Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Crabtree, Robert H.' 'Albrecht, Martin' 'Faller, J. W.' 'Grundemann, Stephan' 'Kovacevic, Anes' #============================================================================== _audit_creation_date '2001-11-13' _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; #============================================================================== # SUBMISSION DETAILS _publ_requested_journal ' J. Chem. Soc., Dalton, 2002,B110946B' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name 'Prof Robert H. Crabtree' _publ_contact_author_address ; Yale Chemistry Department 225 Prospect Street New Haven Connecticut 06520 UNITED STATES OF AMERICA ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' (203)-432-3954 ' _publ_contact_author_fax ' (203)-432-6144 ' _publ_contact_author_email 'ROBERT.CRABTREE@YALE.EDU' #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Bis-Carbene Complexes from Oxidative Addition of Imidazolium C-H Bonds to Palladium(0) ; #============================================================================== _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1994). J. Appl. Cryst., 26, 343. ; #============================================================================== data__2133PdBr2(K1K1_N,C)_6 _database_code_CSD 175637 #============================================================================== _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'Denzo-SMN' _computing_data_reduction 'Denzo-SMN' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan for Windows v. 1.06 (MSC 1999)' _computing_publication_material 'teXsan for Windows v. 1.06 (MSC 1999)' #------------------------------------------------------------------------------ _cell_length_a 26.1740(9) _cell_length_b 26.1740(9) _cell_length_c 9.5139(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6517.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 183.2 _cell_measurement_reflns_used 9565 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.5 #------------------------------------------------------------------------------ _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a ' _symmetry_Int_Tables_number 88 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2-y, +z' '3/4-y,1/4+x,1/4+z' '1/4+y,1/4-x,1/4+z' ' -x, -y, -z' ' +x,1/2+y, -z' '3/4+y,1/4-x,1/4-z' '1/4-y,1/4+x,1/4-z' '1/2+x,1/2+y,1/2+z' '1/2-x, -y,1/2+z' '1/4-y,3/4+x,3/4+z' '3/4+y,3/4-x,3/4+z' '1/2-x,1/2-y,1/2-z' '1/2+x, +y,1/2-z' '1/4+y,3/4-x,3/4-z' '3/4-y,3/4+x,3/4-z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'needle' _exptl_crystal_colour 'paleyellow' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 792.89 _chemical_formula_analytical ? _chemical_formula_sum 'C34 H34 Br2 N6 Pd ' _chemical_formula_moiety 'C34 H34 Br2 N6 Pd ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 3168.00 _exptl_absorpt_coefficient_mu 3.063 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min 0.675 _exptl_absorpt_correction_T_max 0.764 _exptl_special_details ; multi-scan from symmetry-related measurements (Blessing 1995) SORTAV R.H Blessing, Acta Cryst., A51, 33-37 (1995), J. Appl. Cryst., 30, 421-426 (1997). ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 183.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 10939 _reflns_number_total 3939 _reflns_number_gt 2066 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.05100 _diffrn_reflns_av_sigmaI/netI 0.135 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 272 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 272 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Br 0 16 -0.374 2.456 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 48 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Pd 0 8 -1.177 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pd(1) 0.0000 0.0000 0.0000 0.0213(1) 0.500 S Uani d ? Br(1) -0.06053(2) -0.03712(2) -0.16518(6) 0.0344(2) 1.000 . Uani d ? N(1) -0.0438(1) 0.10824(13) 0.0081(4) 0.0259(11) 1.000 . Uani d ? N(2) -0.0863(1) 0.06013(13) 0.1469(4) 0.0255(11) 1.000 . Uani d ? N(3) 0.0075(2) 0.1744(2) -0.0685(5) 0.042(1) 1.000 . Uani d ? C(1) -0.0093(2) 0.1276(2) -0.0950(5) 0.030(1) 1.000 . Uani d ? C(2) 0.0027(2) 0.0999(2) -0.2147(5) 0.031(1) 1.000 . Uani d ? C(3) 0.0342(2) 0.1226(2) -0.3130(6) 0.041(2) 1.000 . Uani d ? C(4) 0.0528(2) 0.1714(2) -0.2869(7) 0.050(2) 1.000 . Uani d ? C(5) 0.0387(2) 0.1951(2) -0.1651(7) 0.050(2) 1.000 . Uani d ? C(11) -0.0478(2) 0.0587(2) 0.0510(5) 0.0230(13) 1.000 . Uani d ? C(12) -0.1047(2) 0.1094(2) 0.1636(5) 0.036(2) 1.000 . Uani d ? C(13) -0.0782(2) 0.1396(2) 0.0778(6) 0.036(2) 1.000 . Uani d ? C(14) -0.1055(2) 0.0182(2) 0.2312(5) 0.028(1) 1.000 . Uani d ? C(15) -0.1462(2) -0.0104(2) 0.1797(5) 0.030(1) 1.000 . Uani d ? C(16) -0.1646(2) -0.0495(2) 0.2655(6) 0.037(2) 1.000 . Uani d ? C(17) -0.1449(2) -0.0587(2) 0.3974(6) 0.042(2) 1.000 . Uani d ? C(18) -0.1067(2) -0.0272(2) 0.4484(5) 0.039(2) 1.000 . Uani d ? C(19) -0.0863(2) 0.0120(2) 0.3677(5) 0.031(1) 1.000 . Uani d ? C(20) -0.1716(2) 0.0015(2) 0.0421(5) 0.041(2) 1.000 . Uani d ? C(22) -0.1653(3) -0.1026(2) 0.4844(7) 0.063(2) 1.000 . Uani d ? C(29) -0.0467(2) 0.0479(2) 0.4272(5) 0.041(2) 1.000 . Uani d ? H(1) -0.0360 0.0360 0.5168 0.049 1.000 . Uiso c ? H(2) -0.2013 -0.1048 0.4731 0.076 1.000 . Uiso c ? H(3) -0.1497 -0.0081 -0.0330 0.050 1.000 . Uiso c ? H(4) -0.0103 0.0664 -0.2286 0.038 1.000 . Uiso c ? H(5) 0.0431 0.1052 -0.3972 0.049 1.000 . Uiso c ? H(6) 0.0747 0.1879 -0.3522 0.060 1.000 . Uiso c ? H(7) 0.0518 0.2283 -0.1475 0.060 1.000 . Uiso c ? H(8) -0.1314 0.1197 0.2250 0.043 1.000 . Uiso c ? H(9) -0.0820 0.1755 0.0667 0.043 1.000 . Uiso c ? H(10) -0.1916 -0.0705 0.2319 0.044 1.000 . Uiso c ? H(11) -0.0942 -0.0324 0.5409 0.046 1.000 . Uiso c ? H(12) -0.1785 0.0371 0.0368 0.050 1.000 . Uiso c ? H(13) -0.2027 -0.0170 0.0354 0.050 1.000 . Uiso c ? H(14) -0.1500 -0.1336 0.4541 0.076 1.000 . Uiso c ? H(15) -0.1574 -0.0970 0.5807 0.076 1.000 . Uiso c ? H(16) -0.0182 0.0494 0.3657 0.049 1.000 . Uiso c ? H(17) -0.0611 0.0811 0.4367 0.049 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.0229(3) 0.0177(3) 0.0233(3) -0.0000(2) -0.0018(2) 0.0004(2) Br(1) 0.0304(3) 0.0370(3) 0.0358(3) -0.0026(2) -0.0073(3) -0.0076(2) N(1) 0.027(2) 0.021(2) 0.030(2) 0.002(2) 0.001(2) 0.003(2) N(2) 0.028(2) 0.022(2) 0.026(2) 0.002(2) 0.000(2) 0.001(2) N(3) 0.041(3) 0.026(2) 0.059(3) -0.006(2) 0.002(2) 0.001(2) C(1) 0.027(3) 0.021(3) 0.041(3) 0.002(2) -0.004(2) 0.008(3) C(2) 0.033(3) 0.026(3) 0.036(3) 0.001(2) -0.003(2) 0.005(2) C(3) 0.037(3) 0.044(3) 0.042(3) 0.008(3) 0.006(3) 0.013(3) C(4) 0.032(3) 0.043(4) 0.074(5) -0.002(3) 0.011(3) 0.021(3) C(5) 0.039(3) 0.032(3) 0.079(5) -0.010(3) 0.001(4) 0.009(3) C(11) 0.023(3) 0.024(3) 0.022(3) 0.000(2) -0.005(2) 0.001(2) C(12) 0.042(3) 0.030(3) 0.036(3) 0.010(2) 0.008(3) 0.002(3) C(13) 0.039(3) 0.023(3) 0.045(3) 0.011(2) 0.004(3) -0.003(3) C(14) 0.033(3) 0.022(3) 0.030(3) 0.000(2) 0.010(2) 0.001(2) C(15) 0.033(3) 0.032(3) 0.026(3) -0.002(2) 0.008(2) -0.005(2) C(16) 0.035(3) 0.035(3) 0.041(3) -0.005(2) 0.012(3) -0.011(3) C(17) 0.051(4) 0.040(3) 0.034(3) 0.004(3) 0.019(3) 0.006(3) C(18) 0.041(3) 0.049(4) 0.026(3) 0.014(3) 0.006(3) 0.007(3) C(19) 0.036(3) 0.034(3) 0.024(3) 0.009(2) 0.002(2) -0.002(2) C(20) 0.040(3) 0.050(4) 0.033(3) -0.008(3) 0.001(3) -0.010(3) C(22) 0.079(5) 0.055(4) 0.055(4) -0.003(4) 0.031(4) 0.010(3) C(29) 0.041(3) 0.049(4) 0.033(3) -0.000(3) -0.006(3) -0.009(3) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2066 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_all 0.048 _refine_ls_wR_factor_ref 0.033 _refine_ls_goodness_of_fit_all 0.832 _refine_ls_goodness_of_fit_ref 0.780 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.36 _refine_diff_density_max 0.35 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) Br(1) 2.4338(4) . . ? Pd(1) Br(1) 2.4338(4) . . ? Pd(1) C(11) 2.041(4) . . ? Pd(1) C(11) 2.041(4) . . ? N(1) C(1) 1.427(5) . . ? N(1) C(11) 1.363(5) . . ? N(1) C(13) 1.387(5) . . ? N(2) C(11) 1.359(5) . . ? N(2) C(12) 1.385(5) . . ? N(2) C(14) 1.449(5) . . ? N(3) C(1) 1.325(5) . . ? N(3) C(5) 1.343(6) . . ? C(1) C(2) 1.386(6) . . ? C(2) C(3) 1.382(6) . . ? C(2) H(4) 0.95 . . no C(3) C(4) 1.387(7) . . ? C(3) H(5) 0.95 . . no C(4) C(5) 1.365(7) . . ? C(4) H(6) 0.95 . . no C(5) H(7) 0.95 . . no C(12) C(13) 1.332(6) . . ? C(12) H(8) 0.95 . . no C(13) H(9) 0.95 . . no C(14) C(15) 1.390(6) . . ? C(14) C(19) 1.402(6) . . ? C(15) C(16) 1.396(6) . . ? C(15) C(20) 1.501(6) . . ? C(16) C(17) 1.378(6) . . ? C(16) H(10) 0.95 . . no C(17) C(18) 1.383(6) . . ? C(17) C(22) 1.514(6) . . ? C(18) C(19) 1.387(6) . . ? C(18) H(11) 0.95 . . no C(19) C(29) 1.510(6) . . ? C(20) H(3) 0.95 . . no C(20) H(12) 0.95 . . no C(20) H(13) 0.95 . . no C(22) H(2) 0.95 . . no C(22) H(14) 0.95 . . no C(22) H(15) 0.95 . . no C(29) H(1) 0.95 . . no C(29) H(16) 0.95 . . no C(29) H(17) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br(1) Pd(1) Br(1) 180.00 . . . ? Br(1) Pd(1) C(11) 93.15(11) . . . ? Br(1) Pd(1) C(11) 86.85(11) . . . ? Br(1) Pd(1) C(11) 86.85(11) 5 5 5 ? Br(1) Pd(1) C(11) 93.15(11) 5 5 5 ? C(11) Pd(1) C(11) 180.00 . . . ? C(1) N(1) C(11) 126.3(3) . . . ? C(1) N(1) C(13) 122.0(3) . . . ? C(11) N(1) C(13) 111.8(3) . . . ? C(11) N(2) C(12) 111.1(3) . . . ? C(11) N(2) C(14) 127.5(3) . . . ? C(12) N(2) C(14) 121.3(3) . . . ? C(1) N(3) C(5) 116.4(4) . . . ? N(1) C(1) N(3) 114.1(4) . . . ? N(1) C(1) C(2) 121.5(4) . . . ? N(3) C(1) C(2) 124.3(4) . . . ? C(1) C(2) C(3) 117.8(4) . . . ? C(1) C(2) H(4) 121.1 . . . no C(3) C(2) H(4) 121.1 . . . no C(2) C(3) C(4) 118.9(5) . . . ? C(2) C(3) H(5) 120.6 . . . no C(4) C(3) H(5) 120.6 . . . no C(3) C(4) C(5) 118.4(5) . . . ? C(3) C(4) H(6) 120.8 . . . no C(5) C(4) H(6) 120.8 . . . no N(3) C(5) C(4) 124.1(5) . . . ? N(3) C(5) H(7) 117.9 . . . no C(4) C(5) H(7) 117.9 . . . no Pd(1) C(11) N(1) 126.7(3) . . . ? Pd(1) C(11) N(2) 129.4(3) . . . ? N(1) C(11) N(2) 103.4(3) . . . ? N(2) C(12) C(13) 107.5(4) . . . ? N(2) C(12) H(8) 126.2 . . . no C(13) C(12) H(8) 126.2 . . . no N(1) C(13) C(12) 106.2(4) . . . ? N(1) C(13) H(9) 126.9 . . . no C(12) C(13) H(9) 126.9 . . . no N(2) C(14) C(15) 118.6(4) . . . ? N(2) C(14) C(19) 118.5(4) . . . ? C(15) C(14) C(19) 122.5(4) . . . ? C(14) C(15) C(16) 117.0(4) . . . ? C(14) C(15) C(20) 122.4(4) . . . ? C(16) C(15) C(20) 120.6(4) . . . ? C(15) C(16) C(17) 122.1(4) . . . ? C(15) C(16) H(10) 118.9 . . . no C(17) C(16) H(10) 118.9 . . . no C(16) C(17) C(18) 119.0(4) . . . ? C(16) C(17) C(22) 119.9(5) . . . ? C(18) C(17) C(22) 121.1(5) . . . ? C(17) C(18) C(19) 121.6(4) . . . ? C(17) C(18) H(11) 119.2 . . . no C(19) C(18) H(11) 119.2 . . . no C(14) C(19) C(18) 117.5(4) . . . ? C(14) C(19) C(29) 121.4(4) . . . ? C(18) C(19) C(29) 121.1(4) . . . ? C(15) C(20) H(3) 109.5 . . . no C(15) C(20) H(12) 109.5 . . . no C(15) C(20) H(13) 109.5 . . . no H(3) C(20) H(12) 109.5 . . . no H(3) C(20) H(13) 109.5 . . . no H(12) C(20) H(13) 109.5 . . . no C(17) C(22) H(2) 109.5 . . . no C(17) C(22) H(14) 109.5 . . . no C(17) C(22) H(15) 109.5 . . . no H(2) C(22) H(14) 109.5 . . . no H(2) C(22) H(15) 109.5 . . . no H(14) C(22) H(15) 109.5 . . . no C(19) C(29) H(1) 109.5 . . . no C(19) C(29) H(16) 109.5 . . . no C(19) C(29) H(17) 109.5 . . . no H(1) C(29) H(16) 109.5 . . . no H(1) C(29) H(17) 109.5 . . . no H(16) C(29) H(17) 109.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag N(3) C(13) 3.535(6) . 8 no C(5) C(5) 3.516(10) . 2 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Pd(1) C(11) N(1) C(1) . . . . 8.6(6) no Pd(1) C(11) N(1) C(13) . . . . -171.4(3) no Pd(1) C(11) N(2) C(12) . . . . 171.4(3) no Pd(1) C(11) N(2) C(14) . . . . -5.0(6) no Pd(1) C(11) N(1) C(1) . . . . -8.6(6) no Pd(1) C(11) N(1) C(13) . . . . 171.4(3) no Pd(1) C(11) N(2) C(12) . . . . -171.4(3) no Pd(1) C(11) N(2) C(14) . . . . 5.0(6) no Br(1) Pd(1) C(11) N(1) . . . . -104.7(3) no Br(1) Pd(1) C(11) N(2) . . . . 84.6(4) no Br(1) Pd(1) C(11) N(1) . . . . -75.3(3) no Br(1) Pd(1) C(11) N(2) . . . . 95.4(4) no N(1) C(1) N(3) C(5) . . . . -177.6(4) no N(1) C(1) C(2) C(3) . . . . 176.4(4) no N(1) C(11) Pd(1) C(11) . . . . 176.4(4) no N(1) C(11) N(2) C(12) . . . . -0.9(4) no N(1) C(11) N(2) C(14) . . . . -177.2(4) no N(1) C(13) C(12) N(2) . . . . 0.5(5) no N(2) C(11) Pd(1) C(11) . . . . 0.5(5) no N(2) C(11) N(1) C(1) . . . . -178.9(4) no N(2) C(11) N(1) C(13) . . . . 1.2(4) no N(2) C(14) C(15) C(16) . . . . -178.3(4) no N(2) C(14) C(15) C(20) . . . . -1.7(6) no N(2) C(14) C(19) C(18) . . . . 177.5(4) no N(2) C(14) C(19) C(29) . . . . 0.4(6) no N(3) C(1) N(1) C(11) . . . . -145.4(4) no N(3) C(1) N(1) C(13) . . . . 34.5(6) no N(3) C(1) C(2) C(3) . . . . -0.2(7) no N(3) C(5) C(4) C(3) . . . . -0.5(8) no C(1) N(1) C(13) C(12) . . . . 179.0(4) no C(1) N(3) C(5) C(4) . . . . 1.2(7) no C(1) C(2) C(3) C(4) . . . . 0.8(7) no C(2) C(1) N(1) C(11) . . . . 37.7(6) no C(2) C(1) N(1) C(13) . . . . -142.4(4) no C(2) C(1) N(3) C(5) . . . . -0.8(7) no C(2) C(3) C(4) C(5) . . . . -0.5(7) no C(11) N(1) C(13) C(12) . . . . -1.1(5) no C(11) N(2) C(12) C(13) . . . . 0.2(5) no C(11) N(2) C(14) C(15) . . . . -92.0(5) no C(11) N(2) C(14) C(19) . . . . 95.3(5) no C(12) N(2) C(14) C(15) . . . . 92.0(5) no C(12) N(2) C(14) C(19) . . . . -80.8(5) no C(13) C(12) N(2) C(14) . . . . 176.9(4) no C(14) C(15) C(16) C(17) . . . . 2.1(7) no C(14) C(19) C(18) C(17) . . . . -0.6(7) no C(15) C(14) C(19) C(18) . . . . 5.1(6) no C(15) C(14) C(19) C(29) . . . . -172.1(4) no C(15) C(16) C(17) C(18) . . . . 2.1(7) no C(15) C(16) C(17) C(22) . . . . -178.3(4) no C(16) C(15) C(14) C(19) . . . . -5.8(6) no C(16) C(17) C(18) C(19) . . . . -2.9(7) no C(17) C(16) C(15) C(20) . . . . -174.5(4) no C(17) C(18) C(19) C(29) . . . . 176.6(4) no C(19) C(14) C(15) C(20) . . . . 170.8(4) no C(19) C(18) C(17) C(22) . . . . 177.5(4) no #------------------------------------------------------------------------------ #===END #============================================================================== data__2135[Pd(K1K2NC)Br]Br_4 _database_code_CSD 175638 #============================================================================== _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'Denzo-SMN' _computing_data_reduction 'Denzo-SMN' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'teXsan for Windows v. 1.06 (MSC 1999)' _computing_publication_material 'teXsan for Windows v. 1.06 (MSC 1999)' #------------------------------------------------------------------------------ _cell_length_a 19.4495(5) _cell_length_b 9.6816(3) _cell_length_c 20.3347(5) _cell_angle_alpha 90 _cell_angle_beta 104.809(2) _cell_angle_gamma 90 _cell_volume 3701.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 183.2 _cell_measurement_reflns_used 26437 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.5 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1829.04 _chemical_formula_analytical ? _chemical_formula_sum 'C53 H66 Br4 Cl12 N12 Pd2 ' _chemical_formula_moiety '2(C22 H26 Br N6 Pd)), 4(C H Cl3), C5, 2(Br)' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1808.00 _exptl_absorpt_coefficient_mu 3.126 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min 0.598 _exptl_absorpt_correction_T_max 0.693 _exptl_special_details ; multi-scan from symmetry-related measurements (Blessing 1995) SORTAV R.H Blessing, Acta Cryst., A51, 33-37 (1995), J. Appl. Cryst., 30, 421-426 (1997). ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; disordered chloroforms, 1/2 pentane, no H included for pentane Z listed as 2 to provide integral numbers for pentane ; _diffrn_ambient_temperature 183.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 29122 _reflns_number_total 8927 _reflns_number_gt 4055 _reflns_threshold_expression I>5.00\s(I) _diffrn_reflns_av_R_equivalents 0.04760 _diffrn_reflns_av_sigmaI/netI 0.118 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 27.45 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 106 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 132 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Br 0 8 -0.374 2.456 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 24 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pd 0 4 -1.177 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 24 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pd(1) 0.97073(2) 0.08245(4) 0.76440(2) 0.03037(9) 1.000 . Uani d ? Br(1) 0.91909(2) -0.06855(6) 0.83679(3) 0.0449(2) 1.000 . Uani d ? Br(2) 1.15423(2) 0.43453(5) 0.51514(2) 0.0393(1) 1.000 . Uani d ? Cl(1) 0.8139(7) 0.196(2) 0.9206(7) 0.247(6) 0.500 S Uani d ? Cl(2) 0.6902(3) 0.3112(12) 0.8436(4) 0.107(2) 0.500 S Uani d ? Cl(3) 0.7700(6) 0.4513(7) 0.9602(4) 0.164(3) 0.500 S Uani d ? Cl(4) 0.5318(9) 0.0158(10) 0.5828(5) 0.269(7) 0.500 S Uani d ? Cl(5) 0.6006(3) 0.0144(8) 0.7225(5) 0.222(4) 0.500 S Uani d ? Cl(6) 0.4574(5) 0.0199(9) 0.6864(6) 0.166(4) 0.500 S Uani d ? Cl(7) 0.4483(3) 0.1131(6) 0.5780(3) 0.151(2) 0.500 S Uani d ? Cl(8) 0.4836(8) 0.0054(11) 0.7060(6) 0.215(5) 0.500 S Uani d ? Cl(9) 0.5770(4) -0.0371(10) 0.6289(6) 0.197(5) 0.500 S Uani d ? Cl(10) 0.7032(6) 0.3651(12) 0.8648(5) 0.164(4) 0.500 S Uani d ? Cl(11) 0.8019(6) 0.3917(9) 0.9968(5) 0.204(5) 0.500 S Uani d ? Cl(12) 0.8203(3) 0.1803(5) 0.9152(3) 0.071(2) 0.500 S Uani d ? N(1) 0.9480(2) 0.2709(4) 0.6564(2) 0.0388(11) 1.000 . Uani d ? N(2) 1.0613(2) 0.2433(4) 0.6814(2) 0.0452(12) 1.000 . Uani d ? N(3) 0.8743(2) 0.1765(4) 0.7152(2) 0.0354(11) 1.000 . Uani d ? N(4) 1.0965(2) -0.1113(4) 0.7867(2) 0.0361(11) 1.000 . Uani d ? N(5) 1.1068(2) 0.0371(4) 0.8672(2) 0.0375(11) 1.000 . Uani d ? N(6) 1.1292(2) -0.2349(5) 0.7024(2) 0.052(1) 1.000 . Uani d ? C(1) 0.8789(2) 0.2609(5) 0.6647(2) 0.039(1) 1.000 . Uani d ? C(2) 0.8218(2) 0.3308(6) 0.6245(3) 0.053(2) 1.000 . Uani d ? C(3) 0.7574(3) 0.3153(6) 0.6392(3) 0.062(2) 1.000 . Uani d ? C(4) 0.7518(2) 0.2318(7) 0.6920(3) 0.060(2) 1.000 . Uani d ? C(5) 0.8112(2) 0.1624(6) 0.7289(2) 0.048(2) 1.000 . Uani d ? C(11) 1.0035(2) 0.2033(5) 0.7003(2) 0.0344(13) 1.000 . Uani d ? C(12) 1.0435(3) 0.3326(6) 0.6265(3) 0.059(2) 1.000 . Uani d ? C(13) 0.9726(3) 0.3516(6) 0.6110(3) 0.053(2) 1.000 . Uani d ? C(14) 1.1365(2) 0.2070(6) 0.7143(3) 0.060(2) 1.000 . Uani d ? C(15) 1.1683(3) 0.1261(7) 0.6682(4) 0.083(2) 1.000 . Uani d ? C(16) 1.1776(3) 0.3392(8) 0.7382(3) 0.080(2) 1.000 . Uani d ? C(21) 1.0751(2) -0.1828(5) 0.7229(3) 0.040(1) 1.000 . Uani d ? C(22) 1.0049(3) -0.1947(5) 0.6878(3) 0.053(2) 1.000 . Uani d ? C(23) 0.9895(3) -0.2627(6) 0.6264(3) 0.070(2) 1.000 . Uani d ? C(24) 1.0450(4) -0.3147(6) 0.6024(3) 0.074(2) 1.000 . Uani d ? C(25) 1.1125(3) -0.3003(6) 0.6426(3) 0.067(2) 1.000 . Uani d ? C(31) 1.0638(2) -0.0008(5) 0.8073(2) 0.0340(13) 1.000 . Uani d ? C(32) 1.1663(2) -0.0471(6) 0.8844(3) 0.053(2) 1.000 . Uani d ? C(33) 1.1601(2) -0.1385(6) 0.8342(3) 0.053(2) 1.000 . Uani d ? C(34) 1.0934(3) 0.1554(6) 0.9092(3) 0.052(2) 1.000 . Uani d ? C(35) 1.1581(3) 0.2471(7) 0.9275(3) 0.078(2) 1.000 . Uani d ? C(36) 1.0726(4) 0.1038(7) 0.9714(3) 0.084(2) 1.000 . Uani d ? C(41) 1.0316(10) 0.018(2) 0.5228(8) 0.101(5) 0.500 S Uiso d ? C(42) 0.950(3) 0.010(7) 0.508(3) 0.38(2) 0.500 S Uiso d ? C(43) 0.9069(8) 0.035(2) 0.5191(8) 0.085(4) 0.500 S Uiso d ? C(44) 0.843(2) 0.079(3) 0.480(1) 0.200(10) 0.500 S Uiso d ? C(45) 0.829(2) -0.008(4) 0.535(2) 0.258(11) 0.500 S Uiso d ? C(46) 0.5247(4) 0.0751(7) 0.6532(4) 0.099(3) 1.000 . Uani d ? C(47) 0.7467(4) 0.2888(8) 0.9280(4) 0.100(3) 1.000 . Uani d ? H(2) 1.1472 0.3288 0.9487 0.094 1.000 . Uiso c ? H(4) 1.0324 0.0450 0.9579 0.101 1.000 . Uiso c ? H(5) 1.1441 0.0404 0.6583 0.099 1.000 . Uiso c ? H(6) 1.1856 0.3871 0.7001 0.096 1.000 . Uiso c ? H(1) 0.8269 0.3878 0.5880 0.064 1.000 . Uiso c ? H(3) 0.7167 0.3621 0.6129 0.075 1.000 . Uiso c ? H(7) 0.7075 0.2219 0.7032 0.072 1.000 . Uiso c ? H(8) 0.8071 0.1032 0.7649 0.058 1.000 . Uiso c ? H(9) 1.0756 0.3731 0.6038 0.071 1.000 . Uiso c ? H(10) 0.9451 0.4089 0.5762 0.063 1.000 . Uiso c ? H(11) 1.1373 0.1519 0.7532 0.072 1.000 . Uiso c ? H(12) 1.1642 0.1761 0.6271 0.099 1.000 . Uiso c ? H(13) 1.2171 0.1098 0.6893 0.099 1.000 . Uiso c ? H(14) 1.2219 0.3171 0.7688 0.096 1.000 . Uiso c ? H(15) 1.1508 0.3961 0.7606 0.096 1.000 . Uiso c ? H(16) 0.9681 -0.1572 0.7054 0.063 1.000 . Uiso c ? H(17) 0.9416 -0.2739 0.6009 0.084 1.000 . Uiso c ? H(18) 1.0363 -0.3592 0.5593 0.088 1.000 . Uiso c ? H(19) 1.1502 -0.3393 0.6269 0.080 1.000 . Uiso c ? H(20) 1.2042 -0.0408 0.9244 0.064 1.000 . Uiso c ? H(21) 1.1931 -0.2091 0.8315 0.064 1.000 . Uiso c ? H(22) 1.0549 0.2078 0.8827 0.062 1.000 . Uiso c ? H(23) 1.1959 0.1995 0.9579 0.094 1.000 . Uiso c ? H(24) 1.1720 0.2707 0.8874 0.094 1.000 . Uiso c ? H(25) 1.0613 0.1800 0.9961 0.101 1.000 . Uiso c ? H(26) 1.1111 0.0537 0.9994 0.101 1.000 . Uiso c ? H(27) 0.5249 0.1732 0.6515 0.119 1.000 . Uiso c ? H(28) 0.7214 0.2417 0.9555 0.120 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.0197(2) 0.0408(2) 0.0304(2) 0.0024(2) 0.00612(13) 0.0051(2) Br(1) 0.0334(3) 0.0536(4) 0.0516(3) 0.0020(2) 0.0184(2) 0.0142(3) Br(2) 0.0288(2) 0.0558(3) 0.0323(3) 0.0021(2) 0.0057(2) 0.0028(2) Cl(1) 0.143(8) 0.36(2) 0.248(12) 0.082(9) 0.081(8) 0.141(11) Cl(2) 0.055(2) 0.199(9) 0.069(3) 0.023(3) 0.017(2) 0.009(4) Cl(3) 0.240(8) 0.085(5) 0.153(7) -0.035(5) 0.025(6) -0.033(4) Cl(4) 0.52(2) 0.180(9) 0.177(9) -0.042(12) 0.216(12) -0.053(7) Cl(5) 0.134(5) 0.166(6) 0.339(11) -0.013(4) 0.011(6) 0.161(7) Cl(6) 0.142(5) 0.103(5) 0.303(13) -0.052(4) 0.146(7) -0.099(7) Cl(7) 0.155(5) 0.139(5) 0.131(4) -0.016(4) -0.015(4) -0.000(4) Cl(8) 0.41(2) 0.122(6) 0.148(6) -0.022(9) 0.143(10) 0.043(5) Cl(9) 0.145(6) 0.196(9) 0.287(13) 0.049(5) 0.123(8) -0.026(8) Cl(10) 0.188(9) 0.186(10) 0.135(8) 0.076(7) 0.073(6) 0.096(8) Cl(11) 0.30(1) 0.143(8) 0.163(8) -0.109(8) 0.052(8) -0.015(5) Cl(12) 0.067(3) 0.068(3) 0.084(3) 0.013(2) 0.030(3) 0.018(2) N(1) 0.028(2) 0.054(3) 0.036(2) 0.007(2) 0.010(2) 0.014(2) N(2) 0.025(2) 0.063(3) 0.051(3) 0.009(2) 0.015(2) 0.024(2) N(3) 0.023(2) 0.051(3) 0.034(2) 0.007(2) 0.010(2) 0.002(2) N(4) 0.023(2) 0.043(3) 0.041(2) 0.005(2) 0.006(2) 0.004(2) N(5) 0.023(2) 0.051(3) 0.034(2) -0.000(2) -0.000(2) 0.006(2) N(6) 0.043(2) 0.054(3) 0.064(3) 0.004(2) 0.024(2) -0.008(3) C(1) 0.027(2) 0.054(3) 0.039(3) 0.008(2) 0.013(2) 0.008(3) C(2) 0.034(3) 0.079(4) 0.045(3) 0.017(3) 0.009(2) 0.026(3) C(3) 0.032(3) 0.096(5) 0.056(4) 0.029(3) 0.006(3) 0.024(3) C(4) 0.026(2) 0.092(5) 0.064(4) 0.020(3) 0.015(3) 0.020(3) C(5) 0.028(2) 0.069(4) 0.049(3) 0.009(3) 0.015(2) 0.014(3) C(11) 0.026(2) 0.046(3) 0.034(3) 0.000(2) 0.012(2) 0.006(2) C(12) 0.041(3) 0.085(5) 0.058(4) 0.010(3) 0.026(3) 0.031(3) C(13) 0.040(3) 0.074(4) 0.045(3) 0.015(3) 0.013(2) 0.027(3) C(14) 0.024(2) 0.082(4) 0.075(4) 0.010(3) 0.015(3) 0.047(3) C(15) 0.042(3) 0.077(5) 0.141(6) 0.023(3) 0.047(4) 0.042(4) C(16) 0.033(3) 0.117(6) 0.091(5) 0.006(3) 0.016(3) 0.023(4) C(21) 0.037(3) 0.033(3) 0.052(3) -0.000(2) 0.011(2) 0.001(2) C(22) 0.042(3) 0.053(4) 0.060(4) 0.002(3) 0.008(3) -0.017(3) C(23) 0.059(4) 0.067(4) 0.077(4) -0.006(3) 0.004(3) -0.027(4) C(24) 0.081(5) 0.065(5) 0.074(4) -0.002(4) 0.017(4) -0.032(4) C(25) 0.075(4) 0.056(4) 0.080(5) 0.006(3) 0.039(4) -0.013(3) C(31) 0.027(2) 0.044(3) 0.032(3) -0.003(2) 0.009(2) 0.007(2) C(32) 0.030(3) 0.079(4) 0.046(3) 0.008(3) 0.001(2) 0.012(3) C(33) 0.027(3) 0.071(4) 0.058(4) 0.020(3) 0.006(2) 0.016(3) C(34) 0.051(3) 0.063(4) 0.036(3) -0.001(3) 0.000(2) -0.008(3) C(35) 0.085(4) 0.078(5) 0.067(4) -0.023(4) 0.010(3) -0.020(4) C(36) 0.099(5) 0.110(6) 0.048(4) -0.023(4) 0.026(3) -0.023(4) C(46) 0.127(7) 0.058(5) 0.125(7) -0.017(4) 0.054(6) -0.011(4) C(47) 0.110(6) 0.081(5) 0.118(7) -0.013(5) 0.043(5) 0.007(5) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4055 _refine_ls_number_parameters 426 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.031 _refine_ls_wR_factor_all 0.0540 _refine_ls_wR_factor_ref 0.041 _refine_ls_goodness_of_fit_all 1.049 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.41 _refine_diff_density_max 0.57 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag PD1 BR1 2.4633(6) . . ? PD1 N3 2.094(4) . . ? PD1 C11 1.974(5) . . ? PD1 C31 1.970(5) . . ? CL1 CL12 0.24(2) . . ? CL1 C47 1.62(2) . . ? CL2 CL10 0.68(2) . . ? CL2 C47 1.798(12) . . ? CL3 CL10 2.21(1) . . ? CL3 CL11 1.017(11) . . ? CL3 C45 2.00(4) . . ? CL3 C47 1.720(11) . . ? CL4 CL7 1.86(2) . . ? CL4 CL9 1.22(1) . . ? CL4 C46 1.582(11) . . ? CL5 CL8 2.22(2) . . ? CL5 CL9 1.91(1) . . ? CL5 C46 1.856(11) . . ? CL6 CL7 2.347(13) . . ? CL6 CL8 0.58(2) . . ? CL6 C46 1.705(11) . . ? CL7 C46 1.876(10) . . ? CL8 C46 1.639(12) . . ? CL9 C46 1.649(11) . . ? CL10 C47 1.535(13) . . ? CL11 C47 1.827(13) . . ? CL12 C47 1.849(11) . . ? N1 C1 1.399(5) . . ? N1 C11 1.378(5) . . ? N1 C13 1.385(6) . . ? N2 C11 1.335(5) . . ? N2 C12 1.385(6) . . ? N2 C14 1.487(6) . . ? N3 C1 1.334(6) . . ? N3 C5 1.333(6) . . ? N4 C21 1.435(6) . . ? N4 C31 1.364(6) . . ? N4 C33 1.386(6) . . ? N5 C31 1.341(6) . . ? N5 C32 1.385(6) . . ? N5 C34 1.490(7) . . ? N6 C21 1.327(6) . . ? N6 C25 1.336(7) . . ? C1 C2 1.376(6) . . ? C2 C3 1.369(7) . . ? C2 H1 0.95 . . no C3 C4 1.371(8) . . ? C3 H3 0.95 . . no C4 C5 1.381(7) . . ? C4 H7 0.95 . . no C5 H8 0.95 . . no C12 C13 1.346(7) . . ? C12 H9 0.95 . . no C13 H10 0.95 . . no C14 C15 1.473(9) . . ? C14 C16 1.521(9) . . ? C14 H11 0.95 . . no C15 H5 0.95 . . no C15 H12 0.95 . . no C15 H13 0.95 . . no C16 H6 0.95 . . no C16 H14 0.95 . . no C16 H15 0.95 . . no C21 C22 1.374(7) . . ? C22 C23 1.375(7) . . ? C22 H16 0.95 . . no C23 C24 1.388(8) . . ? C23 H17 0.95 . . no C24 C25 1.365(9) . . ? C24 H18 0.95 . . no C25 H19 0.95 . . no C32 C33 1.333(8) . . ? C32 H20 0.95 . . no C33 H21 0.95 . . no C34 C35 1.507(8) . . ? C34 C36 1.507(8) . . ? C34 H22 0.95 . . no C35 H2 0.95 . . no C35 H23 0.95 . . no C35 H24 0.95 . . no C36 H4 0.95 . . no C36 H25 0.95 . . no C36 H26 0.95 . . no C41 C41 1.38(4) . . ? C41 C42 1.54(5) . . ? C41 C42 0.84(6) . . ? C41 C43 1.71(3) . . ? C42 C43 0.95(5) . . ? C43 C44 1.36(3) . . ? C43 C45 1.67(4) . . ? C44 C45 1.47(4) . . ? C46 H27 0.95 . . no C47 H28 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag BR1 PD1 N3 95.25(11) . . . ? BR1 PD1 C11 174.76(13) . . . ? BR1 PD1 C31 87.76(13) . . . ? N3 PD1 C11 80.1(2) . . . ? N3 PD1 C31 177.0(2) . . . ? C11 PD1 C31 96.9(2) . . . ? CL12 CL1 C47 156.3(55) . . . ? CL10 CL2 C47 56.8(15) . . . ? CL10 CL3 CL11 122.8(11) . . . ? CL10 CL3 C45 76.1(12) . . . ? CL10 CL3 C47 43.9(5) . . . ? CL11 CL3 C45 119.4(18) . . . ? CL11 CL3 C47 79.2(9) . . . ? C45 CL3 C47 92.1(12) 2_656 2_656 2_656 ? CL7 CL4 CL9 134.5(9) . . . ? CL7 CL4 C46 65.5(6) . . . ? CL9 CL4 C46 70.7(8) . . . ? CL8 CL5 CL9 82.1(5) . . . ? CL8 CL5 C46 46.4(4) . . . ? CL9 CL5 C46 52.0(4) . . . ? CL7 CL6 CL8 125.6(18) . . . ? CL7 CL6 C46 52.3(5) . . . ? CL8 CL6 C46 73.6(16) . . . ? CL4 CL7 CL6 84.3(4) . . . ? CL4 CL7 C46 50.1(4) . . . ? CL6 CL7 C46 46.0(4) . . . ? CL5 CL8 CL6 141.7(19) . . . ? CL5 CL8 C46 55.1(6) . . . ? CL6 CL8 C46 86.6(17) . . . ? CL4 CL9 CL5 126.8(9) . . . ? CL4 CL9 C46 64.9(6) . . . ? CL5 CL9 C46 62.4(5) . . . ? CL2 CL10 CL3 152.1(20) . . . ? CL2 CL10 C47 101.3(20) . . . ? CL3 CL10 C47 51.0(5) . . . ? CL3 CL11 C47 67.6(9) . . . ? CL1 CL12 C47 20.7(48) . . . ? C1 N1 C11 120.5(4) . . . ? C1 N1 C13 128.7(4) . . . ? C11 N1 C13 110.6(4) . . . ? C11 N2 C12 111.0(4) . . . ? C11 N2 C14 127.3(4) . . . ? C12 N2 C14 121.6(4) . . . ? PD1 N3 C1 114.0(3) . . . ? PD1 N3 C5 128.0(3) . . . ? C1 N3 C5 118.0(4) . . . ? C21 N4 C31 127.3(4) . . . ? C21 N4 C33 122.7(4) . . . ? C31 N4 C33 109.7(4) . . . ? C31 N5 C32 110.8(5) . . . ? C31 N5 C34 124.8(4) . . . ? C32 N5 C34 124.4(4) . . . ? C21 N6 C25 116.0(5) . . . ? N1 C1 N3 112.9(4) . . . ? N1 C1 C2 123.2(5) . . . ? N3 C1 C2 123.8(4) . . . ? C1 C2 C3 117.4(5) . . . ? C1 C2 H1 121.3 . . . no C3 C2 H1 121.2 . . . no C2 C3 C4 119.8(5) . . . ? C2 C3 H3 120.2 . . . no C4 C3 H3 120.0 . . . no C3 C4 C5 119.2(5) . . . ? C3 C4 H7 120.4 . . . no C5 C4 H7 120.4 . . . no N3 C5 C4 121.7(5) . . . ? N3 C5 H8 119.2 . . . no C4 C5 H8 119.2 . . . no PD1 C11 N1 112.2(3) . . . ? PD1 C11 N2 143.1(4) . . . ? N1 C11 N2 104.7(4) . . . ? N2 C12 C13 107.6(4) . . . ? N2 C12 H9 126.2 . . . no C13 C12 H9 126.2 . . . no N1 C13 C12 106.0(4) . . . ? N1 C13 H10 127.0 . . . no C12 C13 H10 127.0 . . . no N2 C14 C15 111.3(5) . . . ? N2 C14 C16 108.7(5) . . . ? N2 C14 H11 108.1 . . . no C15 C14 C16 112.3(5) . . . ? C15 C14 H11 108.1 . . . no C16 C14 H11 108.1 . . . no C14 C15 H5 109.5 . . . no C14 C15 H12 109.5 . . . no C14 C15 H13 109.5 . . . no H5 C15 H12 109.5 . . . no H5 C15 H13 109.5 . . . no H12 C15 H13 109.4 . . . no C14 C16 H6 109.4 . . . no C14 C16 H14 109.5 . . . no C14 C16 H15 109.4 . . . no H6 C16 H14 109.5 . . . no H6 C16 H15 109.4 . . . no H14 C16 H15 109.5 . . . no N4 C21 N6 113.4(4) . . . ? N4 C21 C22 122.1(5) . . . ? N6 C21 C22 124.5(5) . . . ? C21 C22 C23 118.0(5) . . . ? C21 C22 H16 121.0 . . . no C23 C22 H16 121.0 . . . no C22 C23 C24 119.0(5) . . . ? C22 C23 H17 120.5 . . . no C24 C23 H17 120.5 . . . no C23 C24 C25 117.8(6) . . . ? C23 C24 H18 121.1 . . . no C25 C24 H18 121.1 . . . no N6 C25 C24 124.6(6) . . . ? N6 C25 H19 117.7 . . . no C24 C25 H19 117.7 . . . no PD1 C31 N4 129.2(3) . . . ? PD1 C31 N5 125.4(4) . . . ? N4 C31 N5 105.2(4) . . . ? N5 C32 C33 106.9(4) . . . ? N5 C32 H20 126.5 . . . no C33 C32 H20 126.5 . . . no N4 C33 C32 107.3(5) . . . ? N4 C33 H21 126.3 . . . no C32 C33 H21 126.3 . . . no N5 C34 C35 109.6(5) . . . ? N5 C34 C36 110.5(5) . . . ? N5 C34 H22 108.3 . . . no C35 C34 C36 112.0(5) . . . ? C35 C34 H22 108.2 . . . no C36 C34 H22 108.2 . . . no C34 C35 H2 109.5 . . . no C34 C35 H23 109.4 . . . no C34 C35 H24 109.5 . . . no H2 C35 H23 109.4 . . . no H2 C35 H24 109.5 . . . no H23 C35 H24 109.5 . . . no C34 C36 H4 109.4 . . . no C34 C36 H25 109.5 . . . no C34 C36 H26 109.4 . . . no H4 C36 H25 109.5 . . . no H4 C36 H26 109.5 . . . no H25 C36 H26 109.5 . . . no C41 C41 C42 32.8(23) 3_756 3_756 3_756 ? C41 C41 C42 84.0(51) 3_756 3_756 3_756 ? C41 C41 C43 101.8(19) 3_756 3_756 3_756 ? C42 C41 C42 116.8(45) . . . ? C42 C41 C43 134.6(28) . . . ? C42 C41 C43 18.3(53) 3_756 3_756 3_756 ? C41 C42 C41 63.2(45) . . . ? C41 C42 C43 149.7(71) . . . ? C41 C42 C43 145.6(97) 3_756 3_756 3_756 ? C41 C43 C42 16.1(46) 3_756 3_756 3_756 ? C41 C43 C44 117.0(18) 3_756 3_756 3_756 ? C41 C43 C45 142.8(17) 3_756 3_756 3_756 ? C42 C43 C44 132.1(50) . . . ? C42 C43 C45 150.3(51) . . . ? C44 C43 C45 57.0(16) . . . ? C43 C44 C45 72.4(22) . . . ? CL3 C45 C43 171.5(26) 2_646 2_646 2_646 ? CL3 C45 C44 121.1(27) 2_646 2_646 2_646 ? C43 C45 C44 50.6(19) . . . ? CL4 C46 CL5 109.6(8) . . . ? CL4 C46 CL6 119.9(8) . . . ? CL4 C46 CL7 64.3(7) . . . ? CL4 C46 CL8 127.8(8) . . . ? CL4 C46 CL9 44.4(6) . . . ? CL4 C46 H27 109.0 . . . no CL5 C46 CL6 98.2(6) . . . ? CL5 C46 CL7 172.3(6) . . . ? CL5 C46 CL8 78.4(7) . . . ? CL5 C46 CL9 65.6(6) . . . ? CL5 C46 H27 109.6 . . . no CL6 C46 CL7 81.7(6) . . . ? CL6 C46 CL8 19.8(8) . . . ? CL6 C46 CL9 120.5(7) . . . ? CL6 C46 H27 109.9 . . . no CL7 C46 CL8 101.4(7) . . . ? CL7 C46 CL9 107.8(7) . . . ? CL7 C46 H27 77.5 . . . no CL8 C46 CL9 111.5(8) . . . ? CL8 C46 H27 116.4 . . . no CL9 C46 H27 129.6 . . . no CL1 C47 CL2 106.7(8) . . . ? CL1 C47 CL3 113.5(9) . . . ? CL1 C47 CL10 118.2(9) . . . ? CL1 C47 CL11 92.4(9) . . . ? CL1 C47 CL12 3.0(8) . . . ? CL1 C47 H28 109.8 . . . no CL2 C47 CL3 106.9(6) . . . ? CL2 C47 CL10 21.9(8) . . . ? CL2 C47 CL11 139.6(7) . . . ? CL2 C47 CL12 103.9(6) . . . ? CL2 C47 H28 109.8 . . . no CL3 C47 CL10 85.1(7) . . . ? CL3 C47 CL11 33.1(4) . . . ? CL3 C47 CL12 115.8(6) . . . ? CL3 C47 H28 109.8 . . . no CL10 C47 CL11 118.0(8) . . . ? CL10 C47 CL12 115.9(7) . . . ? CL10 C47 H28 117.9 . . . no CL11 C47 CL12 95.3(6) . . . ? CL11 C47 H28 95.8 . . . no CL12 C47 H28 110.2 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag N1 C43 3.54(2) . . no C12 C24 3.450(9) . 1_565 no C13 C24 3.546(9) . 1_565 no C15 C44 3.57(3) . 3_756 no C15 C41 3.59(2) . . no C23 C42 3.52(7) . . no C24 C41 3.58(2) . . no C25 C44 3.56(3) . 3_756 no C45 C47 2.68(4) . 2_646 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag PD1 N3 C1 N1 . . . . -1.4(6) no PD1 N3 C1 C2 . . . . 178.4(5) no PD1 N3 C5 C4 . . . . 179.7(4) no PD1 C11 N1 C1 . . . . 6.4(6) no PD1 C11 N1 C13 . . . . -178.3(4) no PD1 C11 N2 C12 . . . . 176.7(5) no PD1 C11 N2 C14 . . . . -6.2(10) no PD1 C31 N4 C21 . . . . 9.5(7) no PD1 C31 N4 C33 . . . . -177.0(4) no PD1 C31 N5 C32 . . . . 176.8(4) no PD1 C31 N5 C34 . . . . -4.3(7) no BR1 PD1 N3 C1 . . . . -173.9(3) no BR1 PD1 N3 C5 . . . . 6.8(5) no BR1 PD1 C11 N1 . . . . 22.2(18) no BR1 PD1 C11 N2 . . . . -155.1(11) no BR1 PD1 C31 N4 . . . . 92.7(4) no BR1 PD1 C31 N5 . . . . -82.8(4) no CL1 CL12 C47 CL2 . . . . 159(13) no CL1 CL12 C47 CL3 . . . . 43(13) no CL1 CL12 C47 CL10 . . . . 140(13) no CL1 CL12 C47 CL11 . . . . 15(13) no CL1 C47 CL2 CL10 . . . . -125.2(18) no CL1 C47 CL3 CL10 . . . . 118.7(10) no CL1 C47 CL3 CL11 . . . . -54.4(15) no CL1 C47 CL3 C45 . . . . -173.9(13) no CL1 C47 CL10 CL2 . . . . 62.6(19) no CL1 C47 CL10 CL3 . . . . -114.2(10) no CL1 C47 CL11 CL3 . . . . 131.8(14) no CL2 CL10 CL3 CL11 . . . . 1.4(46) no CL2 CL10 CL3 C45 . . . . -114.8(40) no CL2 CL10 CL3 C47 . . . . -6.7(37) no CL2 CL10 C47 CL3 . . . . 176.8(17) no CL2 CL10 C47 CL11 . . . . 172.5(16) no CL2 CL10 C47 CL12 . . . . 60.5(18) no CL2 C47 CL1 CL12 . . . . -21(13) no CL2 C47 CL3 CL10 . . . . 1.2(7) no CL2 C47 CL3 CL11 . . . . -171.8(12) no CL2 C47 CL3 C45 . . . . 68.7(12) no CL2 C47 CL10 CL3 . . . . -176.8(17) no CL2 C47 CL11 CL3 . . . . 12.1(18) no CL3 CL10 CL2 C47 . . . . 5.3(29) no CL3 CL10 C47 CL11 . . . . -4.3(9) no CL3 CL10 C47 CL12 . . . . -116.3(8) no CL3 CL11 C47 CL10 . . . . 7.9(16) no CL3 CL11 C47 CL12 . . . . 131.0(13) no CL3 C45 C43 C41 . . . . -79(17) no CL3 C45 C43 C42 . . . . -105(18) no CL3 C45 C43 C44 . . . . 14(16) no CL3 C45 C44 C43 . . . . -177.7(27) no CL3 C47 CL1 CL12 . . . . -138(13) no CL3 C47 CL2 CL10 . . . . -3.3(18) no CL4 CL7 CL6 CL8 . . . . 29.2(27) no CL4 CL7 CL6 C46 . . . . 36.9(5) no CL4 CL7 C46 CL5 . . . . -39.0(43) no CL4 CL7 C46 CL6 . . . . -128.9(7) no CL4 CL7 C46 CL8 . . . . -126.7(8) no CL4 CL7 C46 CL9 . . . . -9.5(8) no CL4 CL9 CL5 CL8 . . . . 48.3(14) no CL4 CL9 CL5 C46 . . . . 9.1(13) no CL4 CL9 C46 CL5 . . . . -171.9(11) no CL4 CL9 C46 CL6 . . . . 103.0(13) no CL4 CL9 C46 CL7 . . . . 12.2(11) no CL4 CL9 C46 CL8 . . . . 122.6(12) no CL4 C46 CL5 CL8 . . . . -126.3(8) no CL4 C46 CL5 CL9 . . . . -6.0(8) no CL4 C46 CL6 CL7 . . . . -53.9(8) no CL4 C46 CL6 CL8 . . . . 119.6(22) no CL4 C46 CL7 CL6 . . . . 128.9(7) no CL4 C46 CL8 CL5 . . . . 106.0(12) no CL4 C46 CL8 CL6 . . . . -72.7(24) no CL4 C46 CL9 CL5 . . . . 171.9(11) no CL5 CL8 CL6 CL7 . . . . 4.6(48) no CL5 CL8 CL6 C46 . . . . -1.7(28) no CL5 CL8 C46 CL6 . . . . 178.7(22) no CL5 CL8 C46 CL7 . . . . 172.2(6) no CL5 CL8 C46 CL9 . . . . 57.7(7) no CL5 CL9 CL4 CL7 . . . . -25.5(25) no CL5 CL9 CL4 C46 . . . . -8.9(12) no CL5 CL9 C46 CL6 . . . . -85.1(8) no CL5 CL9 C46 CL7 . . . . -175.9(5) no CL5 CL9 C46 CL8 . . . . -65.4(8) no CL5 C46 CL4 CL7 . . . . 174.9(5) no CL5 C46 CL4 CL9 . . . . 7.8(11) no CL5 C46 CL6 CL7 . . . . -172.2(6) no CL5 C46 CL6 CL8 . . . . 1.3(21) no CL5 C46 CL7 CL6 . . . . 89.9(44) no CL5 C46 CL8 CL6 . . . . -178.7(22) no CL6 CL7 CL4 CL9 . . . . -17.0(17) no CL6 CL7 CL4 C46 . . . . -34.2(5) no CL6 CL7 C46 CL8 . . . . 2.2(7) no CL6 CL7 C46 CL9 . . . . 119.5(7) no CL6 CL8 CL5 CL9 . . . . -41.3(37) no CL6 CL8 CL5 C46 . . . . 2.1(35) no CL6 CL8 C46 CL7 . . . . -6.5(21) no CL6 CL8 C46 CL9 . . . . -121.0(20) no CL6 C46 CL4 CL7 . . . . 62.6(8) no CL6 C46 CL4 CL9 . . . . -104.5(12) no CL6 C46 CL5 CL8 . . . . -0.4(7) no CL6 C46 CL5 CL9 . . . . 119.8(6) no CL7 CL4 CL9 C46 . . . . -16.6(14) no CL7 CL4 C46 CL8 . . . . 84.5(11) no CL7 CL4 C46 CL9 . . . . 167.1(11) no CL7 CL6 CL8 C46 . . . . 6.3(20) no CL7 CL6 C46 CL8 . . . . -173.5(21) no CL7 CL6 C46 CL9 . . . . -105.8(9) no CL7 C46 CL4 CL9 . . . . -167.1(11) no CL7 C46 CL5 CL8 . . . . -89.2(44) no CL7 C46 CL5 CL9 . . . . 31.0(43) no CL7 C46 CL6 CL8 . . . . 173.5(21) no CL8 CL5 CL9 C46 . . . . 39.2(5) no CL8 CL5 C46 CL9 . . . . -120.3(7) no CL8 CL6 CL7 C46 . . . . -7.7(25) no CL8 CL6 C46 CL9 . . . . 67.7(22) no CL8 C46 CL4 CL9 . . . . -82.6(15) no CL8 C46 CL5 CL9 . . . . 120.3(7) no CL9 CL4 CL7 C46 . . . . 17.2(15) no CL9 CL5 CL8 C46 . . . . -43.4(5) no CL10 CL2 C47 CL11 . . . . -10.2(21) no CL10 CL2 C47 CL12 . . . . -126.3(17) no CL10 CL3 CL11 C47 . . . . -5.7(11) no CL10 CL3 C45 C43 . . . . 175(17) no CL10 CL3 C45 C44 . . . . -172.5(31) no CL10 CL3 C47 CL11 . . . . 173.0(14) no CL10 CL3 C47 CL12 . . . . 116.5(8) no CL10 C47 CL1 CL12 . . . . -41(13) no CL10 C47 CL3 CL11 . . . . -173.0(14) no CL10 C47 CL3 C45 . . . . 67.4(12) no CL11 CL3 CL10 C47 . . . . 8.1(16) no CL11 CL3 C45 C43 . . . . 55(17) no CL11 CL3 C45 C44 . . . . 67.4(33) no CL11 CL3 C47 CL12 . . . . -56.6(14) no CL11 C47 CL1 CL12 . . . . -165(13) no CL11 C47 CL3 C45 . . . . -119.5(18) no CL12 C47 CL3 C45 . . . . -176.1(12) no N1 C1 N3 C5 . . . . 178.0(5) no N1 C1 C2 C3 . . . . -178.0(5) no N1 C11 PD1 N3 . . . . -5.1(3) no N1 C11 PD1 C31 . . . . 174.7(4) no N1 C11 N2 C12 . . . . -0.7(6) no N1 C11 N2 C14 . . . . 176.4(5) no N1 C13 C12 N2 . . . . -1.1(7) no N2 C11 PD1 N3 . . . . 177.6(7) no N2 C11 PD1 C31 . . . . -2.6(7) no N2 C11 N1 C1 . . . . -175.3(5) no N2 C11 N1 C13 . . . . 0.0(6) no N3 PD1 C31 N4 . . . . -80.4(35) no N3 PD1 C31 N5 . . . . 104.1(34) no N3 C1 N1 C11 . . . . -3.3(7) no N3 C1 N1 C13 . . . . -177.7(5) no N3 C1 C2 C3 . . . . 2.2(9) no N3 C5 C4 C3 . . . . 1.2(10) no N4 C21 N6 C25 . . . . -178.7(5) no N4 C21 C22 C23 . . . . 178.7(5) no N4 C31 PD1 C11 . . . . -84.9(4) no N4 C31 N5 C32 . . . . 0.4(5) no N4 C31 N5 C34 . . . . 179.4(4) no N4 C33 C32 N5 . . . . -0.7(6) no N5 C31 PD1 C11 . . . . 99.7(4) no N5 C31 N4 C21 . . . . -174.3(4) no N5 C31 N4 C33 . . . . -0.8(5) no N6 C21 N4 C31 . . . . 148.7(5) no N6 C21 N4 C33 . . . . -24.1(7) no N6 C21 C22 C23 . . . . -1.4(9) no N6 C25 C24 C23 . . . . -2.7(11) no C1 N1 C13 C12 . . . . 175.5(5) no C1 N3 PD1 C11 . . . . 3.7(4) no C1 N3 PD1 C31 . . . . -0.8(36) no C1 N3 C5 C4 . . . . 0.4(8) no C1 C2 C3 C4 . . . . -0.5(10) no C2 C1 N1 C11 . . . . 177.0(5) no C2 C1 N1 C13 . . . . 2.6(9) no C2 C1 N3 C5 . . . . -2.2(8) no C2 C3 C4 C5 . . . . -1.2(10) no C5 N3 PD1 C11 . . . . -175.7(5) no C5 N3 PD1 C31 . . . . 179.9(33) no C11 N1 C13 C12 . . . . 0.7(7) no C11 N2 C12 C13 . . . . 1.1(7) no C11 N2 C14 C15 . . . . 116.4(6) no C11 N2 C14 C16 . . . . -119.4(6) no C12 N2 C14 C15 . . . . -66.7(7) no C12 N2 C14 C16 . . . . 57.5(7) no C13 C12 N2 C14 . . . . -176.2(6) no C21 N4 C33 C32 . . . . 174.8(5) no C21 N6 C25 C24 . . . . 0.7(10) no C21 C22 C23 C24 . . . . -0.7(10) no C22 C21 N4 C31 . . . . -31.4(8) no C22 C21 N4 C33 . . . . 155.8(5) no C22 C21 N6 C25 . . . . 1.4(8) no C22 C23 C24 C25 . . . . 2.5(11) no C31 N4 C33 C32 . . . . 1.0(6) no C31 N5 C32 C33 . . . . 0.2(6) no C31 N5 C34 C35 . . . . -128.5(5) no C31 N5 C34 C36 . . . . 107.6(6) no C32 N5 C34 C35 . . . . 50.3(7) no C32 N5 C34 C36 . . . . -73.5(7) no C33 C32 N5 C34 . . . . -178.8(5) no C41 C41 C42 C43 . . . . 167(16) no C41 C41 C42 C43 . . . . 165(17) no C41 C41 C43 C42 . . . . -13(16) no C41 C41 C43 C44 . . . . 148.4(23) no C41 C41 C43 C45 . . . . -141.5(32) no C41 C42 C41 C42 . . . . 0.0000 no C41 C42 C41 C43 . . . . -167(16) no C41 C42 C43 C44 . . . . 134.2(98) no C41 C42 C43 C45 . . . . -130(10) no C41 C42 C41 C42 . . . . 0.0000 no C41 C42 C41 C43 . . . . 5.8(68) no C41 C42 C43 C44 . . . . 22(20) no C41 C42 C43 C45 . . . . -74(20) no C41 C43 C44 C45 . . . . -137.4(21) no C41 C43 C45 C44 . . . . 92.2(33) no C42 C41 C41 C42 . . . . 180.0000 no C42 C41 C41 C43 . . . . 4.2(50) no C42 C41 C42 C41 . . . . 0.0000 no C42 C41 C42 C43 . . . . -167(16) no C42 C41 C43 C44 . . . . -145.2(35) no C42 C41 C43 C45 . . . . 144.7(41) no C42 C41 C41 C42 . . . . -180.0000 no C42 C41 C41 C43 . . . . 175.8(50) no C42 C41 C42 C41 . . . . 0.00000(10) no C42 C41 C42 C43 . . . . 165(17) no C42 C41 C43 C44 . . . . 162(17) no C42 C41 C43 C45 . . . . -128(17) no C42 C43 C44 C45 . . . . 144.1(70) no C42 C43 C45 C44 . . . . -118(10) no C43 C41 C41 C43 . . . . -180.0000 no #------------------------------------------------------------------------------ #===END #============================================================================== # End of CIF #==============================================================================