(2) . . ? O24 C24 C25 125.9(3) . . ? C23A C24 C25 116.5(3) . . ? C24 O24 C241 118.2(2) . . ? O24 C241 C242 107.9(3) . . ? O24 C241 H24A 110.1 . . ? C242 C241 H24A 110.1 . . ? O24 C241 H24B 110.1 . . ? C242 C241 H24B 110.1 . . ? H24A C241 H24B 108.4 . . ? C241 C242 C243 115.7(3) . . ? C241 C242 H24C 108.4 . . ? C243 C242 H24C 108.4 . . ? C241 C242 H24D 108.4 . . ? C243 C242 H24D 108.4 . . ? H24C C242 H24D 107.4 . . ? C244 C243 C242 114.3(5) . . ? C244 C243 H24E 108.7 . . ? C242 C243 H24E 108.7 . . ? C244 C243 H24F 108.7 . . ? C242 C243 H24F 108.7 . . ? H24E C243 H24F 107.6 . . ? C243 C244 H24G 109.5 . . ? C243 C244 H24H 109.5 . . ? H24G C244 H24H 109.5 . . ? C243 C244 H24I 109.5 . . ? H24G C244 H24I 109.5 . . ? H24H C244 H24I 109.5 . . ? C24 C25 C26 121.8(3) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C27 C26 C25 121.4(3) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? O27 C27 C26 126.3(2) . . ? O27 C27 C27A 117.4(3) . . ? C26 C27 C27A 116.2(2) . . ? C27 O27 C271 118.2(2) . . ? O27 C271 C272 105.7(2) . . ? O27 C271 H27A 110.6 . . ? C272 C271 H27A 110.6 . . ? O27 C271 H27B 110.6 . . ? C272 C271 H27B 110.6 . . ? H27A C271 H27B 108.7 . . ? C271 C272 C273 114.3(3) . . ? C271 C272 H27C 108.7 . . ? C273 C272 H27C 108.7 . . ? C271 C272 H27D 108.7 . . ? C273 C272 H27D 108.7 . . ? H27C C272 H27D 107.6 . . ? C274 C273 C272 112.0(3) . . ? C274 C273 H27E 109.2 . . ? C272 C273 H27E 109.2 . . ? C274 C273 H27F 109.2 . . ? C272 C273 H27F 109.2 . . ? H27E C273 H27F 107.9 . . ? C273 C274 H27G 109.5 . . ? C273 C274 H27H 109.5 . . ? H27G C274 H27H 109.5 . . ? C273 C274 H27I 109.5 . . ? H27G C274 H27I 109.5 . . ? H27H C274 H27I 109.5 . . ? C23A C27A N21 107.3(2) . . ? C23A C27A C27 122.0(3) . . ? N21 C27A C27 130.6(2) . . ? C32 C2' N23 111.6(3) . . ? C32 C2' H2'A 109.3 . . ? N23 C2' H2'A 109.3 . . ? C32 C2' H2'B 109.3 . . ? N23 C2' H2'B 109.3 . . ? H2'A C2' H2'B 108 . . ? N23 C2 H2A 109.5 . . ? N23 C2 H2B 109.5 . . ? N23 C2 H2C 109.5 . . ? C32 C31 C36 119.3(4) . . ? C32 C31 C3' 124.3(3) . . ? C36 C31 C3' 116.3(4) . . ? C31 C32 C33 119.8(3) . . ? C31 C32 C2' 123.3(4) . . ? C33 C32 C2' 116.8(4) . . ? C34 C33 C32 120.0(4) . . ? C34 C33 H33 120 . . ? C32 C33 H33 120 . . ? C35 C34 C33 121.1(4) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C34 C35 C36 119.8(4) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C31 C36 C35 119.8(4) . . ? C31 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? N41 C3' C31 118.5(3) . . ? N41 C3' H3'A 107.7 . . ? C31 C3' H3'A 107.7 . . ? N41 C3' H3'B 107.7 . . ? C31 C3' H3'B 107.7 . . ? H3'A C3' H3'B 107.1 . . ? N41 C3 H3A 109.5 . . ? N41 C3 H3B 109.5 . . ? N41 C3 H3C 109.5 . . ? C42 N41 C47A 109.5(2) . . ? C42 N41 C3' 120.7(3) . . ? C47A N41 C3' 127.7(2) . . ? C42 N41 C3 124.3(3) . . ? C47A N41 C3 125.6(3) . . ? N41 C42 N43 107.7(2) . . ? N41 C42 Pd1 126.05(17) . . ? N43 C42 Pd1 125.19(17) . . ? C42 N43 C43A 109.1(2) . . ? C42 N43 C4 122.1(3) . . ? C43A N43 C4 125.9(2) . . ? C42 N43 C4' 125.1(2) . . ? C43A N43 C4' 124.6(3) . . ? C47A C43A C44 122.5(2) . . ? C47A C43A N43 106.5(2) . . ? C44 C43A N43 131.0(2) . . ? O44 C44 C45 127.2(2) . . ? O44 C44 C43A 117.0(2) . . ? C45 C44 C43A 115.8(2) . . ? C44 O44 C441 118.2(2) . . ? O44 C441 C442 108.5(2) . . ? O44 C441 H44A 110 . . ? C442 C441 H44A 110 . . ? O44 C441 H44B 110 . . ? C442 C441 H44B 110 . . ? H44A C441 H44B 108.4 . . ? C441 C442 C443 117.5(3) . . ? C441 C442 H44C 107.9 . . ? C443 C442 H44C 107.9 . . ? C441 C442 H44D 107.9 . . ? C443 C442 H44D 107.9 . . ? H44C C442 H44D 107.2 . . ? C444 C443 C442 119.2(4) . . ? C444 C443 H44E 107.5 . . ? C442 C443 H44E 107.5 . . ? C444 C443 H44F 107.5 . . ? C442 C443 H44F 107.5 . . ? H44E C443 H44F 107 . . ? C443 C444 H44G 109.5 . . ? C443 C444 H44H 109.5 . . ? H44G C444 H44H 109.5 . . ? C443 C444 H44I 109.5 . . ? H44G C444 H44I 109.5 . . ? H44H C444 H44I 109.5 . . ? C44 C45 C46 122.0(2) . . ? C44 C45 H45 119 . . ? C46 C45 H45 119 . . ? C47 C46 C45 122.8(2) . . ? C47 C46 H46 118.6 . . ? C45 C46 H46 118.6 . . ? O47 C47 C46 127.6(2) . . ? O47 C47 C47A 116.9(2) . . ? C46 C47 C47A 115.5(2) . . ? C47 O47 C471 116.6(2) . . ? O47 C471 C472 107.4(2) . . ? O47 C471 H47A 110.2 . . ? C472 C471 H47A 110.2 . . ? O47 C471 H47B 110.2 . . ? C472 C471 H47B 110.2 . . ? H47A C471 H47B 108.5 . . ? C473 C472 C471 117.4(3) . . ? C473 C472 H47C 108 . . ? C471 C472 H47C 108 . . ? C473 C472 H47D 108 . . ? C471 C472 H47D 108 . . ? H47C C472 H47D 107.2 . . ? C472 C473 C474 112.1(4) . . ? C472 C473 H47E 109.2 . . ? C474 C473 H47E 109.2 . . ? C472 C473 H47F 109.2 . . ? C474 C473 H47F 109.2 . . ? H47E C473 H47F 107.9 . . ? C473 C474 H47G 109.5 . . ? C473 C474 H47H 109.5 . . ? H47G C474 H47H 109.5 . . ? C473 C474 H47I 109.5 . . ? H47G C474 H47I 109.5 . . ? H47H C474 H47I 109.5 . . ? C43A C47A N41 107.1(2) . . ? C43A C47A C47 121.4(2) . . ? N41 C47A C47 131.5(2) . . ? N43 C4 C12 111.6(4) . . ? N43 C4 H4A 109.3 . . ? C12 C4 H4A 109.3 . . ? N43 C4 H4B 109.3 . . ? C12 C4 H4B 109.3 . . ? H4A C4 H4B 108 . . ? N43 C4' H4'A 109.5 . . ? N43 C4' H4'B 109.5 . . ? H4'A C4' H4'B 109.5 . . ? N43 C4' H4'C 109.5 . . ? H4'A C4' H4'C 109.5 . . ? H4'B C4' H4'C 109.5 . . ? Cl12 C01 Cl13 108.5(4) . . ? Cl12 C01 Cl11 106.9(3) . . ? Cl13 C01 Cl11 109.1(3) . . ? Cl12 C01 H01 110.7 . . ? Cl13 C01 H01 110.7 . . ? Cl11 C01 H01 110.7 . . ? S20' C203 H20D 109.5 . . ? S20' C203 H20E 109.5 . . ? H20D C203 H20E 109.5 . . ? S20' C203 H20F 109.5 . . ? H20D C203 H20F 109.5 . . ? H20E C203 H20F 109.5 . . ? S20' C204 H20J 109.5 . . ? S20' C204 H20K 109.5 . . ? H20J C204 H20K 109.5 . . ? S20' C204 H20L 109.5 . . ? H20J C204 H20L 109.5 . . ? H20K C204 H20L 109.5 . . ? O20 S20 C201 108.3(4) . . ? O20 S20 C202 107.9(4) . . ? C201 S20 C202 109.8(4) . . ? O20 S20' C204 105.5(2) . . ? O20 S20' C203 102.5(2) . . ? C204 S20' C203 104.9(4) . . ? O30 S30 C301 108.9(6) . . ? O30 S30 C302 109.6(5) . . ? C301 S30 C302 113.6(5) . . ? O40 S40 C401 110.1(7) . . ? O40 S40 C402 106.3(8) . . ? C401 S40 C402 112.6(6) . . ? 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 C16 C11 C12 C13 1.2(6) . . . . ? C1 C11 C12 C13 -179.2(5) . . . . ? C16 C11 C12 C4 -178.0(5) . . . . ? C1 C11 C12 C4 1.6(7) . . . . ? C11 C12 C13 C14 2.9(7) . . . . ? C4 C12 C13 C14 -177.9(5) . . . . ? C12 C13 C14 C15 -4.6(8) . . . . ? C13 C14 C15 C16 1.9(9) . . . . ? C14 C15 C16 C11 2.2(10) . . . . ? C12 C11 C16 C15 -3.8(9) . . . . ? C1 C11 C16 C15 176.5(6) . . . . ? C16 C11 C1 N21 -76.5(6) . . . . ? C12 C11 C1 N21 103.8(5) . . . . ? C11 C1 N21 C22 -82.5(4) . . . . ? C11 C1 N21 C27A 84.9(4) . . . . ? C11 C1 N21 C1' 173.3(12) . . . . ? C27A N21 C22 N23 -1.4(2) . . . . ? C1' N21 C22 N23 -168.6(3) . . . . ? C1 N21 C22 N23 168.0(2) . . . . ? C27A N21 C22 Pd1 163.09(15) . . . . ? C1' N21 C22 Pd1 -4.1(4) . . . . ? C1 N21 C22 Pd1 -27.5(3) . . . . ? C42 Pd1 C22 N21 97.29(19) . . . . ? Br1 Pd1 C22 N21 -82.88(18) . . . . ? C42 Pd1 C22 N23 -100.45(19) . . . . ? Br1 Pd1 C22 N23 79.38(17) . . . . ? N21 C22 N23 C23A 1.9(2) . . . . ? Pd1 C22 N23 C23A -163.22(15) . . . . ? N21 C22 N23 C2 173.7(3) . . . . ? Pd1 C22 N23 C2 8.5(4) . . . . ? N21 C22 N23 C2' -164.4(2) . . . . ? Pd1 C22 N23 C2' 30.4(3) . . . . ? C22 N23 C23A C27A -1.7(2) . . . . ? C2 N23 C23A C27A -174.0(3) . . . . ? C2' N23 C23A C27A 163.2(2) . . . . ? C22 N23 C23A C24 172.8(2) . . . . ? C2 N23 C23A C24 0.5(4) . . . . ? C2' N23 C23A C24 -22.3(4) . . . . ? C27A C23A C24 O24 176.03(19) . . . . ? N23 C23A C24 O24 2.2(4) . . . . ? C27A C23A C24 C25 -1.3(3) . . . . ? N23 C23A C24 C25 -175.0(2) . . . . ? C23A C24 O24 C241 -179.6(2) . . . . ? C25 C24 O24 C241 -2.6(3) . . . . ? C24 O24 C241 C242 176.3(2) . . . . ? O24 C241 C242 C243 58.0(4) . . . . ? C241 C242 C243 C244 63.4(6) . . . . ? O24 C24 C25 C26 -177.4(2) . . . . ? C23A C24 C25 C26 -0.4(3) . . . . ? C24 C25 C26 C27 1.4(3) . . . . ? C25 C26 C27 O27 -179.9(2) . . . . ? C25 C26 C27 C27A -0.7(3) . . . . ? C26 C27 O27 C271 -5.6(3) . . . . ? C27A C27 O27 C271 175.24(18) . . . . ? C27 O27 C271 C272 178.53(17) . . . . ? O27 C271 C272 C273 178.03(19) . . . . ? C271 C272 C273 C274 177.7(2) . . . . ? N23 C23A C27A N21 0.8(2) . . . . ? C24 C23A C27A N21 -174.34(19) . . . . ? N23 C23A C27A C27 177.13(19) . . . . ? C24 C23A C27A C27 2.0(3) . . . . ? C22 N21 C27A C23A 0.3(2) . . . . ? C1' N21 C27A C23A 167.6(3) . . . . ? C1 N21 C27A C23A -168.4(3) . . . . ? C22 N21 C27A C27 -175.5(2) . . . . ? C1' N21 C27A C27 -8.3(4) . . . . ? C1 N21 C27A C27 15.8(4) . . . . ? O27 C27 C27A C23A 178.37(19) . . . . ? C26 C27 C27A C23A -0.9(3) . . . . ? O27 C27 C27A N21 -6.3(3) . . . . ? C26 C27 C27A N21 174.4(2) . . . . ? C22 N23 C2' C32 82.3(4) . . . . ? C23A N23 C2' C32 -81.2(4) . . . . ? C2 N23 C2' C32 -159.2(13) . . . . ? C36 C31 C32 C33 -0.9(6) . . . . ? C3' C31 C32 C33 -177.5(4) . . . . ? C36 C31 C32 C2' -178.5(4) . . . . ? C3' C31 C32 C2' 4.9(6) . . . . ? N23 C2' C32 C31 -107.4(4) . . . . ? N23 C2' C32 C33 74.9(5) . . . . ? C31 C32 C33 C34 0.7(6) . . . . ? C2' C32 C33 C34 178.4(4) . . . . ? C32 C33 C34 C35 -2.6(7) . . . . ? C33 C34 C35 C36 4.6(7) . . . . ? C32 C31 C36 C35 2.9(6) . . . . ? C3' C31 C36 C35 179.8(4) . . . . ? C34 C35 C36 C31 -4.8(7) . . . . ? C32 C31 C3' N41 103.6(4) . . . . ? C36 C31 C3' N41 -73.1(5) . . . . ? C31 C3' N41 C42 -83.2(4) . . . . ? C31 C3' N41 C47A 78.7(5) . . . . ? C31 C3' N41 C3 170.4(10) . . . . ? C47A N41 C42 N43 -1.1(3) . . . . ? C3' N41 C42 N43 163.9(2) . . . . ? C3 N41 C42 N43 -172.7(4) . . . . ? C47A N41 C42 Pd1 167.80(19) . . . . ? C3' N41 C42 Pd1 -27.3(4) . . . . ? C3 N41 C42 Pd1 -3.9(5) . . . . ? C22 Pd1 C42 N41 96.7(2) . . . . ? Br2 Pd1 C42 N41 -81.6(2) . . . . ? C22 Pd1 C42 N43 -96.3(2) . . . . ? Br2 Pd1 C42 N43 85.4(2) . . . . ? N41 C42 N43 C43A 0.3(3) . . . . ? Pd1 C42 N43 C43A -168.72(18) . . . . ? N41 C42 N43 C4 -161.8(3) . . . . ? Pd1 C42 N43 C4 29.3(4) . . . . ? N41 C42 N43 C4' 168.4(3) . . . . ? Pd1 C42 N43 C4' -0.6(4) . . . . ? C42 N43 C43A C47A 0.6(3) . . . . ? C4 N43 C43A C47A 161.8(3) . . . . ? C4' N43 C43A C47A -167.6(3) . . . . ? C42 N43 C43A C44 178.0(3) . . . . ? C4 N43 C43A C44 -20.8(5) . . . . ? C4' N43 C43A C44 9.8(5) . . . . ? C47A C43A C44 O44 178.5(2) . . . . ? N43 C43A C44 O44 1.5(4) . . . . ? C47A C43A C44 C45 -1.0(4) . . . . ? N43 C43A C44 C45 -178.0(3) . . . . ? C45 C44 O44 C441 -5.5(4) . . . . ? C43A C44 O44 C441 175.1(2) . . . . ? C44 O44 C441 C442 -178.3(3) . . . . ? O44 C441 C442 C443 60.4(3) . . . . ? C441 C442 C443 C444 63.6(5) . . . . ? O44 C44 C45 C46 -178.4(3) . . . . ? C43A C44 C45 C46 1.0(4) . . . . ? C44 C45 C46 C47 0.0(4) . . . . ? C45 C46 C47 O47 177.4(3) . . . . ? C45 C46 C47 C47A -1.0(4) . . . . ? C46 C47 O47 C471 3.1(4) . . . . ? C47A C47 O47 C471 -178.5(2) . . . . ? C47 O47 C471 C472 -176.6(3) . . . . ? O47 C471 C472 C473 -59.4(4) . . . . ? C471 C472 C473 C474 -177.9(3) . . . . ? C44 C43A C47A N41 -178.9(2) . . . . ? N43 C43A C47A N41 -1.3(3) . . . . ? C44 C43A C47A C47 0.0(4) . . . . ? N43 C43A C47A C47 177.6(2) . . . . ? C42 N41 C47A C43A 1.5(3) . . . . ? C3' N41 C47A C43A -162.1(3) . . . . ? C3 N41 C47A C43A 173.0(4) . . . . ? C42 N41 C47A C47 -177.3(3) . . . . ? C3' N41 C47A C47 19.2(5) . . . . ? C3 N41 C47A C47 -5.7(5) . . . . ? O47 C47 C47A C43A -177.6(2) . . . . ? C46 C47 C47A C43A 1.0(4) . . . . ? O47 C47 C47A N41 1.0(4) . . . . ? C46 C47 C47A N41 179.6(3) . . . . ? C42 N43 C4 C12 81.3(4) . . . . ? C43A N43 C4 C12 -77.5(5) . . . . ? C4' N43 C4 C12 -173.4(8) . . . . ? C11 C12 C4 N43 -109.3(5) . . . . ? C13 C12 C4 N43 71.6(5) . . . . ? C204 S20' O20 S20 89.4(4) . . . . ? C203 S20' O20 S20 -20.2(4) . . . . ? C201 S20 O20 S20' 61.4(4) . . . . ? C202 S20 O20 S20' -57.4(3) . . . . ?