data_General _audit_creation_date '2010-06-03' _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Atsushi Kobayashi' _publ_contact_author_email 'akoba@sci.hokudai.ac.jp' _publ_contact_author_fax '+81-11-706-3447' _publ_contact_author_phone '+81-11-706-3819' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'J. Am. Chem. Soc.' _publ_requested_category 'FA' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of Metal--Hydrazone Complexes and Vapochromic Behavior of their Hydrogen-Bonded Proton-Transfer Assemblies ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ; Atsushi Kobayashi, Masa-aki Dosen, Mee Chang, Kiyohiko Nakajima, Shin-ichiro Noro, Masako Kato ; ; Division of Chemistry, Faculty of Science, Hokkaido University Department of Education, Aichi University of Education Research Institute for Electronic Science, Hokkaido University ; ; North-10 West-8, Kita-ku, Sapporo 060-0810, Japan Igaya, Kariya Aichi 448-8542, Japan North-20, West-10, Kita-ku, Sapporo 001-0020, Japan ; _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2006). CrystalStructure (Version 3.8). Single Crystal Structure Analysis Software. Rigaku/MSC, 9009 TX, USA 77381-5209. Rigaku, Tokyo 196-8666, Japan. Sheldrick, G.M. (1997). SHELXL97. University of Gottingen, Germany. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #============================================================================== data___Complex2_[PdBr(mtbhp)] #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C13 H12 Br N3 Pd S ' _chemical_formula_moiety 'C13 H12 Br N3 Pd S ' _chemical_formula_weight 428.62 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 '+X,+Y,+Z' 2 '-X,1/2+Y,1/2-Z' 3 '-X,-Y,-Z' 4 '+X,1/2-Y,1/2+Z' #------------------------------------------------------------------------------ _cell_length_a 7.2466(10) _cell_length_b 8.6870(7) _cell_length_c 21.727(2) _cell_angle_alpha 90.0000 _cell_angle_beta 92.269(5) _cell_angle_gamma 90.0000 _cell_volume 1366.7(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4736 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150.1 #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 2.083 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832.00 _exptl_absorpt_coefficient_mu 4.432 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.233 _exptl_absorpt_correction_T_max 0.412 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 10556 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 25 _diffrn_ambient_temperature 150.1 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3120 _reflns_number_gt 3023 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0649 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3120 _refine_ls_number_parameters 173 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0333P)^2^+1.2290P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.87 _refine_diff_density_min -1.26 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Br' 'Br' -0.290 2.459 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Pd' 'Pd' -0.999 1.007 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd(1) Pd 0.77884(2) 0.144312(19) 0.062450(8) 0.01427(6) Uani 1.00 1 d . . . Br(1) Br 0.83671(5) 0.37504(3) 0.124070(13) 0.03332(8) Uani 1.00 1 d . . . S(1) S 0.88240(7) 0.27830(6) -0.01845(3) 0.01634(12) Uani 1.00 1 d . . . N(1) N 0.7176(2) -0.0512(2) 0.01767(9) 0.0147(3) Uani 1.00 1 d . . . N(2) N 0.6562(2) -0.1701(2) 0.05325(10) 0.0175(3) Uani 1.00 1 d . . . N(3) N 0.7001(2) 0.0127(2) 0.13288(9) 0.0164(3) Uani 1.00 1 d . . . C(1) C 0.8560(2) 0.1681(2) -0.08731(11) 0.0160(4) Uani 1.00 1 d . . . C(2) C 0.9187(3) 0.2405(2) -0.13988(11) 0.0193(4) Uani 1.00 1 d . . . C(3) C 0.9107(3) 0.1673(3) -0.19664(12) 0.0207(4) Uani 1.00 1 d . . . C(4) C 0.8408(3) 0.0185(3) -0.20098(11) 0.0208(4) Uani 1.00 1 d . . . C(5) C 0.7836(3) -0.0554(2) -0.14915(11) 0.0193(4) Uani 1.00 1 d . . . C(6) C 0.7887(2) 0.0158(2) -0.09025(11) 0.0153(4) Uani 1.00 1 d . . . C(7) C 0.7257(3) -0.0807(2) -0.04099(11) 0.0168(4) Uani 1.00 1 d . . . C(8) C 0.6524(3) -0.1324(2) 0.11307(11) 0.0157(4) Uani 1.00 1 d . . . C(9) C 0.5991(3) -0.2433(2) 0.15720(11) 0.0196(4) Uani 1.00 1 d . . . C(10) C 0.5967(3) -0.2050(3) 0.21800(12) 0.0221(5) Uani 1.00 1 d . . . C(11) C 0.6474(3) -0.0558(3) 0.23735(11) 0.0222(4) Uani 1.00 1 d . . . C(12) C 0.6978(3) 0.0471(2) 0.19369(11) 0.0201(4) Uani 1.00 1 d . . . C(13) C 0.7154(3) 0.4314(2) -0.03433(12) 0.0230(5) Uani 1.00 1 d . . . H(1) H 0.9762 0.3413 -0.1352 0.021 Uiso 1.00 1 c R . . H(2) H 0.9577 0.2121 -0.2335 0.013 Uiso 1.00 1 c R . . H(3) H 0.8318 -0.0358 -0.2410 0.026 Uiso 1.00 1 c R . . H(4) H 0.7368 -0.1566 -0.1520 0.026 Uiso 1.00 1 c R . . H(5) H 0.6852 -0.1830 -0.0539 0.012 Uiso 1.00 1 c R . . H(6) H 0.5643 -0.3427 0.1448 0.025 Uiso 1.00 1 c R . . H(7) H 0.5637 -0.2752 0.2465 0.032 Uiso 1.00 1 c R . . H(8) H 0.6460 -0.0269 0.2782 0.025 Uiso 1.00 1 c R . . H(9) H 0.7289 0.1445 0.2035 0.025 Uiso 1.00 1 c R . . H(10) H 0.7459 0.4729 -0.0732 0.025 Uiso 1.00 1 c R . . H(12) H 0.5929 0.3898 -0.0407 0.028 Uiso 1.00 1 c R . . H(13) H 0.7192 0.4853 0.0006 0.028 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.01677(10) 0.00938(10) 0.01659(11) -0.00068(6) -0.00028(7) -0.00108(6) Br(1) 0.0628(2) 0.01434(14) 0.02292(16) -0.00931(11) 0.00343(13) -0.00544(10) S(1) 0.0179(2) 0.0113(2) 0.0198(2) -0.0018(2) -0.0001(2) -0.0005(2) N(1) 0.0148(7) 0.0107(8) 0.0186(9) 0.0001(6) -0.0008(7) 0.0007(7) N(2) 0.0202(9) 0.0107(8) 0.0216(10) -0.0025(7) 0.0005(7) 0.0016(7) N(3) 0.0161(8) 0.0137(9) 0.0194(9) -0.0004(7) 0.0003(7) 0.0007(7) C(1) 0.0132(9) 0.0145(10) 0.0200(11) 0.0006(8) -0.0012(8) 0.0001(8) C(2) 0.0172(10) 0.0171(11) 0.0236(12) 0.0003(8) 0.0010(8) 0.0022(9) C(3) 0.0171(10) 0.0247(12) 0.0204(12) 0.0019(9) 0.0019(8) 0.0042(9) C(4) 0.0205(10) 0.0230(12) 0.0188(11) 0.0029(9) -0.0009(8) -0.0027(9) C(5) 0.0212(10) 0.0154(11) 0.0210(11) 0.0008(8) -0.0012(8) -0.0015(9) C(6) 0.0129(9) 0.0144(10) 0.0184(11) 0.0015(8) -0.0018(7) -0.0002(8) C(7) 0.0181(10) 0.0098(10) 0.0223(11) -0.0003(8) -0.0020(8) -0.0014(8) C(8) 0.0123(9) 0.0140(11) 0.0206(11) 0.0015(7) -0.0005(8) 0.0007(8) C(9) 0.0189(10) 0.0153(11) 0.0244(12) -0.0003(8) -0.0012(8) 0.0033(9) C(10) 0.0197(10) 0.0205(12) 0.0262(12) 0.0022(9) 0.0026(9) 0.0080(10) C(11) 0.0217(10) 0.0271(13) 0.0177(11) 0.0015(9) 0.0010(9) -0.0007(9) C(12) 0.0197(10) 0.0178(11) 0.0230(12) 0.0003(9) 0.0016(8) -0.0035(9) C(13) 0.0284(11) 0.0137(11) 0.0267(13) 0.0052(9) 0.0003(9) -0.0001(9) #============================================================================== _computing_data_collection 'CrystalClear' _computing_cell_refinement 'CrystalClear' _computing_data_reduction 'CrystalStructure' _computing_structure_solution 'SIR2004' _computing_structure_refinement 'SHELXL' _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Pd(1) Br(1) 2.4374(3) yes . . Pd(1) S(1) 2.2609(6) yes . . Pd(1) N(1) 1.9982(19) yes . . Pd(1) N(3) 2.0109(19) yes . . S(1) C(1) 1.780(2) yes . . S(1) C(13) 1.822(2) yes . . N(1) N(2) 1.375(2) yes . . N(1) C(7) 1.304(3) yes . . N(2) C(8) 1.342(3) yes . . N(3) C(8) 1.372(2) yes . . N(3) C(12) 1.355(3) yes . . C(1) C(2) 1.396(3) yes . . C(1) C(6) 1.410(3) yes . . C(2) C(3) 1.387(3) yes . . C(3) C(4) 1.391(3) yes . . C(4) C(5) 1.374(3) yes . . C(5) C(6) 1.421(3) yes . . C(6) C(7) 1.448(3) yes . . C(8) C(9) 1.423(3) yes . . C(9) C(10) 1.363(3) yes . . C(10) C(11) 1.407(3) yes . . C(11) C(12) 1.363(3) yes . . C(2) H(1) 0.973 no . . C(3) H(2) 0.964 no . . C(4) H(3) 0.989 no . . C(5) H(4) 0.944 no . . C(7) H(5) 0.974 no . . C(9) H(6) 0.936 no . . C(10) H(7) 0.907 no . . C(11) H(8) 0.922 no . . C(12) H(9) 0.899 no . . C(13) H(10) 0.952 no . . C(13) H(12) 0.963 no . . C(13) H(13) 0.891 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Br(1) Pd(1) S(1) 87.047(16) yes . . . Br(1) Pd(1) N(1) 175.07(5) yes . . . Br(1) Pd(1) N(3) 95.59(5) yes . . . S(1) Pd(1) N(1) 97.65(5) yes . . . S(1) Pd(1) N(3) 175.73(5) yes . . . N(1) Pd(1) N(3) 79.81(7) yes . . . Pd(1) S(1) C(1) 110.39(7) yes . . . Pd(1) S(1) C(13) 106.53(8) yes . . . C(1) S(1) C(13) 100.66(11) yes . . . Pd(1) N(1) N(2) 115.81(14) yes . . . Pd(1) N(1) C(7) 128.72(16) yes . . . N(2) N(1) C(7) 115.46(19) yes . . . N(1) N(2) C(8) 112.38(18) yes . . . Pd(1) N(3) C(8) 111.06(15) yes . . . Pd(1) N(3) C(12) 129.15(16) yes . . . C(8) N(3) C(12) 119.7(2) yes . . . S(1) C(1) C(2) 114.68(17) yes . . . S(1) C(1) C(6) 124.61(18) yes . . . C(2) C(1) C(6) 120.6(2) yes . . . C(1) C(2) C(3) 121.2(2) yes . . . C(2) C(3) C(4) 119.3(2) yes . . . C(3) C(4) C(5) 120.0(2) yes . . . C(4) C(5) C(6) 122.5(2) yes . . . C(1) C(6) C(5) 116.5(2) yes . . . C(1) C(6) C(7) 128.9(2) yes . . . C(5) C(6) C(7) 114.6(2) yes . . . N(1) C(7) C(6) 129.5(2) yes . . . N(2) C(8) N(3) 120.9(2) yes . . . N(2) C(8) C(9) 120.3(2) yes . . . N(3) C(8) C(9) 118.8(2) yes . . . C(8) C(9) C(10) 120.1(2) yes . . . C(9) C(10) C(11) 120.1(2) yes . . . C(10) C(11) C(12) 118.0(2) yes . . . N(3) C(12) C(11) 123.2(2) yes . . . C(1) C(2) H(1) 118.2 no . . . C(3) C(2) H(1) 120.5 no . . . C(2) C(3) H(2) 123.4 no . . . C(4) C(3) H(2) 117.3 no . . . C(3) C(4) H(3) 120.9 no . . . C(5) C(4) H(3) 119.1 no . . . C(4) C(5) H(4) 120.0 no . . . C(6) C(5) H(4) 117.5 no . . . N(1) C(7) H(5) 115.9 no . . . C(6) C(7) H(5) 114.6 no . . . C(8) C(9) H(6) 120.5 no . . . C(10) C(9) H(6) 119.4 no . . . C(9) C(10) H(7) 120.6 no . . . C(11) C(10) H(7) 119.3 no . . . C(10) C(11) H(8) 121.7 no . . . C(12) C(11) H(8) 120.3 no . . . N(3) C(12) H(9) 115.1 no . . . C(11) C(12) H(9) 121.6 no . . . S(1) C(13) H(10) 105.6 no . . . S(1) C(13) H(12) 110.8 no . . . S(1) C(13) H(13) 103.0 no . . . H(10) C(13) H(12) 105.1 no . . . H(10) C(13) H(13) 123.7 no . . . H(12) C(13) H(13) 108.5 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 _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Br(1) Pd(1) S(1) C(1) -174.86(7) ? . . . . Br(1) Pd(1) S(1) C(13) -66.43(8) ? . . . . Br(1) Pd(1) N(1) N(2) -21.0(7) ? . . . . Br(1) Pd(1) N(1) C(7) 158.0(5) ? . . . . Br(1) Pd(1) N(3) C(8) 179.06(13) ? . . . . Br(1) Pd(1) N(3) C(12) -4.26(19) ? . . . . S(1) Pd(1) N(1) N(2) 176.75(13) ? . . . . S(1) Pd(1) N(1) C(7) -4.26(19) ? . . . . N(1) Pd(1) S(1) C(1) 3.64(9) ? . . . . N(1) Pd(1) S(1) C(13) 112.07(9) ? . . . . S(1) Pd(1) N(3) C(8) -52.9(8) ? . . . . S(1) Pd(1) N(3) C(12) 123.8(7) ? . . . . N(3) Pd(1) S(1) C(1) 56.8(7) ? . . . . N(3) Pd(1) S(1) C(13) 165.3(7) ? . . . . N(1) Pd(1) N(3) C(8) 0.85(14) ? . . . . N(1) Pd(1) N(3) C(12) 177.5(2) ? . . . . N(3) Pd(1) N(1) N(2) 0.22(14) ? . . . . N(3) Pd(1) N(1) C(7) 179.21(19) ? . . . . Pd(1) S(1) C(1) C(2) -179.16(14) ? . . . . Pd(1) S(1) C(1) C(6) -3.0(2) ? . . . . C(13) S(1) C(1) C(2) 68.59(18) ? . . . . C(13) S(1) C(1) C(6) -115.22(19) ? . . . . Pd(1) N(1) N(2) C(8) -1.3(2) ? . . . . Pd(1) N(1) C(7) C(6) 3.2(3) ? . . . . N(2) N(1) C(7) C(6) -177.8(2) ? . . . . C(7) N(1) N(2) C(8) 179.60(18) ? . . . . N(1) N(2) C(8) N(3) 2.2(2) ? . . . . N(1) N(2) C(8) C(9) -177.64(19) ? . . . . Pd(1) N(3) C(8) N(2) -2.0(2) ? . . . . Pd(1) N(3) C(8) C(9) 177.85(16) ? . . . . Pd(1) N(3) C(12) C(11) -177.33(17) ? . . . . C(8) N(3) C(12) C(11) -0.9(3) ? . . . . C(12) N(3) C(8) N(2) -179.0(2) ? . . . . C(12) N(3) C(8) C(9) 0.8(3) ? . . . . S(1) C(1) C(2) C(3) 178.61(17) ? . . . . S(1) C(1) C(6) C(5) -177.83(16) ? . . . . S(1) C(1) C(6) C(7) 1.1(3) ? . . . . C(2) C(1) C(6) C(5) -1.9(3) ? . . . . C(2) C(1) C(6) C(7) 177.1(2) ? . . . . C(6) C(1) C(2) C(3) 2.3(3) ? . . . . C(1) C(2) C(3) C(4) -0.7(3) ? . . . . C(2) C(3) C(4) C(5) -1.2(3) ? . . . . C(3) C(4) C(5) C(6) 1.5(3) ? . . . . C(4) C(5) C(6) C(1) -0.0(3) ? . . . . C(4) C(5) C(6) C(7) -179.1(2) ? . . . . C(1) C(6) C(7) N(1) -0.8(3) ? . . . . C(5) C(6) C(7) N(1) 178.2(2) ? . . . . N(2) C(8) C(9) C(10) 179.5(2) ? . . . . N(3) C(8) C(9) C(10) -0.3(3) ? . . . . C(8) C(9) C(10) C(11) -0.1(2) ? . . . . C(9) C(10) C(11) C(12) 0.1(2) ? . . . . C(10) C(11) C(12) N(3) 0.4(3) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Pd(1) C(6) 3.460(2) ? . 3_755 S(1) N(1) 3.5059(18) ? . 3_755 S(1) N(2) 3.5823(19) ? . 3_755 S(1) C(7) 3.520(2) ? . 3_755 N(1) S(1) 3.5059(18) ? . 3_755 N(1) N(1) 3.337(2) ? . 3_655 N(1) C(1) 3.535(2) ? . 3_755 N(1) C(7) 3.466(2) ? . 3_655 N(2) S(1) 3.5823(19) ? . 3_755 N(2) C(1) 3.582(2) ? . 3_755 N(2) C(2) 3.598(2) ? . 3_755 N(2) C(7) 3.524(2) ? . 3_655 N(2) C(13) 3.533(3) ? . 3_655 N(3) C(2) 3.530(2) ? . 3_755 N(3) C(3) 3.465(3) ? . 3_755 N(3) C(4) 3.597(2) ? . 3_755 N(3) C(5) 3.557(2) ? . 3_655 C(1) N(1) 3.535(2) ? . 3_755 C(1) N(2) 3.582(2) ? . 3_755 C(2) N(2) 3.598(2) ? . 3_755 C(2) N(3) 3.530(2) ? . 3_755 C(2) C(8) 3.277(3) ? . 3_755 C(2) C(9) 3.530(3) ? . 3_755 C(3) N(3) 3.465(3) ? . 3_755 C(3) C(8) 3.600(3) ? . 3_755 C(3) C(11) 3.493(3) ? . 3_755 C(3) C(12) 3.392(3) ? . 3_755 C(4) N(3) 3.597(2) ? . 3_755 C(4) C(10) 3.567(3) ? . 3_655 C(4) C(12) 3.389(3) ? . 3_755 C(5) N(3) 3.557(2) ? . 3_655 C(5) C(12) 3.584(3) ? . 3_655 C(6) Pd(1) 3.460(2) ? . 3_755 C(6) C(8) 3.371(2) ? . 3_655 C(7) S(1) 3.520(2) ? . 3_755 C(7) N(1) 3.466(2) ? . 3_655 C(7) N(2) 3.524(2) ? . 3_655 C(8) C(2) 3.277(3) ? . 3_755 C(8) C(3) 3.600(3) ? . 3_755 C(8) C(6) 3.371(2) ? . 3_655 C(9) C(2) 3.530(3) ? . 3_755 C(10) C(4) 3.567(3) ? . 3_655 C(11) C(3) 3.493(3) ? . 3_755 C(12) C(3) 3.392(3) ? . 3_755 C(12) C(4) 3.389(3) ? . 3_755 C(12) C(5) 3.584(3) ? . 3_655 C(13) N(2) 3.533(3) ? . 3_655 Pd(1) H(5) 3.377 ? . 3_655 Br(1) H(1) 2.819 ? . 3_765 Br(1) H(2) 3.271 ? . 4_555 Br(1) H(3) 3.249 ? . 4_555 Br(1) H(6) 3.191 ? . 1_565 Br(1) H(10) 3.519 ? . 3_765 S(1) H(5) 3.547 ? . 3_755 S(1) H(13) 3.552 ? . 3_765 N(2) H(1) 3.479 ? . 3_755 N(2) H(12) 2.634 ? . 3_655 N(2) H(13) 3.243 ? . 1_545 N(3) H(4) 3.444 ? . 3_655 N(3) H(5) 3.543 ? . 3_655 C(1) H(6) 3.583 ? . 3_655 C(3) H(3) 3.489 ? . 2_754 C(3) H(9) 2.982 ? . 4_554 C(4) H(2) 3.377 ? . 2_744 C(4) H(7) 3.102 ? . 4_544 C(4) H(9) 3.427 ? . 3_755 C(5) H(7) 3.093 ? . 4_544 C(8) H(1) 3.266 ? . 3_755 C(8) H(12) 3.227 ? . 3_655 C(9) H(1) 3.247 ? . 3_755 C(9) H(2) 3.566 ? . 3_755 C(9) H(3) 3.335 ? . 4_545 C(9) H(8) 3.375 ? . 2_645 C(9) H(12) 3.112 ? . 3_655 C(10) H(2) 3.234 ? . 3_755 C(10) H(3) 2.941 ? . 4_545 C(10) H(4) 3.198 ? . 4_545 C(10) H(8) 3.306 ? . 2_645 C(10) H(9) 3.241 ? . 2_645 C(11) H(2) 3.172 ? . 3_755 C(11) H(3) 3.567 ? . 3_655 C(11) H(4) 3.510 ? . 4_545 C(11) H(6) 3.556 ? . 2_655 C(11) H(7) 2.906 ? . 2_655 C(12) H(2) 3.447 ? . 3_755 C(12) H(2) 3.192 ? . 4_555 C(12) H(3) 3.523 ? . 3_755 C(12) H(4) 3.379 ? . 3_655 C(12) H(7) 2.804 ? . 2_655 C(13) H(5) 3.383 ? . 1_565 C(13) H(6) 3.175 ? . 3_655 C(13) H(12) 3.217 ? . 3_665 C(13) H(13) 3.341 ? . 3_665 H(1) Br(1) 2.819 ? . 3_765 H(1) N(2) 3.479 ? . 3_755 H(1) C(8) 3.266 ? . 3_755 H(1) C(9) 3.247 ? . 3_755 H(1) H(3) 3.257 ? . 2_754 H(1) H(6) 3.345 ? . 3_755 H(1) H(8) 3.393 ? . 4_554 H(2) Br(1) 3.271 ? . 4_554 H(2) C(4) 3.377 ? . 2_754 H(2) C(9) 3.566 ? . 3_755 H(2) C(10) 3.234 ? . 3_755 H(2) C(11) 3.172 ? . 3_755 H(2) C(12) 3.447 ? . 3_755 H(2) C(12) 3.192 ? . 4_554 H(2) H(3) 2.738 ? . 2_754 H(2) H(4) 3.582 ? . 2_754 H(2) H(7) 3.534 ? . 3_755 H(2) H(8) 3.464 ? . 3_755 H(2) H(8) 3.562 ? . 4_554 H(2) H(9) 2.449 ? . 4_554 H(3) Br(1) 3.249 ? . 4_554 H(3) C(3) 3.489 ? . 2_744 H(3) C(9) 3.335 ? . 4_544 H(3) C(10) 2.941 ? . 4_544 H(3) C(11) 3.567 ? . 3_655 H(3) C(12) 3.523 ? . 3_755 H(3) H(1) 3.257 ? . 2_744 H(3) H(2) 2.738 ? . 2_744 H(3) H(6) 3.263 ? . 4_544 H(3) H(7) 2.550 ? . 4_544 H(3) H(8) 3.566 ? . 3_655 H(3) H(9) 3.389 ? . 3_755 H(4) N(3) 3.444 ? . 3_655 H(4) C(10) 3.198 ? . 4_544 H(4) C(11) 3.510 ? . 4_544 H(4) C(12) 3.379 ? . 3_655 H(4) H(2) 3.582 ? . 2_744 H(4) H(7) 2.564 ? . 4_544 H(4) H(8) 3.196 ? . 4_544 H(4) H(9) 3.514 ? . 3_655 H(5) Pd(1) 3.377 ? . 3_655 H(5) S(1) 3.547 ? . 3_755 H(5) N(3) 3.543 ? . 3_655 H(5) C(13) 3.383 ? . 1_545 H(5) H(10) 3.053 ? . 1_545 H(5) H(12) 3.442 ? . 3_655 H(5) H(13) 3.121 ? . 1_545 H(6) Br(1) 3.191 ? . 1_545 H(6) C(1) 3.583 ? . 3_655 H(6) C(11) 3.556 ? . 2_645 H(6) C(13) 3.175 ? . 3_655 H(6) H(1) 3.345 ? . 3_755 H(6) H(3) 3.263 ? . 4_545 H(6) H(8) 2.808 ? . 2_645 H(6) H(10) 2.912 ? . 3_655 H(6) H(12) 2.526 ? . 3_655 H(7) C(4) 3.102 ? . 4_545 H(7) C(5) 3.093 ? . 4_545 H(7) C(11) 2.906 ? . 2_645 H(7) C(12) 2.804 ? . 2_645 H(7) H(2) 3.534 ? . 3_755 H(7) H(3) 2.550 ? . 4_545 H(7) H(4) 2.564 ? . 4_545 H(7) H(8) 2.704 ? . 2_645 H(7) H(9) 2.519 ? . 2_645 H(8) C(9) 3.375 ? . 2_655 H(8) C(10) 3.306 ? . 2_655 H(8) H(1) 3.393 ? . 4_555 H(8) H(2) 3.464 ? . 3_755 H(8) H(2) 3.562 ? . 4_555 H(8) H(3) 3.566 ? . 3_655 H(8) H(4) 3.196 ? . 4_545 H(8) H(6) 2.808 ? . 2_655 H(8) H(7) 2.704 ? . 2_655 H(8) H(10) 3.316 ? . 4_555 H(9) C(3) 2.982 ? . 4_555 H(9) C(4) 3.427 ? . 3_755 H(9) C(10) 3.241 ? . 2_655 H(9) H(2) 2.449 ? . 4_555 H(9) H(3) 3.389 ? . 3_755 H(9) H(4) 3.514 ? . 3_655 H(9) H(7) 2.519 ? . 2_655 H(10) Br(1) 3.519 ? . 3_765 H(10) H(5) 3.053 ? . 1_565 H(10) H(6) 2.912 ? . 3_655 H(10) H(8) 3.316 ? . 4_554 H(12) N(2) 2.634 ? . 3_655 H(12) C(8) 3.227 ? . 3_655 H(12) C(9) 3.112 ? . 3_655 H(12) C(13) 3.217 ? . 3_665 H(12) H(5) 3.442 ? . 3_655 H(12) H(6) 2.526 ? . 3_655 H(12) H(12) 2.965 ? . 3_665 H(12) H(13) 2.685 ? . 3_665 H(13) S(1) 3.552 ? . 3_765 H(13) N(2) 3.243 ? . 1_565 H(13) C(13) 3.341 ? . 3_665 H(13) H(5) 3.121 ? . 1_565 H(13) H(12) 2.685 ? . 3_665 H(13) H(13) 3.186 ? . 3_665 #============================================================================== # End of CIF #==============================================================================