Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 # SUBMISSION DETAILS _publ_contact_author_name 'Osamu Yamauchi' _publ_contact_author_address ; Unit Of Chemistry Kansai University Faculty of Engineering Yamate-Cho Suita Osaka 564-8680 JAPAN ; _publ_contact_author_email osamuy@ipcku.kansai-u.ac.jp _publ_requested_category CM #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; pai-pai Stacking assisted binding of aromatic amino acids by copper(II)- aromatic diimine complexes. Effects of ring substituents on ternary complex stability ; loop_ _publ_author_name _publ_author_footnote _publ_author_address T.Yajima ; Kansai University ; ; Unit of Chemistry, Faculty of Engineering, Kansai University, Suita, Osaka 564-8680, Japan. ; R.Takamido ; Nagoya University ; ; Department of Chemistry, Graduate School of Science, Nagoya University, Nagoya 464-8680, Japan. ; Y.Shimazaki ; Kyushu University ; ; Institute for Materials Chemistry and Engineering, Kyushu University, Fukuoka 812-8581, Japan. ; A.Odani ; Nagoya University ; ; Research Center for Materials Science, Nagoya University, Nagoya 464-8680, Japan. ; Y.Nakabayashi ; Kansai University ; ; Unit of Chemistry, Faculty of Engineering, Kansai University, Suita, Osaka 564-8680, Japan. ; ; O.Yamauchi ; ; Kansai University ; ; Unit of Chemistry, Faculty of Engineering, Kansai University, Suita, Osaka 564-8680, Japan. ; #==================================================================== # TEXT #ENTER OTHER REFERENCES _publ_section_references ; Rigaku/MSC and Rigaku Corporation. (2005). CrystalStructure 3.7.0. Single Crystal Structure Analysis Software. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; #------------------------------------------------------------------------------ loop_ _publ_manuscript_incl_extra_item '_geom_extra_table_head_3' '_geom_bond_atom_site_label_D' '_geom_bond_atom_site_label_H' '_geom_contact_atom_site_label_A' '_geom_bond_distance_DH' '_geom_contact_distance_HA' '_geom_contact_distance_DA' '_geom_angle_DHA' '_geom_contact_site_symmetry_A' # # #------------------------------------------------------------------------------ #============================================================================== data__[Cu(dpa)(trp)]ClO4.2H2O(1) _database_code_depnum_ccdc_archive 'CCDC 611926' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C21 H24 Cl Cu N5 O8 ' _chemical_formula_moiety '[Cu(dpa)(trp)]ClO4.2H2O(1)' _chemical_formula_weight 571.43 #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2+X,1/2-Y,-Z 3 -X,1/2+Y,1/2-Z 4 1/2-X,-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 6.7769(10) _cell_length_b 10.96900(10) _cell_length_c 31.0900(3) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 2311.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273.1 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour 'deep blue' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.642 _exptl_crystal_F_000 1172.00 _exptl_absorpt_coefficient_mu 1.120 _exptl_absorpt_correction_type none #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_device_type AFC-5R _diffrn_reflns_number 3011 _diffrn_reflns_theta_max 27.59 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.977 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 40 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement 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 3011 _reflns_number_gt 2915 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.2048 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3011 _refine_ls_number_parameters 344 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0103Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0098 _refine_diff_density_max 2.94 _refine_diff_density_min -1.29 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.320 1.265 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; 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) ; C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 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) ; Cl Cl 0.148 0.159 ; 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 Cu(1) Cu 0.47553(9) 0.09096(5) 0.11798(2) 0.01936(17) Uani 1.00 1 d . . . Cl(1) Cl 0.1717(2) 0.08438(12) -0.03813(3) 0.0257(2) Uani 1.00 1 d . . . O(1) O 0.4466(6) 0.2472(3) 0.14731(12) 0.0255(8) Uani 1.00 1 d . . . O(2) O 0.2451(6) 0.4065(3) 0.15209(12) 0.0275(8) Uani 1.00 1 d . . . O(3) O 0.1743(7) 0.0120(3) 0.00058(12) 0.0327(10) Uani 1.00 1 d . . . O(4) O 0.2168(10) 0.2094(4) -0.02804(16) 0.0491(13) Uani 1.00 1 d . . . O(5) O -0.0207(7) 0.0777(4) -0.05768(17) 0.0452(13) Uani 1.00 1 d . . . O(6) O 0.3142(7) 0.0352(4) -0.06829(13) 0.0413(11) Uani 1.00 1 d . . . O(7) O 0.5950(7) 0.5459(3) 0.14759(12) 0.0335(9) Uani 1.00 1 d . . . O(8) O 0.8955(9) 0.4285(6) 0.20262(14) 0.0572(16) Uani 1.00 1 d . . . N(1) N 0.5618(6) 0.0012(3) 0.16935(12) 0.0213(9) Uani 1.00 1 d . . . N(2) N 0.5592(7) -0.1891(4) 0.13268(12) 0.0229(9) Uani 1.00 1 d . . . N(3) N 0.5772(6) -0.0361(3) 0.07946(12) 0.0200(9) Uani 1.00 1 d . . . N(4) N 0.3103(7) 0.1732(3) 0.07389(12) 0.0232(9) Uani 1.00 1 d . . . N(5) N 0.0867(8) -0.0135(5) 0.20834(16) 0.0387(14) Uani 1.00 1 d . . . C(1) C 0.5844(8) 0.0626(5) 0.20716(17) 0.0263(11) Uani 1.00 1 d . . . C(2) C 0.6085(9) 0.0016(5) 0.24629(17) 0.0321(13) Uani 1.00 1 d . . . C(3) C 0.6171(10) -0.1215(6) 0.24599(18) 0.0351(13) Uani 1.00 1 d . . . C(4) C 0.5997(9) -0.1863(5) 0.20873(18) 0.0316(13) Uani 1.00 1 d . . . C(5) C 0.5722(7) -0.1215(4) 0.16999(16) 0.0221(10) Uani 1.00 1 d . . . C(6) C 0.5827(7) -0.1529(4) 0.09041(16) 0.0225(11) Uani 1.00 1 d . . . C(7) C 0.6113(9) -0.2453(4) 0.05993(18) 0.0287(12) Uani 1.00 1 d . . . C(8) C 0.6544(10) -0.2134(5) 0.01857(17) 0.0299(12) Uani 1.00 1 d . . . C(9) C 0.6662(8) -0.0921(4) 0.00703(13) 0.0255(11) Uani 1.00 1 d . . . C(10) C 0.6236(9) -0.0056(5) 0.03809(16) 0.0287(12) Uani 1.00 1 d . . . C(11) C 0.1755(7) 0.2561(4) 0.09803(14) 0.0204(10) Uani 1.00 1 d . . . C(12) C 0.2965(8) 0.3083(4) 0.13490(13) 0.0209(10) Uani 1.00 1 d . . . C(13) C -0.0057(8) 0.1865(4) 0.11437(17) 0.0271(11) Uani 1.00 1 d . . . C(14) C 0.0559(10) 0.0985(7) 0.1896(2) 0.0423(16) Uani 1.00 1 d . . . C(15) C 0.0411(7) 0.0845(5) 0.14545(18) 0.0291(12) Uani 1.00 1 d . . . C(16) C 0.0631(8) -0.0437(5) 0.13628(19) 0.0303(12) Uani 1.00 1 d . . . C(17) C 0.0569(8) -0.1122(6) 0.0997(2) 0.0344(14) Uani 1.00 1 d . . . C(18) C 0.0733(11) -0.2400(6) 0.1028(2) 0.0443(17) Uani 1.00 1 d . . . C(19) C 0.0906(11) -0.2942(7) 0.1414(2) 0.0460(18) Uani 1.00 1 d . . . C(20) C 0.0986(8) -0.2272(5) 0.1802(2) 0.0357(14) Uani 1.00 1 d . . . C(21) C 0.0882(7) -0.1020(5) 0.17761(19) 0.0289(12) Uani 1.00 1 d . . . H(1) H 0.5815 0.1492 0.2069 0.032 Uiso 1.00 1 c R . . H(2) H 0.6230 0.0464 0.2723 0.038 Uiso 1.00 1 c R . . H(3) H 0.6319 -0.1640 0.2724 0.042 Uiso 1.00 1 c R . . H(4) H 0.6082 -0.2727 0.2085 0.038 Uiso 1.00 1 c R . . H(5) H 0.6022 -0.3286 0.0681 0.035 Uiso 1.00 1 c R . . H(6) H 0.6771 -0.2747 -0.0024 0.036 Uiso 1.00 1 c R . . H(7) H 0.7019 -0.0683 -0.0213 0.031 Uiso 1.00 1 c R . . H(8) H 0.6263 0.0782 0.0304 0.034 Uiso 1.00 1 c R . . H(9) H 0.2366 0.1148 0.0580 0.028 Uiso 1.00 1 c R . . H(10) H 0.3912 0.2187 0.0548 0.028 Uiso 1.00 1 c R . . H(11) H 0.1336 0.3205 0.0798 0.025 Uiso 1.00 1 c R . . H(12) H -0.0910 0.2426 0.1283 0.032 Uiso 1.00 1 c R . . H(13) H -0.0715 0.1521 0.0903 0.032 Uiso 1.00 1 c R . . H(14) H 0.1024 -0.0277 0.2383 0.046 Uiso 1.00 1 c R . . H(15) H 0.0484 0.1739 0.2045 0.051 Uiso 1.00 1 c R . . H(16) H 0.0406 -0.0746 0.0725 0.041 Uiso 1.00 1 c R . . H(17) H 0.0698 -0.2879 0.0773 0.053 Uiso 1.00 1 c R . . H(18) H 0.1003 -0.3805 0.1426 0.055 Uiso 1.00 1 c R . . H(19) H 0.1106 -0.2664 0.2073 0.043 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 Cu(1) 0.0250(3) 0.0157(3) 0.0174(3) 0.0022(2) -0.00112(19) -0.00082(17) Cl(1) 0.0368(6) 0.0179(5) 0.0224(5) -0.0013(4) -0.0023(4) 0.0011(3) O(1) 0.0367(18) 0.0157(15) 0.0242(16) 0.0040(15) -0.0048(15) -0.0031(12) O(2) 0.0399(19) 0.0189(16) 0.0236(15) 0.0036(16) 0.0017(14) -0.0047(12) O(3) 0.055(2) 0.0203(16) 0.0224(17) -0.0010(18) -0.0084(18) 0.0050(13) O(4) 0.083(4) 0.0185(19) 0.046(2) -0.009(2) -0.001(2) 0.0003(16) O(5) 0.045(2) 0.043(2) 0.047(2) 0.007(2) -0.011(2) 0.004(2) O(6) 0.043(2) 0.043(2) 0.038(2) 0.001(2) 0.012(2) -0.0035(18) O(7) 0.042(2) 0.0263(18) 0.0319(18) -0.0025(18) -0.0034(17) -0.0032(15) O(8) 0.059(3) 0.077(4) 0.036(2) 0.019(3) 0.007(2) -0.002(2) N(1) 0.0264(19) 0.0193(18) 0.0182(16) -0.0018(17) -0.0040(16) 0.0017(13) N(2) 0.031(2) 0.0191(19) 0.0187(17) -0.0001(18) 0.0014(15) 0.0066(14) N(3) 0.0235(19) 0.0159(18) 0.0206(17) 0.0019(15) 0.0045(14) 0.0010(14) N(4) 0.036(2) 0.0142(17) 0.0197(15) -0.0004(17) -0.0003(16) -0.0014(12) N(5) 0.040(2) 0.048(3) 0.028(2) -0.003(2) 0.005(2) 0.005(2) C(1) 0.028(2) 0.025(2) 0.026(2) -0.001(2) 0.0028(18) 0.0009(18) C(2) 0.037(2) 0.039(2) 0.020(2) -0.002(2) 0.001(2) -0.0032(19) C(3) 0.041(3) 0.040(3) 0.024(2) -0.006(2) -0.012(2) 0.006(2) C(4) 0.038(3) 0.028(2) 0.029(2) -0.002(2) -0.001(2) 0.008(2) C(5) 0.0217(19) 0.023(2) 0.022(2) 0.0034(18) 0.0009(17) 0.0047(17) C(6) 0.019(2) 0.024(2) 0.024(2) 0.0004(18) 0.0004(17) 0.0059(17) C(7) 0.040(2) 0.015(2) 0.032(2) 0.004(2) -0.006(2) -0.0015(18) C(8) 0.041(2) 0.024(2) 0.025(2) 0.003(2) -0.003(2) -0.0082(18) C(9) 0.033(2) 0.027(2) 0.0168(18) 0.006(2) 0.0046(18) -0.0020(16) C(10) 0.034(2) 0.028(2) 0.024(2) 0.008(2) 0.002(2) 0.0037(19) C(11) 0.024(2) 0.0168(19) 0.0209(19) -0.0000(18) -0.0008(16) -0.0030(14) C(12) 0.027(2) 0.0131(19) 0.0224(19) -0.0027(19) 0.0043(17) -0.0032(14) C(13) 0.028(2) 0.017(2) 0.036(2) 0.0025(19) -0.003(2) 0.0033(18) C(14) 0.042(3) 0.051(4) 0.034(2) -0.006(3) 0.010(2) 0.007(2) C(15) 0.018(2) 0.037(3) 0.032(2) 0.002(2) 0.0049(18) 0.008(2) C(16) 0.018(2) 0.033(2) 0.040(2) 0.002(2) 0.0004(19) 0.012(2) C(17) 0.025(2) 0.039(3) 0.040(3) -0.005(2) -0.010(2) 0.003(2) C(18) 0.043(3) 0.040(3) 0.050(3) 0.002(3) 0.003(3) 0.003(2) C(19) 0.042(3) 0.036(3) 0.059(4) 0.008(3) 0.012(3) 0.010(2) C(20) 0.029(2) 0.036(3) 0.042(3) 0.004(2) 0.002(2) 0.014(2) C(21) 0.020(2) 0.031(2) 0.036(2) -0.007(2) 0.0004(19) 0.005(2) #============================================================================== _computing_data_reduction CrystalStructure _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.7.0' #============================================================================== # 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 Cu(1) O(1) 1.951(3) ? . . Cu(1) N(1) 1.965(4) ? . . Cu(1) N(3) 1.963(4) ? . . Cu(1) N(4) 1.986(4) ? . . Cl(1) O(3) 1.442(3) ? . . Cl(1) O(4) 1.440(4) ? . . Cl(1) O(5) 1.441(5) ? . . Cl(1) O(6) 1.450(4) ? . . O(1) C(12) 1.278(6) ? . . O(2) C(12) 1.252(5) ? . . N(1) C(1) 1.364(6) ? . . N(1) C(5) 1.348(6) ? . . N(2) C(5) 1.380(6) ? . . N(2) C(6) 1.382(6) ? . . N(3) C(6) 1.325(6) ? . . N(3) C(10) 1.366(6) ? . . N(4) C(11) 1.492(6) ? . . N(5) C(14) 1.376(9) ? . . N(5) C(21) 1.362(8) ? . . C(1) C(2) 1.398(7) ? . . C(2) C(3) 1.352(9) ? . . C(3) C(4) 1.364(8) ? . . C(4) C(5) 1.411(7) ? . . C(6) C(7) 1.401(7) ? . . C(7) C(8) 1.364(7) ? . . C(8) C(9) 1.380(7) ? . . C(9) C(10) 1.384(7) ? . . C(11) C(12) 1.521(6) ? . . C(11) C(13) 1.533(7) ? . . C(13) C(15) 1.511(7) ? . . C(14) C(15) 1.384(8) ? . . C(15) C(16) 1.443(8) ? . . C(16) C(17) 1.362(8) ? . . C(16) C(21) 1.445(8) ? . . C(17) C(18) 1.410(9) ? . . C(18) C(19) 1.343(10) ? . . C(19) C(20) 1.414(10) ? . . C(20) C(21) 1.377(8) ? . . N(4) H(9) 0.950 ? . . N(4) H(10) 0.950 ? . . N(5) H(14) 0.950 ? . . C(1) H(1) 0.950 ? . . C(2) H(2) 0.950 ? . . C(3) H(3) 0.950 ? . . C(4) H(4) 0.950 ? . . C(7) H(5) 0.950 ? . . C(8) H(6) 0.950 ? . . C(9) H(7) 0.950 ? . . C(10) H(8) 0.950 ? . . C(11) H(11) 0.950 ? . . C(13) H(12) 0.950 ? . . C(13) H(13) 0.950 ? . . C(14) H(15) 0.950 ? . . C(17) H(16) 0.950 ? . . C(18) H(17) 0.950 ? . . C(19) H(18) 0.950 ? . . C(20) H(19) 0.950 ? . . 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 O(1) Cu(1) N(1) 95.18(16) ? . . . O(1) Cu(1) N(3) 160.78(17) ? . . . O(1) Cu(1) N(4) 82.37(16) ? . . . N(1) Cu(1) N(3) 92.03(17) ? . . . N(1) Cu(1) N(4) 162.93(19) ? . . . N(3) Cu(1) N(4) 95.70(17) ? . . . O(3) Cl(1) O(4) 109.9(2) ? . . . O(3) Cl(1) O(5) 109.6(3) ? . . . O(3) Cl(1) O(6) 109.1(2) ? . . . O(4) Cl(1) O(5) 109.4(3) ? . . . O(4) Cl(1) O(6) 110.8(3) ? . . . O(5) Cl(1) O(6) 108.1(2) ? . . . Cu(1) O(1) C(12) 113.5(3) ? . . . Cu(1) N(1) C(1) 119.1(3) ? . . . Cu(1) N(1) C(5) 121.9(3) ? . . . C(1) N(1) C(5) 118.4(4) ? . . . C(5) N(2) C(6) 129.6(4) ? . . . Cu(1) N(3) C(6) 122.6(3) ? . . . Cu(1) N(3) C(10) 118.8(3) ? . . . C(6) N(3) C(10) 118.2(4) ? . . . Cu(1) N(4) C(11) 105.9(2) ? . . . C(14) N(5) C(21) 109.9(5) ? . . . N(1) C(1) C(2) 121.8(5) ? . . . C(1) C(2) C(3) 118.5(5) ? . . . C(2) C(3) C(4) 121.5(5) ? . . . C(3) C(4) C(5) 118.3(5) ? . . . N(1) C(5) N(2) 121.4(4) ? . . . N(1) C(5) C(4) 121.5(4) ? . . . N(2) C(5) C(4) 117.1(4) ? . . . N(2) C(6) N(3) 121.3(4) ? . . . N(2) C(6) C(7) 116.8(4) ? . . . N(3) C(6) C(7) 122.0(4) ? . . . C(6) C(7) C(8) 118.8(4) ? . . . C(7) C(8) C(9) 120.3(4) ? . . . C(8) C(9) C(10) 117.9(4) ? . . . N(3) C(10) C(9) 122.5(4) ? . . . N(4) C(11) C(12) 106.2(3) ? . . . N(4) C(11) C(13) 110.7(3) ? . . . C(12) C(11) C(13) 111.7(3) ? . . . O(1) C(12) O(2) 123.0(4) ? . . . O(1) C(12) C(11) 117.3(4) ? . . . O(2) C(12) C(11) 119.7(4) ? . . . C(11) C(13) C(15) 114.3(4) ? . . . N(5) C(14) C(15) 109.4(6) ? . . . C(13) C(15) C(14) 124.6(5) ? . . . C(13) C(15) C(16) 128.1(5) ? . . . C(14) C(15) C(16) 107.2(5) ? . . . C(15) C(16) C(17) 134.3(5) ? . . . C(15) C(16) C(21) 105.5(4) ? . . . C(17) C(16) C(21) 120.1(5) ? . . . C(16) C(17) C(18) 119.3(6) ? . . . C(17) C(18) C(19) 120.4(6) ? . . . C(18) C(19) C(20) 122.4(7) ? . . . C(19) C(20) C(21) 117.8(6) ? . . . N(5) C(21) C(16) 107.9(5) ? . . . N(5) C(21) C(20) 132.1(5) ? . . . C(16) C(21) C(20) 119.9(5) ? . . . Cu(1) N(4) H(9) 110.5 ? . . . Cu(1) N(4) H(10) 110.1 ? . . . C(11) N(4) H(9) 110.5 ? . . . C(11) N(4) H(10) 110.3 ? . . . H(9) N(4) H(10) 109.5 ? . . . C(14) N(5) H(14) 125.3 ? . . . C(21) N(5) H(14) 124.8 ? . . . N(1) C(1) H(1) 119.0 ? . . . C(2) C(1) H(1) 119.3 ? . . . C(1) C(2) H(2) 120.3 ? . . . C(3) C(2) H(2) 121.2 ? . . . C(2) C(3) H(3) 119.3 ? . . . C(4) C(3) H(3) 119.2 ? . . . C(3) C(4) H(4) 121.3 ? . . . C(5) C(4) H(4) 120.3 ? . . . C(6) C(7) H(5) 120.5 ? . . . C(8) C(7) H(5) 120.8 ? . . . C(7) C(8) H(6) 120.1 ? . . . C(9) C(8) H(6) 119.6 ? . . . C(8) C(9) H(7) 121.4 ? . . . C(10) C(9) H(7) 120.8 ? . . . N(3) C(10) H(8) 118.7 ? . . . C(9) C(10) H(8) 118.8 ? . . . N(4) C(11) H(11) 109.6 ? . . . C(12) C(11) H(11) 109.3 ? . . . C(13) C(11) H(11) 109.2 ? . . . C(11) C(13) H(12) 108.4 ? . . . C(11) C(13) H(13) 108.2 ? . . . C(15) C(13) H(12) 108.4 ? . . . C(15) C(13) H(13) 108.0 ? . . . H(12) C(13) H(13) 109.5 ? . . . N(5) C(14) H(15) 125.4 ? . . . C(15) C(14) H(15) 125.2 ? . . . C(16) C(17) H(16) 120.6 ? . . . C(18) C(17) H(16) 120.1 ? . . . C(17) C(18) H(17) 119.5 ? . . . C(19) C(18) H(17) 120.0 ? . . . C(18) C(19) H(18) 118.9 ? . . . C(20) C(19) H(18) 118.7 ? . . . C(19) C(20) H(19) 121.8 ? . . . C(21) C(20) H(19) 120.4 ? . . . 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 O(1) Cu(1) N(1) C(1) -2.2(4) ? . . . . O(1) Cu(1) N(1) C(5) 168.1(4) ? . . . . N(1) Cu(1) O(1) C(12) -141.0(3) ? . . . . O(1) Cu(1) N(3) C(6) 143.2(4) ? . . . . O(1) Cu(1) N(3) C(10) -44.3(7) ? . . . . N(3) Cu(1) O(1) C(12) 107.5(5) ? . . . . O(1) Cu(1) N(4) C(11) -33.4(3) ? . . . . N(4) Cu(1) O(1) C(12) 22.0(3) ? . . . . N(1) Cu(1) N(3) C(6) 31.1(4) ? . . . . N(1) Cu(1) N(3) C(10) -156.4(4) ? . . . . N(3) Cu(1) N(1) C(1) 160.0(4) ? . . . . N(3) Cu(1) N(1) C(5) -29.7(4) ? . . . . N(1) Cu(1) N(4) C(11) 49.4(7) ? . . . . N(4) Cu(1) N(1) C(1) -83.0(7) ? . . . . N(4) Cu(1) N(1) C(5) 87.3(6) ? . . . . N(3) Cu(1) N(4) C(11) 165.9(3) ? . . . . N(4) Cu(1) N(3) C(6) -133.6(4) ? . . . . N(4) Cu(1) N(3) C(10) 38.9(4) ? . . . . Cu(1) O(1) C(12) O(2) 174.6(3) ? . . . . Cu(1) O(1) C(12) C(11) -4.3(5) ? . . . . Cu(1) N(1) C(1) C(2) 167.7(4) ? . . . . Cu(1) N(1) C(5) N(2) 12.4(6) ? . . . . Cu(1) N(1) C(5) C(4) -168.5(4) ? . . . . C(1) N(1) C(5) N(2) -177.2(4) ? . . . . C(1) N(1) C(5) C(4) 1.9(7) ? . . . . C(5) N(1) C(1) C(2) -3.0(7) ? . . . . C(5) N(2) C(6) N(3) -16.3(8) ? . . . . C(5) N(2) C(6) C(7) 164.1(5) ? . . . . C(6) N(2) C(5) N(1) 17.5(8) ? . . . . C(6) N(2) C(5) C(4) -161.7(5) ? . . . . Cu(1) N(3) C(6) N(2) -14.8(6) ? . . . . Cu(1) N(3) C(6) C(7) 164.8(4) ? . . . . Cu(1) N(3) C(10) C(9) -169.6(4) ? . . . . C(6) N(3) C(10) C(9) 3.2(8) ? . . . . C(10) N(3) C(6) N(2) 172.7(5) ? . . . . C(10) N(3) C(6) C(7) -7.7(7) ? . . . . Cu(1) N(4) C(11) C(12) 37.8(4) ? . . . . Cu(1) N(4) C(11) C(13) -83.6(4) ? . . . . C(14) N(5) C(21) C(16) 1.9(6) ? . . . . C(14) N(5) C(21) C(20) -174.4(6) ? . . . . C(21) N(5) C(14) C(15) -1.4(7) ? . . . . N(1) C(1) C(2) C(3) 2.6(9) ? . . . . C(1) C(2) C(3) C(4) -1.1(10) ? . . . . C(2) C(3) C(4) C(5) 0.1(8) ? . . . . C(3) C(4) C(5) N(1) -0.5(7) ? . . . . C(3) C(4) C(5) N(2) 178.6(5) ? . . . . N(2) C(6) C(7) C(8) -173.6(5) ? . . . . N(3) C(6) C(7) C(8) 6.7(8) ? . . . . C(6) C(7) C(8) C(9) -1.1(9) ? . . . . C(7) C(8) C(9) C(10) -3.1(9) ? . . . . C(8) C(9) C(10) N(3) 2.1(9) ? . . . . N(4) C(11) C(12) O(1) -23.4(5) ? . . . . N(4) C(11) C(12) O(2) 157.7(4) ? . . . . N(4) C(11) C(13) C(15) 61.7(5) ? . . . . C(12) C(11) C(13) C(15) -56.4(5) ? . . . . C(13) C(11) C(12) O(1) 97.4(5) ? . . . . C(13) C(11) C(12) O(2) -81.5(5) ? . . . . C(11) C(13) C(15) C(14) 88.6(6) ? . . . . C(11) C(13) C(15) C(16) -96.7(6) ? . . . . N(5) C(14) C(15) C(13) 175.9(5) ? . . . . N(5) C(14) C(15) C(16) 0.3(5) ? . . . . C(13) C(15) C(16) C(17) 2.5(10) ? . . . . C(13) C(15) C(16) C(21) -174.6(5) ? . . . . C(14) C(15) C(16) C(17) 177.9(6) ? . . . . C(14) C(15) C(16) C(21) 0.8(6) ? . . . . C(15) C(16) C(17) C(18) -176.2(6) ? . . . . C(15) C(16) C(21) N(5) -1.6(6) ? . . . . C(15) C(16) C(21) C(20) 175.2(4) ? . . . . C(17) C(16) C(21) N(5) -179.2(5) ? . . . . C(17) C(16) C(21) C(20) -2.4(8) ? . . . . C(21) C(16) C(17) C(18) 0.6(8) ? . . . . C(16) C(17) C(18) C(19) 1.4(10) ? . . . . C(17) C(18) C(19) C(20) -1.7(11) ? . . . . C(18) C(19) C(20) C(21) -0.1(9) ? . . . . C(19) C(20) C(21) N(5) 178.1(6) ? . . . . C(19) C(20) C(21) C(16) 2.1(8) ? . . . . #============================================================================== data__[Cu((CONH2)2bpy)(phe)]ClO4.H2O(2) _database_code_depnum_ccdc_archive 'CCDC 611927' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C21 H22 Cl Cu N5 O9 ' _chemical_formula_moiety '[Cu((CONH2)2bpy)(phe)]ClO4.H2O(2)' _chemical_formula_weight 587.43 #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,-Z #------------------------------------------------------------------------------ _cell_length_a 9.9415(8) _cell_length_b 11.9758(7) _cell_length_c 10.0268(8) _cell_angle_alpha 90.0000 _cell_angle_beta 94.766(7) _cell_angle_gamma 90.0000 _cell_volume 1189.64(15) _cell_formula_units_Z 2 _cell_measurement_reflns_used 21 _cell_measurement_theta_min 35.5 _cell_measurement_theta_max 39.5 _cell_measurement_temperature 296.1 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour blue _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 1.640 _exptl_crystal_F_000 602.00 _exptl_absorpt_coefficient_mu 2.896 _exptl_absorpt_correction_type DIFABS #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 1985 _diffrn_reflns_av_R_equivalents 0.160 _diffrn_reflns_theta_max 60.04 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 60.04 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 3 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% -1.48 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement 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 1866 _reflns_number_gt 1883 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1256 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 1985 _refine_ls_number_parameters 354 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0031Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.65 _refine_diff_density_min -0.68 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu -1.965 0.589 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.049 0.032 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; C C 0.018 0.009 ; 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 0.031 0.018 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.364 0.702 ; 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 Cu(1) Cu -0.20642(6) 0.77127(12) 0.30000(6) 0.0330(2) Uani 1.00 1 d . . . Cl(1) Cl 0.28509(18) 0.73967(17) 0.70523(19) 0.0560(4) Uani 1.00 1 d . . . O(1) O 0.2208(4) 0.3250(4) 0.4601(4) 0.0520(12) Uani 1.00 1 d . . . O(2) O 0.3646(6) 1.1291(5) 0.3698(6) 0.0712(19) Uani 1.00 1 d . . . O(3) O -0.3585(4) 0.6725(3) 0.3113(4) 0.0392(11) Uani 1.00 1 d . . . O(4) O -0.5642(4) 0.6382(4) 0.2203(4) 0.0538(13) Uani 1.00 1 d . . . O(5) O 0.3670(7) 0.7852(12) 0.6160(10) 0.171(4) Uani 1.00 1 d . . . O(6) O 0.2853(9) 0.7964(12) 0.8241(10) 0.196(6) Uani 1.00 1 d . . . O(7) O 0.3376(8) 0.6361(6) 0.7337(12) 0.132(3) Uani 1.00 1 d . . . O(8) O 0.1503(5) 0.7295(5) 0.6460(6) 0.0749(17) Uani 1.00 1 d . . . O(9) O 0.2927(7) 0.5465(5) 0.9978(6) 0.081(2) Uani 1.00 1 d . . . N(1) N -0.0712(4) 0.6497(4) 0.3385(4) 0.0301(12) Uani 1.00 1 d . . . N(2) N 0.3710(5) 0.4374(5) 0.3694(6) 0.0507(17) Uani 1.00 1 d . . . N(3) N 0.4455(4) 0.9556(4) 0.3445(6) 0.0527(16) Uani 1.00 1 d . . . N(4) N -0.0401(4) 0.8656(4) 0.3069(4) 0.0301(11) Uani 1.00 1 d . . . N(5) N -0.3427(5) 0.8709(4) 0.2033(5) 0.0413(13) Uani 1.00 1 d . . . C(1) C -0.0972(6) 0.5413(5) 0.3465(6) 0.0378(15) Uani 1.00 1 d . . . C(2) C 0.0040(5) 0.4622(5) 0.3661(5) 0.0358(14) Uani 1.00 1 d . . . C(3) C 0.2495(6) 0.4141(5) 0.4044(5) 0.0387(15) Uani 1.00 1 d . . . C(4) C 0.1380(6) 0.4973(4) 0.3748(5) 0.0320(14) Uani 1.00 1 d . . . C(5) C 0.1642(6) 0.6112(5) 0.3614(5) 0.0347(15) Uani 1.00 1 d . . . C(6) C 0.0583(5) 0.6837(5) 0.3430(5) 0.0303(14) Uani 1.00 1 d . . . C(7) C 0.0758(5) 0.8067(5) 0.3292(5) 0.0313(13) Uani 1.00 1 d . . . C(8) C 0.2000(5) 0.8567(5) 0.3433(5) 0.0349(14) Uani 1.00 1 d . . . C(9) C 0.3493(6) 1.0197(5) 0.3498(6) 0.0397(17) Uani 1.00 1 d . . . C(10) C 0.2106(6) 0.9736(4) 0.3361(5) 0.0330(14) Uani 1.00 1 d . . . C(11) C 0.0914(6) 1.0325(5) 0.3150(6) 0.0363(15) Uani 1.00 1 d . . . C(12) C -0.0309(6) 0.9758(5) 0.2993(6) 0.0382(15) Uani 1.00 1 d . . . C(13) C -0.4452(5) 0.7944(5) 0.1386(6) 0.0453(17) Uani 1.00 1 d . . . C(14) C -0.4592(5) 0.6937(5) 0.2304(5) 0.0377(15) Uani 1.00 1 d . . . C(15) C -0.4091(6) 0.7561(8) -0.0009(6) 0.063(2) Uani 1.00 1 d . . . C(16) C -0.2788(7) 0.6939(7) 0.0007(6) 0.054(2) Uani 1.00 1 d . . . C(17) C -0.1566(8) 0.7471(7) -0.0128(7) 0.063(2) Uani 1.00 1 d . . . C(18) C -0.0374(8) 0.6847(13) -0.0071(8) 0.086(3) Uani 1.00 1 d . . . C(19) C -0.0393(11) 0.5738(11) 0.0127(8) 0.085(3) Uani 1.00 1 d . . . C(20) C -0.1585(13) 0.5202(9) 0.0251(8) 0.085(3) Uani 1.00 1 d . . . C(21) C -0.2776(10) 0.5790(8) 0.0188(7) 0.069(2) Uani 1.00 1 d . . . H(1) H -0.1884 0.5169 0.3369 0.045 Uiso 1.00 1 c R . . H(2) H -0.0164 0.3853 0.3768 0.043 Uiso 1.00 1 c R . . H(3) H 0.4445 0.3875 0.3881 0.061 Uiso 1.00 1 c R . . H(4) H 0.3846 0.5061 0.3252 0.061 Uiso 1.00 1 c R . . H(5) H 0.2547 0.6372 0.3632 0.042 Uiso 1.00 1 c R . . H(6) H 0.2795 0.8127 0.3561 0.042 Uiso 1.00 1 c R . . H(7) H 0.4296 0.8779 0.3322 0.064 Uiso 1.00 1 c R . . H(8) H 0.5352 0.9835 0.3521 0.065 Uiso 1.00 1 c R . . H(9) H 0.0940 1.1116 0.3101 0.044 Uiso 1.00 1 c R . . H(10) H -0.1126 1.0165 0.2827 0.046 Uiso 1.00 1 c R . . H(11) H -0.3020 0.9136 0.1376 0.049 Uiso 1.00 1 c R . . H(12) H -0.3819 0.9197 0.2639 0.049 Uiso 1.00 1 c R . . H(13) H -0.5292 0.8326 0.1290 0.054 Uiso 1.00 1 c R . . H(14) H -0.4019 0.8203 -0.0556 0.075 Uiso 1.00 1 c R . . H(15) H -0.4796 0.7095 -0.0388 0.075 Uiso 1.00 1 c R . . H(16) H -0.1578 0.8256 -0.0263 0.076 Uiso 1.00 1 c R . . H(17) H 0.0454 0.7212 -0.0196 0.104 Uiso 1.00 1 c R . . H(18) H 0.0419 0.5317 0.0222 0.103 Uiso 1.00 1 c R . . H(19) H -0.1580 0.4415 0.0377 0.103 Uiso 1.00 1 c R . . H(20) H -0.3593 0.5395 0.0274 0.084 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 Cu(1) 0.0239(4) 0.0279(4) 0.0470(4) -0.0001(3) 0.0020(2) 0.0047(3) Cl(1) 0.0486(8) 0.0417(10) 0.0756(10) 0.0066(7) -0.0078(7) 0.0007(7) O(1) 0.053(2) 0.032(2) 0.074(2) 0.011(2) 0.022(2) 0.014(2) O(2) 0.063(3) 0.051(3) 0.101(4) -0.010(2) 0.012(3) -0.007(2) O(3) 0.0273(19) 0.037(2) 0.054(2) -0.0067(19) 0.0040(17) 0.0070(19) O(4) 0.038(2) 0.057(3) 0.066(2) -0.014(2) 0.002(2) 0.003(2) O(5) 0.080(4) 0.251(14) 0.176(8) -0.071(7) -0.028(5) 0.124(9) O(6) 0.133(7) 0.28(2) 0.165(8) 0.088(10) -0.063(7) -0.145(11) O(7) 0.071(4) 0.058(4) 0.266(11) 0.024(4) 0.010(5) 0.038(6) O(8) 0.057(3) 0.063(3) 0.101(4) 0.011(3) -0.021(3) -0.005(3) O(9) 0.093(4) 0.067(3) 0.082(3) -0.011(3) 0.006(3) -0.024(3) N(1) 0.027(2) 0.027(2) 0.036(2) 0.000(2) 0.0020(18) 0.0028(19) N(2) 0.039(3) 0.037(3) 0.078(4) 0.009(2) 0.014(2) 0.016(2) N(3) 0.020(2) 0.021(2) 0.120(5) -0.000(2) 0.022(2) -0.012(3) N(4) 0.025(2) 0.029(2) 0.036(2) 0.001(2) 0.0037(17) 0.003(2) N(5) 0.031(2) 0.040(2) 0.053(2) -0.000(2) 0.002(2) 0.010(2) C(1) 0.036(3) 0.026(3) 0.052(3) -0.005(2) 0.003(2) -0.000(2) C(2) 0.039(3) 0.024(2) 0.044(3) -0.001(2) 0.002(2) 0.004(2) C(3) 0.042(3) 0.033(3) 0.042(2) 0.005(2) 0.009(2) 0.005(2) C(4) 0.038(3) 0.019(2) 0.039(2) 0.001(2) 0.006(2) 0.007(2) C(5) 0.031(3) 0.026(3) 0.047(3) -0.001(2) 0.005(2) 0.002(2) C(6) 0.029(2) 0.025(2) 0.037(2) -0.003(2) 0.005(2) -0.001(2) C(7) 0.026(2) 0.028(2) 0.039(2) 0.002(2) 0.003(2) 0.006(2) C(8) 0.028(2) 0.025(2) 0.052(3) -0.002(2) 0.007(2) 0.003(2) C(9) 0.035(3) 0.025(3) 0.059(3) -0.003(2) 0.008(2) -0.002(2) C(10) 0.035(3) 0.025(3) 0.039(2) 0.000(2) 0.005(2) 0.003(2) C(11) 0.038(3) 0.024(2) 0.048(3) 0.002(2) 0.009(2) 0.001(2) C(12) 0.033(3) 0.028(3) 0.055(3) 0.005(2) 0.007(2) 0.002(2) C(13) 0.024(2) 0.045(4) 0.065(3) -0.000(2) -0.003(2) 0.010(3) C(14) 0.026(2) 0.044(3) 0.044(3) -0.000(2) 0.007(2) -0.003(2) C(15) 0.048(3) 0.092(6) 0.046(3) -0.024(4) -0.008(2) 0.020(4) C(16) 0.055(4) 0.072(5) 0.035(3) -0.013(3) 0.007(2) -0.008(3) C(17) 0.061(4) 0.068(5) 0.061(3) -0.006(4) 0.014(3) -0.011(3) C(18) 0.062(5) 0.140(11) 0.058(4) -0.008(6) 0.018(4) -0.029(5) C(19) 0.099(8) 0.099(8) 0.058(4) 0.026(7) 0.015(4) -0.017(5) C(20) 0.131(9) 0.062(5) 0.064(5) 0.007(6) 0.027(5) -0.006(4) C(21) 0.086(6) 0.066(5) 0.059(4) -0.014(5) 0.023(4) -0.009(4) #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction CrystalStructure _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.7.0' #============================================================================== # 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 Cu(1) O(3) 1.931(4) ? . . Cu(1) N(1) 1.998(4) ? . . Cu(1) N(4) 1.999(5) ? . . Cu(1) N(5) 1.995(5) ? . . Cl(1) O(5) 1.371(11) ? . . Cl(1) O(6) 1.372(12) ? . . Cl(1) O(7) 1.366(8) ? . . Cl(1) O(8) 1.425(6) ? . . O(1) C(3) 1.249(8) ? . . O(2) C(9) 1.331(9) ? . . O(3) C(14) 1.261(6) ? . . O(4) C(14) 1.235(7) ? . . N(1) C(1) 1.328(7) ? . . N(1) C(6) 1.347(7) ? . . N(2) C(3) 1.316(8) ? . . N(3) C(9) 1.231(8) ? . . N(4) C(7) 1.353(7) ? . . N(4) C(12) 1.326(8) ? . . N(5) C(13) 1.479(8) ? . . C(1) C(2) 1.383(8) ? . . C(2) C(4) 1.393(8) ? . . C(3) C(4) 1.502(8) ? . . C(4) C(5) 1.398(8) ? . . C(5) C(6) 1.366(8) ? . . C(6) C(7) 1.491(8) ? . . C(7) C(8) 1.369(8) ? . . C(8) C(10) 1.406(8) ? . . C(9) C(10) 1.482(8) ? . . C(10) C(11) 1.380(8) ? . . C(11) C(12) 1.389(8) ? . . C(13) C(14) 1.531(9) ? . . C(13) C(15) 1.542(9) ? . . C(15) C(16) 1.493(11) ? . . C(16) C(17) 1.388(11) ? . . C(16) C(21) 1.388(13) ? . . C(17) C(18) 1.398(13) ? . . C(18) C(19) 1.34(2) ? . . C(19) C(20) 1.363(17) ? . . C(20) C(21) 1.375(16) ? . . N(2) H(3) 0.950 ? . . N(2) H(4) 0.950 ? . . N(3) H(7) 0.950 ? . . N(3) H(8) 0.950 ? . . N(5) H(11) 0.950 ? . . N(5) H(12) 0.950 ? . . C(1) H(1) 0.950 ? . . C(2) H(2) 0.950 ? . . C(5) H(5) 0.950 ? . . C(8) H(6) 0.950 ? . . C(11) H(9) 0.950 ? . . C(12) H(10) 0.950 ? . . C(13) H(13) 0.950 ? . . C(15) H(14) 0.950 ? . . C(15) H(15) 0.950 ? . . C(17) H(16) 0.950 ? . . C(18) H(17) 0.950 ? . . C(19) H(18) 0.950 ? . . C(20) H(19) 0.950 ? . . C(21) H(20) 0.950 ? . . 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 O(3) Cu(1) N(1) 93.42(19) ? . . . O(3) Cu(1) N(4) 173.65(18) ? . . . O(3) Cu(1) N(5) 83.8(2) ? . . . N(1) Cu(1) N(4) 82.2(2) ? . . . N(1) Cu(1) N(5) 161.6(2) ? . . . N(4) Cu(1) N(5) 101.9(2) ? . . . O(5) Cl(1) O(6) 114.3(7) ? . . . O(5) Cl(1) O(7) 105.0(7) ? . . . O(5) Cl(1) O(8) 110.5(4) ? . . . O(6) Cl(1) O(7) 107.2(7) ? . . . O(6) Cl(1) O(8) 109.8(4) ? . . . O(7) Cl(1) O(8) 109.8(4) ? . . . Cu(1) O(3) C(14) 115.0(4) ? . . . Cu(1) N(1) C(1) 126.4(3) ? . . . Cu(1) N(1) C(6) 114.3(3) ? . . . C(1) N(1) C(6) 119.0(5) ? . . . Cu(1) N(4) C(7) 113.7(4) ? . . . Cu(1) N(4) C(12) 128.4(4) ? . . . C(7) N(4) C(12) 117.8(5) ? . . . Cu(1) N(5) C(13) 105.0(4) ? . . . N(1) C(1) C(2) 122.3(5) ? . . . C(1) C(2) C(4) 118.8(5) ? . . . O(1) C(3) N(2) 123.3(6) ? . . . O(1) C(3) C(4) 117.6(5) ? . . . N(2) C(3) C(4) 119.1(5) ? . . . C(2) C(4) C(3) 119.9(5) ? . . . C(2) C(4) C(5) 118.3(5) ? . . . C(3) C(4) C(5) 121.7(5) ? . . . C(4) C(5) C(6) 119.0(5) ? . . . N(1) C(6) C(5) 122.4(5) ? . . . N(1) C(6) C(7) 114.5(5) ? . . . C(5) C(6) C(7) 123.1(5) ? . . . N(4) C(7) C(6) 115.2(5) ? . . . N(4) C(7) C(8) 122.5(5) ? . . . C(6) C(7) C(8) 122.3(5) ? . . . C(7) C(8) C(10) 120.1(5) ? . . . O(2) C(9) N(3) 122.8(6) ? . . . O(2) C(9) C(10) 118.3(5) ? . . . N(3) C(9) C(10) 118.9(5) ? . . . C(8) C(10) C(9) 116.1(5) ? . . . C(8) C(10) C(11) 116.7(5) ? . . . C(9) C(10) C(11) 127.2(5) ? . . . C(10) C(11) C(12) 120.0(5) ? . . . N(4) C(12) C(11) 122.9(5) ? . . . N(5) C(13) C(14) 108.5(4) ? . . . N(5) C(13) C(15) 112.2(5) ? . . . C(14) C(13) C(15) 110.5(6) ? . . . O(3) C(14) O(4) 124.4(6) ? . . . O(3) C(14) C(13) 116.1(5) ? . . . O(4) C(14) C(13) 119.6(5) ? . . . C(13) C(15) C(16) 113.9(5) ? . . . C(15) C(16) C(17) 122.4(8) ? . . . C(15) C(16) C(21) 119.6(7) ? . . . C(17) C(16) C(21) 118.0(7) ? . . . C(16) C(17) C(18) 119.8(9) ? . . . C(17) C(18) C(19) 120.8(9) ? . . . C(18) C(19) C(20) 120.2(10) ? . . . C(19) C(20) C(21) 120.4(10) ? . . . C(16) C(21) C(20) 120.8(9) ? . . . C(3) N(2) H(3) 121.5 ? . . . C(3) N(2) H(4) 118.5 ? . . . H(3) N(2) H(4) 120.0 ? . . . C(9) N(3) H(7) 119.7 ? . . . C(9) N(3) H(8) 120.3 ? . . . H(7) N(3) H(8) 120.0 ? . . . Cu(1) N(5) H(11) 110.3 ? . . . Cu(1) N(5) H(12) 110.8 ? . . . C(13) N(5) H(11) 110.3 ? . . . C(13) N(5) H(12) 110.9 ? . . . H(11) N(5) H(12) 109.5 ? . . . N(1) C(1) H(1) 118.9 ? . . . C(2) C(1) H(1) 118.7 ? . . . C(1) C(2) H(2) 121.3 ? . . . C(4) C(2) H(2) 119.8 ? . . . C(4) C(5) H(5) 120.1 ? . . . C(6) C(5) H(5) 120.8 ? . . . C(7) C(8) H(6) 120.3 ? . . . C(10) C(8) H(6) 119.6 ? . . . C(10) C(11) H(9) 119.4 ? . . . C(12) C(11) H(9) 120.6 ? . . . N(4) C(12) H(10) 117.3 ? . . . C(11) C(12) H(10) 119.8 ? . . . N(5) C(13) H(13) 108.3 ? . . . C(14) C(13) H(13) 108.5 ? . . . C(15) C(13) H(13) 108.7 ? . . . C(13) C(15) H(14) 108.5 ? . . . C(13) C(15) H(15) 108.5 ? . . . C(16) C(15) H(14) 107.6 ? . . . C(16) C(15) H(15) 108.7 ? . . . H(14) C(15) H(15) 109.5 ? . . . C(16) C(17) H(16) 117.9 ? . . . C(18) C(17) H(16) 122.3 ? . . . C(17) C(18) H(17) 119.3 ? . . . C(19) C(18) H(17) 119.8 ? . . . C(18) C(19) H(18) 121.2 ? . . . C(20) C(19) H(18) 118.6 ? . . . C(19) C(20) H(19) 119.0 ? . . . C(21) C(20) H(19) 120.6 ? . . . C(16) C(21) H(20) 120.5 ? . . . C(20) C(21) H(20) 118.6 ? . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(3) Cu(1) N(1) C(1) 8.0(5) ? . . . . O(3) Cu(1) N(1) C(6) -178.8(3) ? . . . . N(1) Cu(1) O(3) C(14) -144.0(4) ? . . . . O(3) Cu(1) N(4) C(7) 48(2) ? . . . . O(3) Cu(1) N(4) C(12) -128.8(17) ? . . . . N(4) Cu(1) O(3) C(14) 170.4(17) ? . . . . O(3) Cu(1) N(5) C(13) -29.0(3) ? . . . . N(5) Cu(1) O(3) C(14) 17.7(4) ? . . . . N(1) Cu(1) N(4) C(7) 1.4(3) ? . . . . N(1) Cu(1) N(4) C(12) -174.9(5) ? . . . . N(4) Cu(1) N(1) C(1) -176.6(5) ? . . . . N(4) Cu(1) N(1) C(6) -3.4(3) ? . . . . N(1) Cu(1) N(5) C(13) 53.1(8) ? . . . . N(5) Cu(1) N(1) C(1) -72.6(8) ? . . . . N(5) Cu(1) N(1) C(6) 100.6(7) ? . . . . N(4) Cu(1) N(5) C(13) 154.0(3) ? . . . . N(5) Cu(1) N(4) C(7) -160.3(3) ? . . . . N(5) Cu(1) N(4) C(12) 23.4(5) ? . . . . Cu(1) O(3) C(14) O(4) 178.0(5) ? . . . . Cu(1) O(3) C(14) C(13) -0.8(6) ? . . . . Cu(1) N(1) C(1) C(2) 176.2(4) ? . . . . Cu(1) N(1) C(6) C(5) -176.6(4) ? . . . . Cu(1) N(1) C(6) C(7) 4.6(5) ? . . . . C(1) N(1) C(6) C(5) -2.9(8) ? . . . . C(1) N(1) C(6) C(7) 178.3(5) ? . . . . C(6) N(1) C(1) C(2) 3.3(8) ? . . . . Cu(1) N(4) C(7) C(6) 0.6(6) ? . . . . Cu(1) N(4) C(7) C(8) -177.0(4) ? . . . . Cu(1) N(4) C(12) C(11) 175.3(4) ? . . . . C(7) N(4) C(12) C(11) -0.9(8) ? . . . . C(12) N(4) C(7) C(6) 177.3(5) ? . . . . C(12) N(4) C(7) C(8) -0.3(7) ? . . . . Cu(1) N(5) C(13) C(14) 34.6(5) ? . . . . Cu(1) N(5) C(13) C(15) -87.8(5) ? . . . . N(1) C(1) C(2) C(4) -1.4(9) ? . . . . C(1) C(2) C(4) C(3) 176.3(5) ? . . . . C(1) C(2) C(4) C(5) -0.9(8) ? . . . . O(1) C(3) C(4) C(2) -21.8(8) ? . . . . O(1) C(3) C(4) C(5) 155.4(5) ? . . . . N(2) C(3) C(4) C(2) 157.5(5) ? . . . . N(2) C(3) C(4) C(5) -25.4(8) ? . . . . C(2) C(4) C(5) C(6) 1.3(8) ? . . . . C(3) C(4) C(5) C(6) -175.9(5) ? . . . . C(4) C(5) C(6) N(1) 0.6(8) ? . . . . C(4) C(5) C(6) C(7) 179.3(5) ? . . . . N(1) C(6) C(7) N(4) -3.5(7) ? . . . . N(1) C(6) C(7) C(8) 174.2(5) ? . . . . C(5) C(6) C(7) N(4) 177.8(5) ? . . . . C(5) C(6) C(7) C(8) -4.6(8) ? . . . . N(4) C(7) C(8) C(10) 0.7(8) ? . . . . C(6) C(7) C(8) C(10) -176.8(5) ? . . . . C(7) C(8) C(10) C(9) -178.9(5) ? . . . . C(7) C(8) C(10) C(11) 0.2(6) ? . . . . O(2) C(9) C(10) C(8) -167.1(6) ? . . . . O(2) C(9) C(10) C(11) 14.0(9) ? . . . . N(3) C(9) C(10) C(8) 11.7(8) ? . . . . N(3) C(9) C(10) C(11) -167.2(6) ? . . . . C(8) C(10) C(11) C(12) -1.3(8) ? . . . . C(9) C(10) C(11) C(12) 177.6(5) ? . . . . C(10) C(11) C(12) N(4) 1.8(9) ? . . . . N(5) C(13) C(14) O(3) -24.1(7) ? . . . . N(5) C(13) C(14) O(4) 157.1(5) ? . . . . N(5) C(13) C(15) C(16) 60.6(9) ? . . . . C(14) C(13) C(15) C(16) -60.6(8) ? . . . . C(15) C(13) C(14) O(3) 99.4(6) ? . . . . C(15) C(13) C(14) O(4) -79.5(6) ? . . . . C(13) C(15) C(16) C(17) -90.5(8) ? . . . . C(13) C(15) C(16) C(21) 88.3(8) ? . . . . C(15) C(16) C(17) C(18) 178.4(6) ? . . . . C(15) C(16) C(21) C(20) -177.9(6) ? . . . . C(17) C(16) C(21) C(20) 1.0(10) ? . . . . C(21) C(16) C(17) C(18) -0.5(8) ? . . . . C(16) C(17) C(18) C(19) -0.6(10) ? . . . . C(17) C(18) C(19) C(20) 1.2(13) ? . . . . C(18) C(19) C(20) C(21) -0.6(11) ? . . . . C(19) C(20) C(21) C(16) -0.5(10) ? . . . . #============================================================================== # End of CIF #==============================================================================