Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Kinoshita, Isamu' 'Collins, Terrence J.' 'Isobe, Kiyoshi' 'Nishioka, Takanori' 'Tanaka, Rika' 'Wright, L. James' 'Yano, Toshihiro' _publ_contact_author_name 'Prof Isamu Kinoshita' _publ_contact_author_address ; Molecular Materials Science Osaka City University 3-3-138 Sugimoto, Sumiyoshi-ku Osaka 558-8585 JAPAN ; _publ_contact_author_email 'ISAMU@SCI.OSAKA-CU.AC.JP' _publ_section_title ; Mononuclear - Dinuclear Helicate Switching Behavior of N,N'-bis[(S)-1-2-(pyridyl)ethyl]-pyridine-2,6-dicarboxamidatecopper(II) via a Deprotonation-Protonation Process ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _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__M-helix2 _database_code_CSD 182239 _audit_creation_date 'Mon Jan 28 20:53:18 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #----------------------------------------------------------------------------- # CHEMICAL DATA _chemical_formula_sum 'C43 H40 Cl2 Cu2 N10 O2 ' _chemical_formula_moiety 'C43 H40 Cl2 Cu2 N10 O2 ' _chemical_formula_weight 926.85 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 14.804(2) _cell_length_b 16.226(3) _cell_length_c 17.416(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4183(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 13420 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'Block' _exptl_crystal_colour 'Green' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.195 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.577 _exptl_absorpt_correction_T_max 0.787 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 13420 _diffrn_reflns_av_R_equivalents 0.106 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). 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 9297 _reflns_number_gt 7825 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.1054 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7825 _refine_ls_number_parameters 568 _refine_ls_goodness_of_fit_ref 1.231 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0020 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 0.01(1) _refine_diff_density_max 0.50 _refine_diff_density_min -0.36 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) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Cu' 'Cu' 0.320 1.265 ;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) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu -0.52095(3) -0.62172(3) -0.12872(3) 0.0206(1) Uani 1.00 d . . . Cu(2) Cu -0.59984(3) -0.44573(3) -0.03035(3) 0.0184(1) Uani 1.00 d . . . Cl(1) Cl -0.3988(1) -0.5642(2) 0.3437(2) 0.069(1) Uani 0.81 d P . . Cl(2) Cl -0.3549(3) -0.7072(2) 0.4370(3) 0.104(2) Uani 0.81 d P . . Cl(3) Cl -0.3361(7) -0.660(2) 0.4664(6) 0.094(7) Uani 0.20 d P . . Cl(4) Cl -0.3969(7) -0.6040(9) 0.3169(7) 0.06188(4) Uiso 0.20 d P . . O(1) O -0.7758(2) -0.5989(2) -0.2103(2) 0.0354(9) Uani 1.00 d . . . O(2) O -0.3754(2) -0.3843(2) -0.1567(2) 0.0279(8) Uani 1.00 d . . . O(3) O -0.7733(2) -0.6246(2) 0.0398(2) 0.0255(7) Uani 1.00 d . . . O(4) O -0.3099(2) -0.5500(2) 0.0117(2) 0.0237(7) Uani 1.00 d . . . N(1) N -0.5311(2) -0.7356(2) -0.0793(2) 0.0237(9) Uani 1.00 d . . . N(2) N -0.6411(2) -0.6491(2) -0.1601(2) 0.0237(9) Uani 1.00 d . . . N(3) N -0.5696(2) -0.5006(2) -0.1752(2) 0.0186(8) Uani 1.00 d . . . N(4) N -0.4852(2) -0.4006(2) -0.0636(2) 0.0165(8) Uani 1.00 d . . . N(5) N -0.5490(2) -0.4039(2) 0.0781(2) 0.0202(8) Uani 1.00 d . . . N(6) N -0.6897(2) -0.3734(2) -0.0892(2) 0.0185(8) Uani 1.00 d . . . N(7) N -0.7089(2) -0.5056(2) -0.0089(2) 0.0175(8) Uani 1.00 d . . . N(8) N -0.5456(2) -0.5727(2) 0.0146(2) 0.0151(8) Uani 1.00 d . . . N(9) N -0.4028(2) -0.5891(2) -0.0884(2) 0.0166(7) Uani 1.00 d . . . N(10) N -0.4379(2) -0.6167(3) -0.2379(2) 0.0267(9) Uani 1.00 d . . . C(1) C -0.4667(3) -0.7753(3) -0.0384(3) 0.028(1) Uani 1.00 d . . . C(2) C -0.4832(3) -0.8476(3) -0.0004(3) 0.038(1) Uani 1.00 d . . . C(3) C -0.5690(3) -0.8813(4) -0.0035(3) 0.042(1) Uani 1.00 d . . . C(4) C -0.6342(3) -0.8426(3) -0.0470(3) 0.037(1) Uani 1.00 d . . . C(5) C -0.6144(3) -0.7697(3) -0.0842(3) 0.028(1) Uani 1.00 d . . . C(6) C -0.6821(2) -0.7250(3) -0.1324(3) 0.027(1) Uani 1.00 d . . . C(7) C -0.7167(3) -0.7801(3) -0.1983(3) 0.039(1) Uani 1.00 d . . . C(8) C -0.6931(3) -0.5945(3) -0.1953(3) 0.025(1) Uani 1.00 d . . . C(9) C -0.6423(3) -0.5182(3) -0.2191(3) 0.022(1) Uani 1.00 d . . . C(10) C -0.6651(3) -0.4708(3) -0.2812(3) 0.027(1) Uani 1.00 d . . . C(11) C -0.6108(3) -0.4067(3) -0.3037(3) 0.030(1) Uani 1.00 d . . . C(12) C -0.5363(3) -0.3883(3) -0.2586(3) 0.026(1) Uani 1.00 d . . . C(13) C -0.5199(3) -0.4343(3) -0.1928(2) 0.0213(10) Uani 1.00 d . . . C(14) C -0.4518(3) -0.4043(3) -0.1346(3) 0.0193(10) Uani 1.00 d . . . C(15) C -0.4241(2) -0.3684(3) -0.0048(2) 0.0179(9) Uani 1.00 d . . . C(16) C -0.4100(3) -0.2755(3) -0.0145(3) 0.033(1) Uani 1.00 d . . . C(17) C -0.4613(2) -0.3863(3) 0.0733(3) 0.0190(9) Uani 1.00 d . . . C(18) C -0.4069(3) -0.3838(3) 0.1384(3) 0.026(1) Uani 1.00 d . . . C(19) C -0.4459(3) -0.3953(4) 0.2093(3) 0.034(1) Uani 1.00 d . . . C(20) C -0.5373(3) -0.4090(3) 0.2145(3) 0.030(1) Uani 1.00 d . . . C(21) C -0.5858(3) -0.4138(3) 0.1486(3) 0.025(1) Uani 1.00 d . . . C(22) C -0.6705(3) -0.3051(3) -0.1296(3) 0.0228(10) Uani 1.00 d . . . C(23) C -0.7323(3) -0.2678(3) -0.1769(3) 0.029(1) Uani 1.00 d . . . C(24) C -0.8166(3) -0.3025(3) -0.1844(3) 0.027(1) Uani 1.00 d . . . C(25) C -0.8382(3) -0.3715(3) -0.1429(3) 0.024(1) Uani 1.00 d . . . C(26) C -0.7740(3) -0.4063(3) -0.0937(2) 0.0173(9) Uani 1.00 d . . . C(27) C -0.7934(2) -0.4778(3) -0.0422(3) 0.0182(10) Uani 1.00 d . . . C(28) C -0.8622(3) -0.4503(3) 0.0188(3) 0.028(1) Uani 1.00 d . . . C(29) C -0.7083(3) -0.5777(3) 0.0276(3) 0.0190(9) Uani 1.00 d . . . C(30) C -0.6159(2) -0.6014(3) 0.0559(3) 0.0188(10) Uani 1.00 d . . . C(31) C -0.6044(3) -0.6470(3) 0.1215(3) 0.033(1) Uani 1.00 d . . . C(32) C -0.5174(3) -0.6610(4) 0.1489(3) 0.046(2) Uani 1.00 d . . . C(33) C -0.4455(3) -0.6307(3) 0.1071(3) 0.032(1) Uani 1.00 d . . . C(34) C -0.4611(3) -0.5909(3) 0.0390(3) 0.0202(10) Uani 1.00 d . . . C(35) C -0.3844(2) -0.5724(3) -0.0162(3) 0.0173(9) Uani 1.00 d . . . C(36) C -0.3265(3) -0.5843(3) -0.1425(3) 0.022(1) Uani 1.00 d . . . C(37) C -0.2663(3) -0.6615(3) -0.1330(3) 0.028(1) Uani 1.00 d . . . C(38) C -0.3596(3) -0.5787(3) -0.2234(3) 0.0190(10) Uani 1.00 d . . . C(39) C -0.3092(3) -0.5408(3) -0.2806(3) 0.026(1) Uani 1.00 d . . . C(40) C -0.3388(3) -0.5418(3) -0.3546(3) 0.033(1) Uani 1.00 d . . . C(41) C -0.4210(3) -0.5822(3) -0.3713(3) 0.033(1) Uani 1.00 d . . . C(42) C -0.4667(3) -0.6172(3) -0.3110(3) 0.031(1) Uani 1.00 d . . . C(43) C -0.3177(4) -0.6113(6) 0.4026(5) 0.056(3) Uani 0.81 d P . . C(44) C -0.324(2) -0.666(2) 0.370(2) 0.056(3) Uani 0.20 d P . . H(1) H -0.4076 -0.7513 -0.0369 0.0333 Uiso 1.00 calc . . . H(2) H -0.4362 -0.8736 0.0287 0.0486 Uiso 1.00 calc . . . H(3) H -0.5817 -0.9312 0.0233 0.0515 Uiso 1.00 calc . . . H(4) H -0.6944 -0.8653 -0.0513 0.0424 Uiso 1.00 calc . . . H(5) H -0.7323 -0.7115 -0.1000 0.0352 Uiso 1.00 calc . . . H(6) H -0.6925 -0.8331 -0.1948 0.0540 Uiso 1.00 calc . . . H(7) H -0.6980 -0.7554 -0.2465 0.0540 Uiso 1.00 calc . . . H(8) H -0.7809 -0.7818 -0.1978 0.0540 Uiso 1.00 calc . . . H(9) H -0.7193 -0.4824 -0.3088 0.0344 Uiso 1.00 calc . . . H(10) H -0.6234 -0.3761 -0.3489 0.0380 Uiso 1.00 calc . . . H(11) H -0.4967 -0.3438 -0.2724 0.0333 Uiso 1.00 calc . . . H(12) H -0.3673 -0.3952 -0.0107 0.0220 Uiso 1.00 calc . . . H(13) H -0.3839 -0.2659 -0.0627 0.0393 Uiso 1.00 calc . . . H(14) H -0.3734 -0.2573 0.0256 0.0393 Uiso 1.00 calc . . . H(15) H -0.4682 -0.2503 -0.0118 0.0393 Uiso 1.00 calc . . . H(16) H -0.3439 -0.3737 0.1342 0.0318 Uiso 1.00 calc . . . H(17) H -0.4104 -0.3934 0.2547 0.0426 Uiso 1.00 calc . . . H(18) H -0.5656 -0.4159 0.2636 0.0381 Uiso 1.00 calc . . . H(19) H -0.6497 -0.4235 0.1528 0.0320 Uiso 1.00 calc . . . H(20) H -0.6120 -0.2813 -0.1249 0.0280 Uiso 1.00 calc . . . H(21) H -0.7173 -0.2199 -0.2062 0.0349 Uiso 1.00 calc . . . H(22) H -0.8607 -0.2786 -0.2174 0.0362 Uiso 1.00 calc . . . H(23) H -0.8963 -0.3954 -0.1479 0.0295 Uiso 1.00 calc . . . H(24) H -0.8187 -0.5207 -0.0725 0.0236 Uiso 1.00 calc . . . H(25) H -0.9141 -0.4273 -0.0051 0.0333 Uiso 1.00 calc . . . H(26) H -0.8356 -0.4106 0.0519 0.0333 Uiso 1.00 calc . . . H(27) H -0.8802 -0.4971 0.0485 0.0333 Uiso 1.00 calc . . . H(28) H -0.6545 -0.6693 0.1475 0.0406 Uiso 1.00 calc . . . H(29) H -0.5073 -0.6886 0.1969 0.0547 Uiso 1.00 calc . . . H(30) H -0.3848 -0.6382 0.1237 0.0407 Uiso 1.00 calc . . . H(31) H -0.2912 -0.5367 -0.1307 0.0281 Uiso 1.00 calc . . . H(32) H -0.3040 -0.7100 -0.1359 0.0341 Uiso 1.00 calc . . . H(33) H -0.2242 -0.6642 -0.1748 0.0341 Uiso 1.00 calc . . . H(34) H -0.2357 -0.6608 -0.0863 0.0341 Uiso 1.00 calc . . . H(35) H -0.2542 -0.5119 -0.2677 0.0311 Uiso 1.00 calc . . . H(36) H -0.3040 -0.5165 -0.3949 0.0432 Uiso 1.00 calc . . . H(37) H -0.4436 -0.5859 -0.4231 0.0410 Uiso 1.00 calc . . . H(38) H -0.5227 -0.6444 -0.3209 0.0346 Uiso 1.00 calc . . . 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) 0.0124(2) 0.0229(3) 0.0265(3) -0.0032(2) -0.0005(2) -0.0017(3) Cu(2) 0.0122(2) 0.0256(3) 0.0174(3) -0.0039(2) -0.0005(2) 0.0036(3) Cl(1) 0.041(1) 0.070(2) 0.096(2) -0.002(1) -0.013(1) 0.006(2) Cl(2) 0.088(2) 0.074(2) 0.149(4) -0.019(2) 0.036(2) 0.047(2) Cl(3) 0.053(6) 0.20(2) 0.031(5) -0.035(8) 0.011(4) 0.001(8) O(1) 0.015(2) 0.046(2) 0.046(2) -0.002(1) -0.006(1) -0.006(2) O(2) 0.017(1) 0.042(2) 0.024(2) -0.010(1) 0.004(1) 0.002(2) O(3) 0.017(1) 0.022(2) 0.037(2) -0.006(1) 0.004(1) 0.001(2) O(4) 0.012(1) 0.029(2) 0.030(2) 0.000(1) -0.004(1) -0.006(2) N(1) 0.019(2) 0.018(2) 0.034(2) -0.004(1) 0.008(2) -0.005(2) N(2) 0.015(2) 0.022(2) 0.033(2) -0.002(1) -0.001(2) -0.007(2) N(3) 0.015(2) 0.026(2) 0.015(2) -0.001(1) 0.000(1) -0.006(2) N(4) 0.013(2) 0.021(2) 0.015(2) -0.004(1) -0.004(1) -0.002(1) N(5) 0.015(2) 0.028(2) 0.018(2) -0.002(1) 0.001(1) -0.001(2) N(6) 0.017(2) 0.016(2) 0.022(2) 0.000(1) 0.002(1) -0.003(2) N(7) 0.011(2) 0.018(2) 0.023(2) 0.000(1) 0.003(1) 0.002(2) N(8) 0.015(2) 0.016(2) 0.015(2) -0.001(1) 0.000(1) 0.001(1) N(9) 0.010(2) 0.017(2) 0.022(2) 0.004(1) 0.004(2) 0.002(2) N(10) 0.019(2) 0.036(3) 0.024(2) -0.004(2) 0.000(2) -0.003(2) C(1) 0.023(2) 0.023(3) 0.039(3) 0.002(2) 0.007(2) -0.005(2) C(2) 0.036(3) 0.029(3) 0.050(4) 0.005(2) 0.015(3) 0.008(2) C(3) 0.044(3) 0.021(3) 0.061(4) 0.001(2) 0.020(3) 0.007(3) C(4) 0.025(2) 0.034(3) 0.051(4) -0.007(2) 0.017(2) -0.012(3) C(5) 0.023(2) 0.018(3) 0.042(3) -0.006(2) 0.015(2) -0.009(2) C(6) 0.011(2) 0.024(3) 0.046(3) -0.003(2) 0.007(2) -0.012(2) C(7) 0.029(3) 0.039(3) 0.050(4) -0.005(2) 0.001(2) -0.023(3) C(8) 0.016(2) 0.035(3) 0.025(3) -0.006(2) 0.002(2) -0.012(2) C(9) 0.015(2) 0.031(3) 0.021(3) 0.001(2) -0.001(2) -0.010(2) C(10) 0.020(2) 0.041(3) 0.021(3) 0.006(2) -0.006(2) -0.008(2) C(11) 0.033(3) 0.040(3) 0.017(2) 0.004(2) -0.004(2) 0.002(2) C(12) 0.026(2) 0.038(3) 0.014(2) -0.004(2) 0.000(2) -0.001(2) C(13) 0.015(2) 0.030(3) 0.019(2) -0.002(2) 0.003(2) -0.003(2) C(14) 0.017(2) 0.024(3) 0.017(2) -0.002(2) 0.001(2) 0.005(2) C(15) 0.015(2) 0.020(3) 0.019(2) -0.006(2) -0.002(2) 0.002(2) C(16) 0.044(3) 0.030(3) 0.023(3) -0.012(2) -0.006(2) 0.004(2) C(17) 0.017(2) 0.020(2) 0.020(2) -0.003(2) -0.002(2) -0.002(2) C(18) 0.020(2) 0.033(3) 0.025(3) -0.007(2) -0.008(2) -0.001(2) C(19) 0.029(2) 0.055(4) 0.017(3) -0.005(2) -0.004(2) 0.002(2) C(20) 0.034(3) 0.043(3) 0.014(3) -0.005(2) 0.001(2) -0.003(2) C(21) 0.020(2) 0.032(3) 0.023(3) -0.003(2) 0.004(2) 0.000(2) C(22) 0.029(2) 0.022(3) 0.017(2) 0.000(2) 0.003(2) -0.002(2) C(23) 0.039(3) 0.021(3) 0.027(3) 0.006(2) 0.010(2) 0.003(2) C(24) 0.040(3) 0.029(3) 0.013(3) 0.013(2) -0.005(2) -0.002(2) C(25) 0.023(2) 0.029(3) 0.020(3) 0.008(2) -0.003(2) -0.006(2) C(26) 0.021(2) 0.018(3) 0.013(2) 0.003(2) 0.002(2) -0.005(2) C(27) 0.012(2) 0.022(2) 0.020(3) 0.001(2) -0.003(2) -0.001(2) C(28) 0.022(2) 0.029(3) 0.034(3) 0.005(2) 0.008(2) 0.008(2) C(29) 0.023(2) 0.021(3) 0.013(2) 0.002(2) 0.005(2) -0.005(2) C(30) 0.016(2) 0.018(3) 0.023(3) 0.000(2) 0.003(2) 0.000(2) C(31) 0.025(2) 0.043(3) 0.030(3) 0.000(2) 0.003(2) 0.013(2) C(32) 0.033(3) 0.073(4) 0.034(3) 0.010(3) 0.001(3) 0.032(3) C(33) 0.019(2) 0.047(3) 0.030(3) 0.005(2) -0.005(2) 0.013(3) C(34) 0.017(2) 0.024(3) 0.020(3) 0.003(2) -0.003(2) -0.001(2) C(35) 0.013(2) 0.020(3) 0.019(3) 0.004(2) 0.001(2) 0.003(2) C(36) 0.013(2) 0.033(3) 0.022(3) -0.004(2) 0.005(2) 0.000(2) C(37) 0.020(2) 0.038(3) 0.025(3) 0.007(2) 0.003(2) 0.000(2) C(38) 0.018(2) 0.018(3) 0.021(3) 0.005(2) 0.004(2) -0.003(2) C(39) 0.023(2) 0.024(3) 0.032(3) -0.001(2) 0.000(2) 0.003(2) C(40) 0.031(2) 0.044(3) 0.025(3) 0.008(2) 0.009(2) 0.008(2) C(41) 0.032(3) 0.042(3) 0.025(3) 0.009(2) -0.002(2) 0.001(2) C(42) 0.018(2) 0.040(3) 0.036(3) 0.000(2) -0.004(2) -0.013(3) C(43) 0.034(3) 0.054(6) 0.082(7) 0.000(4) 0.003(4) 0.022(5) C(44) 0.034(3) 0.054(6) 0.082(7) 0.000(4) 0.003(4) 0.022(5) #------------------------------------------------------------------------------ _computing_data_collection 'CRYSTALCLEAR' _computing_cell_refinement 'CRYSTALCLEAR' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS97 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 Cu(1) N(1) 2.044(4) . . yes Cu(1) N(2) 1.914(3) . . yes Cu(1) N(3) 2.244(4) . . yes Cu(1) N(8) 2.644(3) . . yes Cu(1) N(9) 1.958(3) . . yes Cu(1) N(10) 2.266(4) . . yes Cu(2) N(3) 2.712(4) . . yes Cu(2) N(4) 1.937(3) . . yes Cu(2) N(5) 2.143(4) . . yes Cu(2) N(6) 2.049(3) . . yes Cu(2) N(7) 1.920(3) . . yes Cu(2) N(8) 2.346(3) . . yes Cl(1) Cl(4) 0.80(1) . . yes Cl(1) C(43) 1.754(8) . . yes Cl(1) C(44) 2.04(4) . . yes Cl(2) Cl(3) 0.97(2) . . yes Cl(2) C(43) 1.756(10) . . yes Cl(2) C(44) 1.42(4) . . yes Cl(3) C(43) 1.39(2) . . yes Cl(3) C(44) 1.69(4) . . yes Cl(4) C(43) 1.90(1) . . yes Cl(4) C(44) 1.75(4) . . yes O(1) C(8) 1.254(5) . . yes O(2) C(14) 1.238(5) . . yes O(3) C(29) 1.245(5) . . yes O(4) C(35) 1.258(4) . . yes N(1) C(1) 1.352(6) . . yes N(1) C(5) 1.355(5) . . yes N(2) C(6) 1.455(6) . . yes N(2) C(8) 1.323(6) . . yes N(3) C(9) 1.351(5) . . yes N(3) C(13) 1.339(6) . . yes N(4) C(14) 1.332(6) . . yes N(4) C(15) 1.464(5) . . yes N(5) C(17) 1.332(5) . . yes N(5) C(21) 1.354(6) . . yes N(6) C(22) 1.342(6) . . yes N(6) C(26) 1.360(5) . . yes N(7) C(27) 1.452(5) . . yes N(7) C(29) 1.331(6) . . yes N(8) C(30) 1.349(5) . . yes N(8) C(34) 1.353(5) . . yes N(9) C(35) 1.315(6) . . yes N(9) C(36) 1.472(5) . . yes N(10) C(38) 1.337(5) . . yes N(10) C(42) 1.343(6) . . yes C(1) C(2) 1.370(7) . . yes C(2) C(3) 1.383(7) . . yes C(3) C(4) 1.378(7) . . yes C(4) C(5) 1.380(7) . . yes C(5) C(6) 1.495(6) . . yes C(6) C(7) 1.543(7) . . yes C(8) C(9) 1.506(7) . . yes C(9) C(10) 1.370(7) . . yes C(10) C(11) 1.371(7) . . yes C(11) C(12) 1.386(6) . . yes C(12) C(13) 1.390(6) . . yes C(13) C(14) 1.510(6) . . yes C(15) C(16) 1.531(7) . . yes C(15) C(17) 1.495(6) . . yes C(17) C(18) 1.391(6) . . yes C(18) C(19) 1.376(7) . . yes C(19) C(20) 1.374(6) . . yes C(20) C(21) 1.355(6) . . yes C(22) C(23) 1.372(7) . . yes C(23) C(24) 1.375(7) . . yes C(24) C(25) 1.371(7) . . yes C(25) C(26) 1.399(6) . . yes C(26) C(27) 1.494(6) . . yes C(27) C(28) 1.537(6) . . yes C(29) C(30) 1.505(5) . . yes C(30) C(31) 1.371(7) . . yes C(31) C(32) 1.392(7) . . yes C(32) C(33) 1.379(7) . . yes C(33) C(34) 1.369(7) . . yes C(34) C(35) 1.518(6) . . yes C(36) C(37) 1.547(6) . . yes C(36) C(38) 1.494(6) . . yes C(38) C(39) 1.389(6) . . yes C(39) C(40) 1.359(7) . . yes C(40) C(41) 1.413(6) . . yes C(41) C(42) 1.372(7) . . yes C(43) C(44) 1.06(4) . . yes #------------------------------------------------------------------------------ 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 N(1) Cu(1) N(2) 80.9(1) . . . yes N(1) Cu(1) N(3) 156.9(1) . . . yes N(1) Cu(1) N(8) 82.2(1) . . . yes N(1) Cu(1) N(9) 99.1(1) . . . yes N(1) Cu(1) N(10) 115.2(1) . . . yes N(2) Cu(1) N(3) 78.6(1) . . . yes N(2) Cu(1) N(8) 102.2(1) . . . yes N(2) Cu(1) N(9) 174.9(2) . . . yes N(2) Cu(1) N(10) 105.8(1) . . . yes N(3) Cu(1) N(8) 91.9(1) . . . yes N(3) Cu(1) N(9) 100.4(1) . . . yes N(3) Cu(1) N(10) 80.8(1) . . . yes N(8) Cu(1) N(9) 72.8(1) . . . yes N(8) Cu(1) N(10) 148.9(1) . . . yes N(9) Cu(1) N(10) 78.8(1) . . . yes N(3) Cu(2) N(4) 72.6(1) . . . yes N(3) Cu(2) N(5) 149.9(1) . . . yes N(3) Cu(2) N(6) 80.2(1) . . . yes N(3) Cu(2) N(7) 98.8(1) . . . yes N(3) Cu(2) N(8) 88.0(1) . . . yes N(4) Cu(2) N(5) 80.6(1) . . . yes N(4) Cu(2) N(6) 101.7(1) . . . yes N(4) Cu(2) N(7) 170.3(1) . . . yes N(4) Cu(2) N(8) 97.6(1) . . . yes N(5) Cu(2) N(6) 119.2(1) . . . yes N(5) Cu(2) N(7) 106.5(1) . . . yes N(5) Cu(2) N(8) 82.2(1) . . . yes N(6) Cu(2) N(7) 80.9(1) . . . yes N(6) Cu(2) N(8) 153.2(1) . . . yes N(7) Cu(2) N(8) 77.2(1) . . . yes Cl(4) Cl(1) C(43) 88.0(9) . . . yes Cl(4) Cl(1) C(44) 57(1) . . . yes C(43) Cl(1) C(44) 31(1) . . . yes Cl(3) Cl(2) C(43) 51(1) . . . yes Cl(3) Cl(2) C(44) 87(1) . . . yes C(43) Cl(2) C(44) 36(1) . . . yes Cl(2) Cl(3) C(43) 94.7(9) . . . yes Cl(2) Cl(3) C(44) 56(1) . . . yes C(43) Cl(3) C(44) 38(1) . . . yes Cl(1) Cl(4) C(43) 67.3(8) . . . yes Cl(1) Cl(4) C(44) 100(1) . . . yes C(43) Cl(4) C(44) 33(1) . . . yes Cu(1) N(1) C(1) 126.9(3) . . . yes Cu(1) N(1) C(5) 114.2(3) . . . yes C(1) N(1) C(5) 118.7(4) . . . yes Cu(1) N(2) C(6) 119.2(3) . . . yes Cu(1) N(2) C(8) 121.1(3) . . . yes C(6) N(2) C(8) 118.6(3) . . . yes Cu(1) N(3) C(9) 105.9(3) . . . yes Cu(1) N(3) C(13) 127.6(3) . . . yes C(9) N(3) C(13) 118.6(4) . . . yes Cu(2) N(4) C(14) 125.9(3) . . . yes Cu(2) N(4) C(15) 117.8(3) . . . yes C(14) N(4) C(15) 115.8(3) . . . yes Cu(2) N(5) C(17) 110.8(3) . . . yes Cu(2) N(5) C(21) 128.4(3) . . . yes C(17) N(5) C(21) 118.4(4) . . . yes Cu(2) N(6) C(22) 126.7(3) . . . yes Cu(2) N(6) C(26) 113.5(3) . . . yes C(22) N(6) C(26) 119.2(3) . . . yes Cu(2) N(7) C(27) 119.3(3) . . . yes Cu(2) N(7) C(29) 122.1(3) . . . yes C(27) N(7) C(29) 118.0(3) . . . yes C(30) N(8) C(34) 118.0(3) . . . yes Cu(1) N(9) C(35) 125.7(3) . . . yes Cu(1) N(9) C(36) 118.0(3) . . . yes C(35) N(9) C(36) 116.3(3) . . . yes Cu(1) N(10) C(38) 109.2(3) . . . yes Cu(1) N(10) C(42) 128.5(3) . . . yes C(38) N(10) C(42) 117.3(4) . . . yes N(1) C(1) C(2) 122.4(4) . . . yes C(1) C(2) C(3) 118.9(5) . . . yes C(2) C(3) C(4) 119.0(5) . . . yes C(3) C(4) C(5) 120.0(4) . . . yes N(1) C(5) C(4) 120.9(4) . . . yes N(1) C(5) C(6) 116.6(4) . . . yes C(4) C(5) C(6) 122.5(4) . . . yes N(2) C(6) C(5) 108.6(3) . . . yes N(2) C(6) C(7) 112.4(4) . . . yes C(5) C(6) C(7) 111.0(4) . . . yes O(1) C(8) N(2) 128.7(4) . . . yes O(1) C(8) C(9) 118.5(4) . . . yes N(2) C(8) C(9) 112.8(3) . . . yes N(3) C(9) C(8) 114.6(4) . . . yes N(3) C(9) C(10) 121.6(4) . . . yes C(8) C(9) C(10) 123.8(4) . . . yes C(9) C(10) C(11) 120.5(4) . . . yes C(10) C(11) C(12) 117.9(4) . . . yes C(11) C(12) C(13) 119.4(4) . . . yes N(3) C(13) C(12) 121.6(4) . . . yes N(3) C(13) C(14) 118.2(4) . . . yes C(12) C(13) C(14) 119.8(4) . . . yes O(2) C(14) N(4) 128.0(4) . . . yes O(2) C(14) C(13) 119.1(4) . . . yes N(4) C(14) C(13) 112.9(3) . . . yes N(4) C(15) C(16) 111.0(3) . . . yes N(4) C(15) C(17) 109.9(3) . . . yes C(16) C(15) C(17) 109.9(4) . . . yes N(5) C(17) C(15) 117.3(4) . . . yes N(5) C(17) C(18) 121.3(4) . . . yes C(15) C(17) C(18) 121.5(3) . . . yes C(17) C(18) C(19) 119.0(4) . . . yes C(18) C(19) C(20) 119.6(4) . . . yes C(19) C(20) C(21) 118.4(4) . . . yes N(5) C(21) C(20) 123.2(4) . . . yes N(6) C(22) C(23) 122.5(4) . . . yes C(22) C(23) C(24) 118.8(4) . . . yes C(23) C(24) C(25) 119.7(4) . . . yes C(24) C(25) C(26) 119.6(4) . . . yes N(6) C(26) C(25) 120.0(4) . . . yes N(6) C(26) C(27) 116.6(3) . . . yes C(25) C(26) C(27) 123.4(3) . . . yes N(7) C(27) C(26) 108.3(3) . . . yes N(7) C(27) C(28) 112.7(4) . . . yes C(26) C(27) C(28) 108.6(3) . . . yes O(3) C(29) N(7) 127.9(4) . . . yes O(3) C(29) C(30) 119.4(4) . . . yes N(7) C(29) C(30) 112.8(3) . . . yes N(8) C(30) C(29) 116.0(4) . . . yes N(8) C(30) C(31) 122.3(4) . . . yes C(29) C(30) C(31) 121.6(4) . . . yes C(30) C(31) C(32) 119.2(4) . . . yes C(31) C(32) C(33) 118.3(5) . . . yes C(32) C(33) C(34) 119.7(4) . . . yes N(8) C(34) C(33) 122.1(4) . . . yes N(8) C(34) C(35) 116.6(4) . . . yes C(33) C(34) C(35) 121.0(3) . . . yes O(4) C(35) N(9) 127.5(4) . . . yes O(4) C(35) C(34) 117.9(4) . . . yes N(9) C(35) C(34) 114.2(3) . . . yes N(9) C(36) C(37) 109.2(4) . . . yes N(9) C(36) C(38) 110.8(3) . . . yes C(37) C(36) C(38) 109.8(4) . . . yes N(10) C(38) C(36) 115.8(4) . . . yes N(10) C(38) C(39) 122.3(4) . . . yes C(36) C(38) C(39) 121.9(4) . . . yes C(38) C(39) C(40) 120.1(4) . . . yes C(39) C(40) C(41) 118.5(4) . . . yes C(40) C(41) C(42) 117.4(5) . . . yes N(10) C(42) C(41) 124.4(4) . . . yes Cl(1) C(43) Cl(2) 111.8(4) . . . yes Cl(1) C(43) Cl(3) 125.4(6) . . . yes Cl(1) C(43) Cl(4) 24.8(5) . . . yes Cl(1) C(43) C(44) 89(1) . . . yes Cl(2) C(43) Cl(3) 33.4(9) . . . yes Cl(2) C(43) Cl(4) 97.5(6) . . . yes Cl(2) C(43) C(44) 53(2) . . . yes Cl(3) C(43) Cl(4) 122.9(8) . . . yes Cl(3) C(43) C(44) 86(2) . . . yes Cl(4) C(43) C(44) 65(2) . . . yes Cl(1) C(44) Cl(2) 112(1) . . . yes Cl(1) C(44) Cl(3) 96(1) . . . yes Cl(1) C(44) Cl(4) 22.5(6) . . . yes Cl(1) C(44) C(43) 59(1) . . . yes Cl(2) C(44) Cl(3) 35(1) . . . yes Cl(2) C(44) Cl(4) 120(1) . . . yes Cl(2) C(44) C(43) 89(2) . . . yes Cl(3) C(44) Cl(4) 115(2) . . . yes Cl(3) C(44) C(43) 55(2) . . . yes Cl(4) C(44) C(43) 81(2) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu(1) N(1) C(1) C(2) 172.6(4) . . . . yes Cu(1) N(1) C(5) C(4) -173.5(4) . . . . yes Cu(1) N(1) C(5) C(6) 7.2(5) . . . . yes Cu(1) N(2) C(6) C(5) -2.4(5) . . . . yes Cu(1) N(2) C(6) C(7) -125.6(3) . . . . yes Cu(1) N(2) C(8) O(1) -169.8(4) . . . . yes Cu(1) N(2) C(8) C(9) 10.3(5) . . . . yes Cu(1) N(3) C(9) C(8) 27.9(4) . . . . yes Cu(1) N(3) C(9) C(10) -150.4(4) . . . . yes Cu(1) N(3) C(13) C(12) 138.4(4) . . . . yes Cu(1) N(3) C(13) C(14) -48.6(5) . . . . yes Cu(1) N(9) C(35) O(4) -178.8(3) . . . . yes Cu(1) N(9) C(35) C(34) 7.6(5) . . . . yes Cu(1) N(9) C(36) C(37) -102.4(3) . . . . yes Cu(1) N(9) C(36) C(38) 18.7(4) . . . . yes Cu(1) N(10) C(38) C(36) 27.0(4) . . . . yes Cu(1) N(10) C(38) C(39) -156.9(4) . . . . yes Cu(1) N(10) C(42) C(41) 152.5(4) . . . . yes Cu(2) N(4) C(14) O(2) -171.6(4) . . . . yes Cu(2) N(4) C(14) C(13) 10.5(5) . . . . yes Cu(2) N(4) C(15) C(16) -115.6(3) . . . . yes Cu(2) N(4) C(15) C(17) 6.2(4) . . . . yes Cu(2) N(5) C(17) C(15) 21.5(5) . . . . yes Cu(2) N(5) C(17) C(18) -159.0(4) . . . . yes Cu(2) N(5) C(21) C(20) 158.4(4) . . . . yes Cu(2) N(6) C(22) C(23) 169.6(4) . . . . yes Cu(2) N(6) C(26) C(25) -168.9(3) . . . . yes Cu(2) N(6) C(26) C(27) 13.1(5) . . . . yes Cu(2) N(7) C(27) C(26) 3.9(4) . . . . yes Cu(2) N(7) C(27) C(28) -116.3(3) . . . . yes Cu(2) N(7) C(29) O(3) -174.4(4) . . . . yes Cu(2) N(7) C(29) C(30) 5.6(5) . . . . yes Cl(1) Cl(4) C(43) Cl(2) 127.6(9) . . . . yes Cl(1) Cl(4) C(43) Cl(3) 104(1) . . . . yes Cl(1) Cl(4) C(43) C(44) 171(2) . . . . yes Cl(1) Cl(4) C(44) Cl(2) 76(2) . . . . yes Cl(1) Cl(4) C(44) Cl(3) 37(2) . . . . yes Cl(1) Cl(4) C(44) C(43) -7(2) . . . . yes Cl(1) C(43) Cl(2) Cl(3) -121(1) . . . . yes Cl(1) C(43) Cl(2) C(44) 72(2) . . . . yes Cl(1) C(43) Cl(3) Cl(2) 75(1) . . . . yes Cl(1) C(43) Cl(3) C(44) 87(1) . . . . yes Cl(1) C(43) Cl(4) C(44) -171(2) . . . . yes Cl(1) C(43) C(44) Cl(2) -117(1) . . . . yes Cl(1) C(43) C(44) Cl(3) -125.5(6) . . . . yes Cl(1) C(43) C(44) Cl(4) 3.5(9) . . . . yes Cl(1) C(44) Cl(2) Cl(3) -67(1) . . . . yes Cl(1) C(44) Cl(2) C(43) -55(1) . . . . yes Cl(1) C(44) Cl(3) Cl(2) 121(1) . . . . yes Cl(1) C(44) Cl(3) C(43) -44(1) . . . . yes Cl(1) C(44) Cl(4) C(43) 7(2) . . . . yes Cl(1) C(44) C(43) Cl(2) 117(1) . . . . yes Cl(1) C(44) C(43) Cl(3) 125.5(6) . . . . yes Cl(1) C(44) C(43) Cl(4) -3.5(9) . . . . yes Cl(2) Cl(3) C(43) Cl(4) 45(1) . . . . yes Cl(2) Cl(3) C(43) C(44) -11(1) . . . . yes Cl(2) Cl(3) C(44) Cl(4) 107(2) . . . . yes Cl(2) Cl(3) C(44) C(43) 165(2) . . . . yes Cl(2) C(43) Cl(1) Cl(4) -57.8(10) . . . . yes Cl(2) C(43) Cl(1) C(44) -50(1) . . . . yes Cl(2) C(43) Cl(3) C(44) 11(1) . . . . yes Cl(2) C(43) Cl(4) C(44) -44(2) . . . . yes Cl(2) C(43) C(44) Cl(3) -7(1) . . . . yes Cl(2) C(43) C(44) Cl(4) 121(1) . . . . yes Cl(2) C(44) Cl(1) Cl(4) -114(2) . . . . yes Cl(2) C(44) Cl(1) C(43) 74(2) . . . . yes Cl(2) C(44) Cl(3) C(43) -165(2) . . . . yes Cl(2) C(44) Cl(4) C(43) 84(3) . . . . yes Cl(2) C(44) C(43) Cl(3) 7(1) . . . . yes Cl(2) C(44) C(43) Cl(4) -121(1) . . . . yes Cl(3) Cl(2) C(43) Cl(4) -142(1) . . . . yes Cl(3) Cl(2) C(43) C(44) 165(2) . . . . yes Cl(3) Cl(2) C(44) Cl(4) -91(2) . . . . yes Cl(3) Cl(2) C(44) C(43) -11(1) . . . . yes Cl(3) C(43) Cl(1) Cl(4) -92(1) . . . . yes Cl(3) C(43) Cl(1) C(44) -85(2) . . . . yes Cl(3) C(43) Cl(2) C(44) -165(2) . . . . yes Cl(3) C(43) Cl(4) C(44) -67(2) . . . . yes Cl(3) C(43) C(44) Cl(4) 128(1) . . . . yes Cl(3) C(44) Cl(1) Cl(4) -146(2) . . . . yes Cl(3) C(44) Cl(1) C(43) 42(1) . . . . yes Cl(3) C(44) Cl(2) C(43) 11(1) . . . . yes Cl(3) C(44) Cl(4) C(43) 44(1) . . . . yes Cl(3) C(44) C(43) Cl(4) -128(1) . . . . yes Cl(4) Cl(1) C(43) C(44) -7(2) . . . . yes Cl(4) Cl(1) C(44) C(43) 171(2) . . . . yes Cl(4) C(43) Cl(1) C(44) 7(2) . . . . yes Cl(4) C(43) Cl(2) C(44) 51(2) . . . . yes Cl(4) C(43) Cl(3) C(44) 57(1) . . . . yes Cl(4) C(44) Cl(1) C(43) -171(2) . . . . yes Cl(4) C(44) Cl(2) C(43) -79(2) . . . . yes Cl(4) C(44) Cl(3) C(43) -58(1) . . . . yes O(1) C(8) N(2) C(6) -1.5(8) . . . . yes O(1) C(8) C(9) N(3) 152.6(4) . . . . yes O(1) C(8) C(9) C(10) -29.1(7) . . . . yes O(2) C(14) N(4) C(15) 0.5(6) . . . . yes O(2) C(14) C(13) N(3) 136.0(4) . . . . yes O(2) C(14) C(13) C(12) -50.9(6) . . . . yes O(3) C(29) N(7) C(27) -2.8(7) . . . . yes O(3) C(29) C(30) N(8) 150.7(4) . . . . yes O(3) C(29) C(30) C(31) -31.6(6) . . . . yes O(4) C(35) N(9) C(36) 2.6(6) . . . . yes O(4) C(35) C(34) N(8) 146.5(4) . . . . yes O(4) C(35) C(34) C(33) -39.2(6) . . . . yes N(1) Cu(1) N(2) C(6) 4.8(3) . . . . yes N(1) Cu(1) N(2) C(8) 173.0(4) . . . . yes N(1) Cu(1) N(3) C(9) -45.6(5) . . . . yes N(1) Cu(1) N(3) C(13) 166.5(4) . . . . yes N(1) Cu(1) N(9) C(35) -68.5(4) . . . . yes N(1) Cu(1) N(9) C(36) 110.1(3) . . . . yes N(1) Cu(1) N(10) C(38) -107.8(3) . . . . yes N(1) Cu(1) N(10) C(42) 98.6(4) . . . . yes N(1) C(1) C(2) C(3) -0.2(8) . . . . yes N(1) C(5) C(4) C(3) 0.6(8) . . . . yes N(1) C(5) C(6) N(2) -3.4(6) . . . . yes N(1) C(5) C(6) C(7) 120.7(4) . . . . yes N(2) Cu(1) N(1) C(1) 178.9(4) . . . . yes N(2) Cu(1) N(1) C(5) -6.6(3) . . . . yes N(2) Cu(1) N(3) C(9) -17.8(3) . . . . yes N(2) Cu(1) N(3) C(13) -165.7(4) . . . . yes N(2) Cu(1) N(9) C(35) 21(1) . . . . yes N(2) Cu(1) N(9) C(36) -159(1) . . . . yes N(2) Cu(1) N(10) C(38) 164.9(3) . . . . yes N(2) Cu(1) N(10) C(42) 11.3(5) . . . . yes N(2) C(6) C(5) C(4) 177.4(5) . . . . yes N(2) C(8) C(9) N(3) -27.4(6) . . . . yes N(2) C(8) C(9) C(10) 150.8(5) . . . . yes N(3) Cu(1) N(1) C(1) -153.5(4) . . . . yes N(3) Cu(1) N(1) C(5) 21.0(6) . . . . yes N(3) Cu(1) N(2) C(6) -164.5(4) . . . . yes N(3) Cu(1) N(2) C(8) 3.7(4) . . . . yes N(3) Cu(1) N(9) C(35) 99.0(3) . . . . yes N(3) Cu(1) N(9) C(36) -82.3(3) . . . . yes N(3) Cu(1) N(10) C(38) 89.7(3) . . . . yes N(3) Cu(1) N(10) C(42) -64.0(4) . . . . yes N(3) C(9) C(10) C(11) 4.3(7) . . . . yes N(3) C(13) C(12) C(11) 5.9(7) . . . . yes N(3) C(13) C(14) N(4) -46.0(5) . . . . yes N(4) Cu(2) N(5) C(17) -13.7(3) . . . . yes N(4) Cu(2) N(5) C(21) -175.3(4) . . . . yes N(4) Cu(2) N(6) C(22) -9.3(4) . . . . yes N(4) Cu(2) N(6) C(26) 162.1(3) . . . . yes N(4) Cu(2) N(7) C(27) -104.1(9) . . . . yes N(4) Cu(2) N(7) C(29) 67.3(10) . . . . yes N(4) C(14) C(13) C(12) 127.2(4) . . . . yes N(4) C(15) C(17) N(5) -18.9(5) . . . . yes N(4) C(15) C(17) C(18) 161.6(4) . . . . yes N(5) Cu(2) N(4) C(14) 175.5(4) . . . . yes N(5) Cu(2) N(4) C(15) 3.5(3) . . . . yes N(5) Cu(2) N(6) C(22) 76.4(4) . . . . yes N(5) Cu(2) N(6) C(26) -112.2(3) . . . . yes N(5) Cu(2) N(7) C(27) 119.9(3) . . . . yes N(5) Cu(2) N(7) C(29) -68.6(4) . . . . yes N(5) C(17) C(15) C(16) 103.5(4) . . . . yes N(5) C(17) C(18) C(19) -3.8(7) . . . . yes N(5) C(21) C(20) C(19) -1.4(8) . . . . yes N(6) Cu(2) N(4) C(14) -66.5(4) . . . . yes N(6) Cu(2) N(4) C(15) 121.5(3) . . . . yes N(6) Cu(2) N(5) C(17) -111.9(3) . . . . yes N(6) Cu(2) N(5) C(21) 86.5(4) . . . . yes N(6) Cu(2) N(7) C(27) 2.1(3) . . . . yes N(6) Cu(2) N(7) C(29) 173.5(4) . . . . yes N(6) C(22) C(23) C(24) -1.3(7) . . . . yes N(6) C(26) C(25) C(24) -2.2(6) . . . . yes N(6) C(26) C(27) N(7) -11.1(5) . . . . yes N(6) C(26) C(27) C(28) 111.6(4) . . . . yes N(7) Cu(2) N(4) C(14) 37(1) . . . . yes N(7) Cu(2) N(4) C(15) -134.0(8) . . . . yes N(7) Cu(2) N(5) C(17) 159.4(3) . . . . yes N(7) Cu(2) N(5) C(21) -2.2(4) . . . . yes N(7) Cu(2) N(6) C(22) -179.8(4) . . . . yes N(7) Cu(2) N(6) C(26) -8.4(3) . . . . yes N(7) C(27) C(26) C(25) 171.1(4) . . . . yes N(7) C(29) C(30) N(8) -29.2(5) . . . . yes N(7) C(29) C(30) C(31) 148.5(4) . . . . yes N(8) C(30) C(31) C(32) 3.2(7) . . . . yes N(8) C(34) C(33) C(32) 6.7(8) . . . . yes N(8) C(34) C(35) N(9) -39.3(5) . . . . yes N(9) Cu(1) N(1) C(1) -6.3(4) . . . . yes N(9) Cu(1) N(1) C(5) 168.2(3) . . . . yes N(9) Cu(1) N(2) C(6) -86(1) . . . . yes N(9) Cu(1) N(2) C(8) 81(1) . . . . yes N(9) Cu(1) N(3) C(9) 167.3(3) . . . . yes N(9) Cu(1) N(3) C(13) 19.4(4) . . . . yes N(9) Cu(1) N(10) C(38) -12.9(3) . . . . yes N(9) Cu(1) N(10) C(42) -166.5(5) . . . . yes N(9) C(35) C(34) C(33) 135.1(5) . . . . yes N(9) C(36) C(38) N(10) -30.9(5) . . . . yes N(9) C(36) C(38) C(39) 153.0(4) . . . . yes N(10) Cu(1) N(1) C(1) 75.6(4) . . . . yes N(10) Cu(1) N(1) C(5) -109.9(3) . . . . yes N(10) Cu(1) N(2) C(6) 118.6(3) . . . . yes N(10) Cu(1) N(2) C(8) -73.2(4) . . . . yes N(10) Cu(1) N(3) C(9) 90.6(3) . . . . yes N(10) Cu(1) N(3) C(13) -57.4(4) . . . . yes N(10) Cu(1) N(9) C(35) 177.4(4) . . . . yes N(10) Cu(1) N(9) C(36) -4.0(3) . . . . yes N(10) C(38) C(36) C(37) 89.9(4) . . . . yes N(10) C(38) C(39) C(40) -0.3(7) . . . . yes N(10) C(42) C(41) C(40) -1.1(8) . . . . yes C(1) N(1) C(5) C(4) 1.5(7) . . . . yes C(1) N(1) C(5) C(6) -177.8(4) . . . . yes C(1) C(2) C(3) C(4) 2.2(8) . . . . yes C(2) C(1) N(1) C(5) -1.7(7) . . . . yes C(2) C(3) C(4) C(5) -2.4(8) . . . . yes C(3) C(4) C(5) C(6) 179.8(5) . . . . yes C(4) C(5) C(6) C(7) -58.5(6) . . . . yes C(5) C(6) N(2) C(8) -170.8(4) . . . . yes C(6) N(2) C(8) C(9) 178.5(4) . . . . yes C(7) C(6) N(2) C(8) 65.9(5) . . . . yes C(8) C(9) N(3) C(13) 179.3(4) . . . . yes C(8) C(9) C(10) C(11) -173.8(4) . . . . yes C(9) N(3) C(13) C(12) -6.1(6) . . . . yes C(9) N(3) C(13) C(14) 166.9(4) . . . . yes C(9) C(10) C(11) C(12) -4.4(7) . . . . yes C(10) C(9) N(3) C(13) 1.0(6) . . . . yes C(10) C(11) C(12) C(13) -0.5(7) . . . . yes C(11) C(12) C(13) C(14) -167.0(4) . . . . yes C(13) C(14) N(4) C(15) -177.3(3) . . . . yes C(14) N(4) C(15) C(16) 71.6(4) . . . . yes C(14) N(4) C(15) C(17) -166.6(4) . . . . yes C(15) C(17) N(5) C(21) -174.8(4) . . . . yes C(15) C(17) C(18) C(19) 175.7(5) . . . . yes C(16) C(15) C(17) C(18) -76.0(5) . . . . yes C(17) N(5) C(21) C(20) -2.1(7) . . . . yes C(17) C(18) C(19) C(20) 0.2(8) . . . . yes C(18) C(17) N(5) C(21) 4.7(6) . . . . yes C(18) C(19) C(20) C(21) 2.3(8) . . . . yes C(22) N(6) C(26) C(25) 3.2(6) . . . . yes C(22) N(6) C(26) C(27) -174.8(4) . . . . yes C(22) C(23) C(24) C(25) 2.3(7) . . . . yes C(23) C(22) N(6) C(26) -1.4(7) . . . . yes C(23) C(24) C(25) C(26) -0.5(7) . . . . yes C(24) C(25) C(26) C(27) 175.5(4) . . . . yes C(25) C(26) C(27) C(28) -66.2(5) . . . . yes C(26) C(27) N(7) C(29) -167.9(4) . . . . yes C(27) N(7) C(29) C(30) 177.1(4) . . . . yes C(28) C(27) N(7) C(29) 71.9(5) . . . . yes C(29) C(30) N(8) C(34) 178.4(4) . . . . yes C(29) C(30) C(31) C(32) -174.3(5) . . . . yes C(30) N(8) C(34) C(33) -5.8(6) . . . . yes C(30) N(8) C(34) C(35) 168.5(4) . . . . yes C(30) C(31) C(32) C(33) -2.3(8) . . . . yes C(31) C(30) N(8) C(34) 0.7(6) . . . . yes C(31) C(32) C(33) C(34) -2.5(8) . . . . yes C(32) C(33) C(34) C(35) -167.4(5) . . . . yes C(34) C(35) N(9) C(36) -171.0(3) . . . . yes C(35) N(9) C(36) C(37) 76.3(5) . . . . yes C(35) N(9) C(36) C(38) -162.5(4) . . . . yes C(36) C(38) N(10) C(42) -176.0(4) . . . . yes C(36) C(38) C(39) C(40) 175.6(4) . . . . yes C(37) C(36) C(38) C(39) -86.2(5) . . . . yes C(38) N(10) C(42) C(41) 0.6(7) . . . . yes C(38) C(39) C(40) C(41) -0.2(7) . . . . yes C(39) C(38) N(10) C(42) 0.1(6) . . . . yes C(39) C(40) C(41) C(42) 0.9(7) . . . . yes C(43) Cl(1) Cl(4) C(44) 4(1) . . . . yes C(43) Cl(2) Cl(3) C(44) -8(1) . . . . yes C(43) Cl(3) Cl(2) C(44) 8(1) . . . . yes C(43) Cl(4) Cl(1) C(44) -4(1) . . . . yes C(43) Cl(4) Cl(1) C(44) -4(1) . . . . yes #------------------------------------------------------------------------------ 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 ? ? ? ? ? ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data__rs-helix _database_code_CSD 182240 _audit_creation_date 'Wed Feb 13 19:36:27 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C42 H50 Cu2 N10 O10 ' _chemical_formula_moiety 'C42 H50 Cu2 N10 O10 ' _chemical_formula_weight 982.01 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 10.483(1) _cell_length_b 12.709(1) _cell_length_c 17.889(2) _cell_angle_alpha 83.592(10) _cell_angle_beta 79.837(9) _cell_angle_gamma 67.482(7) _cell_volume 2164.5(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8158 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 193.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Green' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.053 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.720 _exptl_absorpt_correction_T_max 0.810 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 447 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). 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 9348 _reflns_number_gt 7142 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1101 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 7142 _refine_ls_number_parameters 729 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.0499P)^2^+1.4793P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_diff_density_max 0.71 _refine_diff_density_min -0.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.12668(4) 0.31905(3) 0.77255(2) 0.0185(1) Uani 1.00 d . . . Cu(2) Cu -0.17622(4) 0.25239(3) 0.75682(2) 0.0182(1) Uani 1.00 d . . . O(1) O -0.1910(2) 0.5733(2) 0.8878(1) 0.0292(5) Uani 1.00 d . . . O(2) O 0.0911(2) -0.0188(2) 0.8670(1) 0.0269(5) Uani 1.00 d . . . O(3) O -0.2596(2) 0.5649(2) 0.6467(1) 0.0286(5) Uani 1.00 d . . . O(4) O 0.2902(2) 0.0358(2) 0.6446(1) 0.0317(5) Uani 1.00 d . . . O(5) O 0.2848(3) -0.1826(2) 0.6630(2) 0.0464(7) Uani 1.00 d . . . O(6) O 0.4348(3) 0.0885(3) 0.4246(2) 0.0609(9) Uani 1.00 d . . . O(7) O -0.2658(3) 0.7756(2) 0.6858(2) 0.0539(8) Uani 1.00 d . . . O(8) O -0.3237(3) 0.2115(2) 1.1827(2) 0.0491(7) Uani 1.00 d . . . O(9) O -0.4038(3) 0.7750(2) 0.8367(2) 0.0504(7) Uani 1.00 d . . . O(10) O -0.4744(3) 0.7069(2) 0.5646(2) 0.0425(6) Uani 1.00 d . . . N(1) N 0.1970(3) 0.4200(2) 0.6900(1) 0.0194(5) Uani 1.00 d . . . N(2) N 0.0044(3) 0.4663(2) 0.8082(1) 0.0172(5) Uani 1.00 d . . . N(3) N -0.0474(3) 0.2778(2) 0.8611(1) 0.0191(5) Uani 1.00 d . . . N(4) N -0.0642(3) 0.1001(2) 0.7890(1) 0.0189(5) Uani 1.00 d . . . N(5) N -0.1906(3) 0.1653(2) 0.6682(1) 0.0227(5) Uani 1.00 d . . . N(6) N -0.3398(3) 0.2979(2) 0.8457(1) 0.0198(5) Uani 1.00 d . . . N(7) N -0.2649(2) 0.4106(2) 0.7268(1) 0.0172(5) Uani 1.00 d . . . N(8) N 0.0038(3) 0.2950(2) 0.6646(1) 0.0176(5) Uani 1.00 d . . . N(9) N 0.2357(3) 0.1694(2) 0.7340(1) 0.0189(5) Uani 1.00 d . . . N(10) N 0.2416(3) 0.2387(2) 0.8678(2) 0.0243(6) Uani 1.00 d . . . C(1) C 0.2956(3) 0.3855(3) 0.6289(2) 0.0255(7) Uani 1.00 d . . . C(2) C 0.3328(4) 0.4601(3) 0.5771(2) 0.0311(8) Uani 1.00 d . . . C(3) C 0.2669(4) 0.5762(3) 0.5879(2) 0.0332(8) Uani 1.00 d . . . C(4) C 0.1661(4) 0.6120(3) 0.6497(2) 0.0278(7) Uani 1.00 d . . . C(5) C 0.1331(3) 0.5318(2) 0.7004(2) 0.0180(6) Uani 1.00 d . . . C(6) C 0.0288(3) 0.5671(2) 0.7719(2) 0.0191(6) Uani 1.00 d . . . C(7) C 0.0861(4) 0.6176(3) 0.8252(2) 0.0290(7) Uani 1.00 d . . . C(8) C -0.1010(3) 0.4811(2) 0.8639(2) 0.0185(6) Uani 1.00 d . . . C(9) C -0.1015(3) 0.3706(2) 0.9033(2) 0.0182(6) Uani 1.00 d . . . C(10) C -0.1460(3) 0.3645(3) 0.9807(2) 0.0221(6) Uani 1.00 d . . . C(11) C -0.1277(3) 0.2594(3) 1.0172(2) 0.0255(7) Uani 1.00 d . . . C(12) C -0.0692(3) 0.1630(3) 0.9743(2) 0.0246(7) Uani 1.00 d . . . C(13) C -0.0342(3) 0.1756(2) 0.8965(2) 0.0191(6) Uani 1.00 d . . . C(14) C 0.0062(3) 0.0755(2) 0.8470(2) 0.0194(6) Uani 1.00 d . . . C(15) C -0.0500(3) 0.0060(3) 0.7439(2) 0.0214(6) Uani 1.00 d . . . C(16) C -0.1197(4) -0.0720(3) 0.7899(2) 0.0347(8) Uani 1.00 d . . . C(17) C -0.1163(4) 0.0540(3) 0.6731(2) 0.0257(7) Uani 1.00 d . . . C(18) C -0.1060(6) -0.0153(3) 0.6155(2) 0.049(1) Uani 1.00 d . . . C(19) C -0.1761(6) 0.0309(4) 0.5546(3) 0.059(1) Uani 1.00 d . . . C(20) C -0.2541(5) 0.1458(4) 0.5507(2) 0.050(1) Uani 1.00 d . . . C(21) C -0.2586(4) 0.2107(3) 0.6087(2) 0.0325(8) Uani 1.00 d . . . C(22) C -0.3621(3) 0.2304(3) 0.9057(2) 0.0266(7) Uani 1.00 d . . . C(23) C -0.4609(4) 0.2723(3) 0.9678(2) 0.0317(8) Uani 1.00 d . . . C(24) C -0.5399(4) 0.3874(3) 0.9678(2) 0.0334(8) Uani 1.00 d . . . C(25) C -0.5192(3) 0.4573(3) 0.9054(2) 0.0281(7) Uani 1.00 d . . . C(26) C -0.4180(3) 0.4097(3) 0.8447(2) 0.0202(6) Uani 1.00 d . . . C(27) C -0.3939(3) 0.4785(3) 0.7733(2) 0.0198(6) Uani 1.00 d . . . C(28) C -0.5198(4) 0.5125(4) 0.7311(2) 0.0348(8) Uani 1.00 d . . . C(29) C -0.2116(3) 0.4614(2) 0.6691(2) 0.0186(6) Uani 1.00 d . . . C(30) C -0.0808(3) 0.3822(2) 0.6246(2) 0.0181(6) Uani 1.00 d . . . C(31) C -0.0530(4) 0.3978(3) 0.5467(2) 0.0264(7) Uani 1.00 d . . . C(32) C 0.0624(4) 0.3170(3) 0.5075(2) 0.0315(8) Uani 1.00 d . . . C(33) C 0.1480(3) 0.2260(3) 0.5473(2) 0.0253(7) Uani 1.00 d . . . C(34) C 0.1174(3) 0.2195(2) 0.6261(2) 0.0188(6) Uani 1.00 d . . . C(35) C 0.2210(3) 0.1323(2) 0.6715(2) 0.0205(6) Uani 1.00 d . . . C(36) C 0.3448(3) 0.0919(3) 0.7767(2) 0.0246(7) Uani 1.00 d . . . C(37) C 0.4880(4) 0.0948(4) 0.7415(3) 0.046(1) Uani 1.00 d . . . C(38) C 0.3125(3) 0.1276(3) 0.8576(2) 0.0238(7) Uani 1.00 d . . . C(39) C 0.3559(4) 0.0509(3) 0.9181(2) 0.0327(8) Uani 1.00 d . . . C(40) C 0.3235(4) 0.0894(3) 0.9904(2) 0.0372(8) Uani 1.00 d . . . C(41) C 0.2523(4) 0.2047(3) 1.0011(2) 0.0324(8) Uani 1.00 d . . . C(42) C 0.2138(3) 0.2762(3) 0.9385(2) 0.0280(7) Uani 1.00 d . . . H(1) H 0.337(4) 0.308(3) 0.626(2) 0.0341(1) Uiso 1.00 calc . . . H(2) H 0.399(4) 0.432(3) 0.539(2) 0.0275(1) Uiso 1.00 calc . . . H(3) H 0.292(4) 0.627(3) 0.553(2) 0.0342(1) Uiso 1.00 calc . . . H(4) H 0.118(4) 0.684(3) 0.662(2) 0.0353(1) Uiso 1.00 calc . . . H(5) H -0.058(3) 0.623(3) 0.759(2) 0.01784(10) Uiso 1.00 calc . . . H(6) H 0.173(4) 0.560(3) 0.843(2) 0.0387(1) Uiso 1.00 calc . . . H(7) H 0.106(4) 0.684(3) 0.798(2) 0.0344(1) Uiso 1.00 calc . . . H(8) H 0.024(4) 0.638(3) 0.869(2) 0.0330(1) Uiso 1.00 calc . . . H(9) H -0.191(3) 0.436(3) 1.007(2) 0.0224(1) Uiso 1.00 calc . . . H(10) H -0.155(3) 0.252(3) 1.070(2) 0.0219(1) Uiso 1.00 calc . . . H(11) H -0.060(3) 0.095(3) 0.997(2) 0.01424(10) Uiso 1.00 calc . . . H(12) H 0.041(4) -0.033(3) 0.730(2) 0.0275(1) Uiso 1.00 calc . . . H(13) H -0.073(4) -0.108(3) 0.836(2) 0.0385(1) Uiso 1.00 calc . . . H(14) H -0.217(4) -0.026(3) 0.808(2) 0.0439(1) Uiso 1.00 calc . . . H(15) H -0.113(4) -0.130(4) 0.760(2) 0.0477(2) Uiso 1.00 calc . . . H(16) H -0.060(5) -0.086(4) 0.618(3) 0.0637(2) Uiso 1.00 calc . . . H(17) H -0.167(5) -0.018(4) 0.514(3) 0.0850(2) Uiso 1.00 calc . . . H(18) H -0.303(4) 0.179(3) 0.510(2) 0.0445(1) Uiso 1.00 calc . . . H(19) H -0.308(4) 0.289(3) 0.609(2) 0.0268(1) Uiso 1.00 calc . . . H(20) H -0.305(4) 0.149(3) 0.903(2) 0.0361(1) Uiso 1.00 calc . . . H(21) H -0.474(4) 0.222(3) 1.007(2) 0.0274(1) Uiso 1.00 calc . . . H(22) H -0.610(4) 0.419(3) 1.010(2) 0.0414(1) Uiso 1.00 calc . . . H(23) H -0.574(3) 0.537(3) 0.905(2) 0.0198(1) Uiso 1.00 calc . . . H(24) H -0.392(3) 0.543(3) 0.787(2) 0.0216(1) Uiso 1.00 calc . . . H(25) H -0.530(4) 0.437(3) 0.719(2) 0.0313(1) Uiso 1.00 calc . . . H(26) H -0.603(5) 0.558(4) 0.761(3) 0.0717(2) Uiso 1.00 calc . . . H(27) H -0.506(5) 0.534(4) 0.682(3) 0.0578(2) Uiso 1.00 calc . . . H(28) H -0.115(3) 0.465(3) 0.518(2) 0.0232(1) Uiso 1.00 calc . . . H(29) H 0.076(4) 0.326(3) 0.452(2) 0.0347(1) Uiso 1.00 calc . . . H(30) H 0.224(4) 0.170(3) 0.523(2) 0.0237(1) Uiso 1.00 calc . . . H(31) H 0.347(4) 0.025(3) 0.776(2) 0.0292(1) Uiso 1.00 calc . . . H(32) H 0.485(4) 0.180(4) 0.745(2) 0.0525(2) Uiso 1.00 calc . . . H(33) H 0.556(6) 0.042(4) 0.773(3) 0.0823(2) Uiso 1.00 calc . . . H(34) H 0.504(5) 0.078(4) 0.691(3) 0.0616(2) Uiso 1.00 calc . . . H(35) H 0.396(4) -0.019(3) 0.911(2) 0.0388(1) Uiso 1.00 calc . . . H(36) H 0.357(4) 0.039(3) 1.036(2) 0.0416(1) Uiso 1.00 calc . . . H(37) H 0.227(4) 0.236(3) 1.049(2) 0.0396(1) Uiso 1.00 calc . . . H(38) H 0.165(4) 0.359(3) 0.942(2) 0.0293(1) Uiso 1.00 calc . . . 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) 0.0202(2) 0.0127(2) 0.0202(2) -0.0038(1) -0.0016(1) -0.0011(1) Cu(2) 0.0195(2) 0.0131(2) 0.0178(2) -0.0016(1) -0.0028(1) -0.0003(1) O(1) 0.027(1) 0.016(1) 0.035(1) -0.0003(9) 0.0043(10) -0.0036(9) O(2) 0.027(1) 0.017(1) 0.030(1) 0.0008(9) -0.0086(10) 0.0012(9) O(3) 0.028(1) 0.016(1) 0.036(1) -0.0040(9) -0.003(1) 0.0057(9) O(4) 0.032(1) 0.017(1) 0.038(1) 0.0003(10) -0.001(1) -0.0106(10) O(5) 0.042(2) 0.030(1) 0.063(2) -0.012(1) 0.006(1) -0.012(1) O(6) 0.055(2) 0.050(2) 0.069(2) -0.016(2) 0.013(2) -0.009(2) O(7) 0.065(2) 0.049(2) 0.055(2) -0.025(2) -0.016(2) -0.004(1) O(8) 0.047(2) 0.035(1) 0.049(2) -0.006(1) 0.013(1) -0.005(1) O(9) 0.049(2) 0.043(2) 0.047(2) 0.000(1) -0.016(1) -0.005(1) O(10) 0.043(2) 0.036(1) 0.038(2) -0.001(1) -0.009(1) -0.008(1) N(1) 0.019(1) 0.019(1) 0.022(1) -0.007(1) -0.003(1) -0.0038(10) N(2) 0.019(1) 0.014(1) 0.018(1) -0.0061(10) -0.0018(10) -0.0004(9) N(3) 0.018(1) 0.016(1) 0.020(1) -0.0029(10) -0.0012(10) 0.0003(9) N(4) 0.021(1) 0.012(1) 0.021(1) -0.0027(10) -0.003(1) -0.0007(9) N(5) 0.028(1) 0.022(1) 0.022(1) -0.012(1) -0.006(1) 0.001(1) N(6) 0.016(1) 0.020(1) 0.023(1) -0.007(1) -0.003(1) 0.0010(10) N(7) 0.015(1) 0.014(1) 0.020(1) -0.0027(9) -0.0030(10) -0.0001(9) N(8) 0.019(1) 0.014(1) 0.018(1) -0.0044(10) -0.0014(10) -0.0026(9) N(9) 0.016(1) 0.014(1) 0.024(1) -0.0018(10) -0.004(1) -0.0010(10) N(10) 0.019(1) 0.022(1) 0.029(1) -0.004(1) -0.005(1) -0.001(1) C(1) 0.025(2) 0.027(2) 0.027(2) -0.011(1) 0.000(1) -0.008(1) C(2) 0.034(2) 0.045(2) 0.019(2) -0.022(2) 0.003(1) -0.007(1) C(3) 0.044(2) 0.041(2) 0.023(2) -0.027(2) -0.006(2) 0.006(1) C(4) 0.035(2) 0.023(2) 0.027(2) -0.013(1) -0.006(1) 0.002(1) C(5) 0.019(1) 0.018(1) 0.019(1) -0.009(1) -0.006(1) 0.002(1) C(6) 0.019(1) 0.013(1) 0.023(2) -0.004(1) -0.003(1) -0.001(1) C(7) 0.031(2) 0.031(2) 0.027(2) -0.015(2) 0.004(2) -0.011(1) C(8) 0.016(1) 0.018(1) 0.020(1) -0.004(1) -0.002(1) -0.002(1) C(9) 0.013(1) 0.018(1) 0.020(1) -0.003(1) 0.000(1) -0.001(1) C(10) 0.021(2) 0.022(2) 0.020(2) -0.005(1) -0.002(1) -0.003(1) C(11) 0.029(2) 0.031(2) 0.016(2) -0.012(1) -0.001(1) 0.001(1) C(12) 0.029(2) 0.020(2) 0.023(2) -0.008(1) -0.005(1) 0.005(1) C(13) 0.016(1) 0.020(1) 0.020(1) -0.004(1) -0.004(1) 0.001(1) C(14) 0.019(1) 0.018(1) 0.019(1) -0.007(1) 0.000(1) 0.002(1) C(15) 0.020(2) 0.015(1) 0.028(2) -0.004(1) -0.004(1) -0.005(1) C(16) 0.045(2) 0.022(2) 0.042(2) -0.016(2) -0.014(2) 0.007(2) C(17) 0.031(2) 0.023(2) 0.025(2) -0.012(1) -0.003(1) -0.004(1) C(18) 0.090(4) 0.024(2) 0.036(2) -0.020(2) -0.018(2) -0.005(2) C(19) 0.112(4) 0.044(3) 0.038(2) -0.038(3) -0.028(3) -0.005(2) C(20) 0.088(3) 0.048(3) 0.034(2) -0.040(2) -0.034(2) 0.011(2) C(21) 0.045(2) 0.028(2) 0.030(2) -0.019(2) -0.014(2) 0.005(1) C(22) 0.021(2) 0.026(2) 0.033(2) -0.010(1) -0.003(1) 0.003(1) C(23) 0.023(2) 0.043(2) 0.029(2) -0.016(2) -0.001(1) 0.007(2) C(24) 0.021(2) 0.046(2) 0.027(2) -0.009(2) 0.004(1) -0.005(2) C(25) 0.020(2) 0.030(2) 0.028(2) -0.003(1) -0.001(1) -0.006(1) C(26) 0.014(1) 0.022(2) 0.025(2) -0.006(1) -0.006(1) -0.003(1) C(27) 0.016(1) 0.016(1) 0.024(2) -0.003(1) -0.001(1) -0.003(1) C(28) 0.019(2) 0.043(2) 0.035(2) -0.004(2) -0.007(2) 0.008(2) C(29) 0.018(1) 0.017(1) 0.021(2) -0.005(1) -0.007(1) 0.001(1) C(30) 0.019(1) 0.018(1) 0.019(1) -0.008(1) -0.003(1) 0.000(1) C(31) 0.029(2) 0.029(2) 0.021(2) -0.010(1) -0.006(1) 0.004(1) C(32) 0.038(2) 0.041(2) 0.014(2) -0.016(2) 0.002(1) 0.000(1) C(33) 0.026(2) 0.028(2) 0.021(2) -0.010(1) 0.003(1) -0.009(1) C(34) 0.021(1) 0.016(1) 0.021(2) -0.008(1) -0.001(1) -0.004(1) C(35) 0.019(1) 0.014(1) 0.025(2) -0.005(1) 0.002(1) -0.001(1) C(36) 0.018(2) 0.017(2) 0.032(2) 0.001(1) -0.005(1) -0.001(1) C(37) 0.018(2) 0.069(3) 0.043(3) -0.006(2) -0.002(2) -0.007(2) C(38) 0.015(1) 0.023(2) 0.032(2) -0.005(1) -0.007(1) 0.001(1) C(39) 0.028(2) 0.023(2) 0.042(2) -0.002(1) -0.013(2) 0.004(1) C(40) 0.034(2) 0.045(2) 0.033(2) -0.013(2) -0.017(2) 0.009(2) C(41) 0.027(2) 0.043(2) 0.029(2) -0.013(2) -0.007(1) -0.005(2) C(42) 0.020(2) 0.031(2) 0.034(2) -0.007(1) -0.006(1) -0.006(1) #------------------------------------------------------------------------------ _computing_data_collection 'CRYSTALCLEAR' _computing_cell_refinement 'CRYSTALCLEAR' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 Cu(1) N(1) 2.070(3) . . yes Cu(1) N(2) 1.922(2) . . yes Cu(1) N(9) 1.936(2) . . yes Cu(1) N(10) 2.189(3) . . yes Cu(2) N(4) 1.925(2) . . yes Cu(2) N(5) 2.089(3) . . yes Cu(2) N(6) 2.070(2) . . yes Cu(2) N(7) 1.923(2) . . yes O(1) C(8) 1.252(3) . . yes O(2) C(14) 1.248(3) . . yes O(3) C(29) 1.261(3) . . yes O(4) C(35) 1.261(3) . . yes N(1) C(1) 1.348(4) . . yes N(1) C(5) 1.337(4) . . yes N(2) C(6) 1.461(4) . . yes N(2) C(8) 1.320(4) . . yes N(3) C(9) 1.349(4) . . yes N(3) C(13) 1.348(4) . . yes N(4) C(14) 1.319(4) . . yes N(4) C(15) 1.464(4) . . yes N(5) C(17) 1.330(4) . . yes N(5) C(21) 1.337(5) . . yes N(6) C(22) 1.343(4) . . yes N(6) C(26) 1.342(4) . . yes N(7) C(27) 1.461(3) . . yes N(7) C(29) 1.310(4) . . yes N(8) C(30) 1.350(3) . . yes N(8) C(34) 1.340(3) . . yes N(9) C(35) 1.315(4) . . yes N(9) C(36) 1.463(4) . . yes N(10) C(38) 1.336(4) . . yes N(10) C(42) 1.344(4) . . yes C(1) C(2) 1.367(5) . . yes C(2) C(3) 1.388(5) . . yes C(3) C(4) 1.370(5) . . yes C(4) C(5) 1.390(5) . . yes C(5) C(6) 1.514(4) . . yes C(6) C(7) 1.522(6) . . yes C(8) C(9) 1.500(4) . . yes C(9) C(10) 1.384(4) . . yes C(10) C(11) 1.379(4) . . yes C(11) C(12) 1.391(5) . . yes C(12) C(13) 1.383(4) . . yes C(13) C(14) 1.512(4) . . yes C(15) C(16) 1.535(6) . . yes C(15) C(17) 1.508(5) . . yes C(17) C(18) 1.391(6) . . yes C(18) C(19) 1.373(7) . . yes C(19) C(20) 1.375(6) . . yes C(20) C(21) 1.381(7) . . yes C(22) C(23) 1.375(4) . . yes C(23) C(24) 1.378(5) . . yes C(24) C(25) 1.386(5) . . yes C(25) C(26) 1.384(4) . . yes C(26) C(27) 1.506(4) . . yes C(27) C(28) 1.529(5) . . yes C(29) C(30) 1.505(4) . . yes C(30) C(31) 1.381(4) . . yes C(31) C(32) 1.385(4) . . yes C(32) C(33) 1.377(4) . . yes C(33) C(34) 1.389(4) . . yes C(34) C(35) 1.502(4) . . yes C(36) C(37) 1.535(6) . . yes C(36) C(38) 1.507(5) . . yes C(38) C(39) 1.388(5) . . yes C(39) C(40) 1.374(5) . . yes C(40) C(41) 1.384(5) . . yes C(41) C(42) 1.377(5) . . yes #------------------------------------------------------------------------------ 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 N(1) Cu(1) N(2) 81.14(9) . . . yes N(1) Cu(1) N(9) 100.44(10) . . . yes N(1) Cu(1) N(10) 120.7(1) . . . yes N(2) Cu(1) N(9) 175.0(1) . . . yes N(2) Cu(1) N(10) 103.31(10) . . . yes N(9) Cu(1) N(10) 80.1(1) . . . yes N(4) Cu(2) N(5) 81.5(1) . . . yes N(4) Cu(2) N(6) 102.10(9) . . . yes N(4) Cu(2) N(7) 171.3(1) . . . yes N(5) Cu(2) N(6) 118.6(1) . . . yes N(5) Cu(2) N(7) 104.0(1) . . . yes N(6) Cu(2) N(7) 81.35(9) . . . yes Cu(1) N(1) C(1) 127.6(2) . . . yes Cu(1) N(1) C(5) 113.8(2) . . . yes C(1) N(1) C(5) 118.6(3) . . . yes Cu(1) N(2) C(6) 118.5(2) . . . yes Cu(1) N(2) C(8) 123.2(2) . . . yes C(6) N(2) C(8) 118.2(2) . . . yes C(9) N(3) C(13) 118.2(2) . . . yes Cu(2) N(4) C(14) 124.2(2) . . . yes Cu(2) N(4) C(15) 118.0(2) . . . yes C(14) N(4) C(15) 117.7(2) . . . yes Cu(2) N(5) C(17) 112.9(2) . . . yes Cu(2) N(5) C(21) 127.0(2) . . . yes C(17) N(5) C(21) 120.0(3) . . . yes Cu(2) N(6) C(22) 126.4(2) . . . yes Cu(2) N(6) C(26) 113.6(2) . . . yes C(22) N(6) C(26) 119.5(2) . . . yes Cu(2) N(7) C(27) 118.1(2) . . . yes Cu(2) N(7) C(29) 123.2(2) . . . yes C(27) N(7) C(29) 118.6(2) . . . yes C(30) N(8) C(34) 117.9(2) . . . yes Cu(1) N(9) C(35) 125.1(2) . . . yes Cu(1) N(9) C(36) 117.7(2) . . . yes C(35) N(9) C(36) 117.1(2) . . . yes Cu(1) N(10) C(38) 110.4(2) . . . yes Cu(1) N(10) C(42) 127.2(2) . . . yes C(38) N(10) C(42) 118.6(3) . . . yes N(1) C(1) C(2) 122.7(3) . . . yes C(1) C(2) C(3) 118.8(3) . . . yes C(2) C(3) C(4) 118.9(4) . . . yes C(3) C(4) C(5) 119.5(3) . . . yes N(1) C(5) C(4) 121.5(3) . . . yes N(1) C(5) C(6) 117.1(3) . . . yes C(4) C(5) C(6) 121.4(3) . . . yes N(2) C(6) C(5) 108.4(2) . . . yes N(2) C(6) C(7) 110.4(3) . . . yes C(5) C(6) C(7) 109.7(3) . . . yes O(1) C(8) N(2) 127.8(3) . . . yes O(1) C(8) C(9) 119.6(2) . . . yes N(2) C(8) C(9) 112.5(2) . . . yes N(3) C(9) C(8) 116.9(2) . . . yes N(3) C(9) C(10) 122.4(3) . . . yes C(8) C(9) C(10) 120.5(3) . . . yes C(9) C(10) C(11) 119.2(3) . . . yes C(10) C(11) C(12) 118.6(3) . . . yes C(11) C(12) C(13) 119.2(3) . . . yes N(3) C(13) C(12) 122.2(3) . . . yes N(3) C(13) C(14) 117.3(2) . . . yes C(12) C(13) C(14) 120.2(3) . . . yes O(2) C(14) N(4) 128.1(3) . . . yes O(2) C(14) C(13) 118.9(3) . . . yes N(4) C(14) C(13) 112.8(2) . . . yes N(4) C(15) C(16) 110.7(3) . . . yes N(4) C(15) C(17) 109.1(2) . . . yes C(16) C(15) C(17) 109.9(3) . . . yes N(5) C(17) C(15) 117.8(3) . . . yes N(5) C(17) C(18) 120.3(3) . . . yes C(15) C(17) C(18) 121.9(3) . . . yes C(17) C(18) C(19) 119.8(4) . . . yes C(18) C(19) C(20) 119.3(5) . . . yes C(19) C(20) C(21) 118.3(4) . . . yes N(5) C(21) C(20) 122.2(3) . . . yes N(6) C(22) C(23) 122.3(3) . . . yes C(22) C(23) C(24) 118.6(3) . . . yes C(23) C(24) C(25) 119.5(3) . . . yes C(24) C(25) C(26) 119.1(3) . . . yes N(6) C(26) C(25) 121.1(3) . . . yes N(6) C(26) C(27) 116.4(2) . . . yes C(25) C(26) C(27) 122.4(3) . . . yes N(7) C(27) C(26) 109.1(2) . . . yes N(7) C(27) C(28) 111.6(3) . . . yes C(26) C(27) C(28) 108.7(3) . . . yes O(3) C(29) N(7) 127.7(2) . . . yes O(3) C(29) C(30) 118.6(3) . . . yes N(7) C(29) C(30) 113.7(2) . . . yes N(8) C(30) C(29) 116.4(2) . . . yes N(8) C(30) C(31) 122.8(2) . . . yes C(29) C(30) C(31) 120.8(2) . . . yes C(30) C(31) C(32) 118.5(3) . . . yes C(31) C(32) C(33) 119.4(3) . . . yes C(32) C(33) C(34) 118.7(3) . . . yes N(8) C(34) C(33) 122.6(2) . . . yes N(8) C(34) C(35) 117.5(2) . . . yes C(33) C(34) C(35) 119.6(2) . . . yes O(4) C(35) N(9) 126.8(3) . . . yes O(4) C(35) C(34) 118.3(3) . . . yes N(9) C(35) C(34) 114.7(2) . . . yes N(9) C(36) C(37) 110.8(3) . . . yes N(9) C(36) C(38) 109.2(2) . . . yes C(37) C(36) C(38) 109.0(3) . . . yes N(10) C(38) C(36) 115.9(3) . . . yes N(10) C(38) C(39) 121.5(3) . . . yes C(36) C(38) C(39) 122.5(3) . . . yes C(38) C(39) C(40) 119.5(3) . . . yes C(39) C(40) C(41) 119.2(3) . . . yes C(40) C(41) C(42) 118.3(3) . . . yes N(10) C(42) C(41) 122.8(3) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu(1) N(1) C(1) C(2) 179.1(3) . . . . yes Cu(1) N(1) C(5) C(4) -179.1(3) . . . . yes Cu(1) N(1) C(5) C(6) 4.0(4) . . . . yes Cu(1) N(2) C(6) C(5) 11.6(3) . . . . yes Cu(1) N(2) C(6) C(7) -108.5(2) . . . . yes Cu(1) N(2) C(8) O(1) -175.1(3) . . . . yes Cu(1) N(2) C(8) C(9) 8.4(4) . . . . yes Cu(1) N(9) C(35) O(4) 179.8(3) . . . . yes Cu(1) N(9) C(35) C(34) 4.6(4) . . . . yes Cu(1) N(9) C(36) C(37) -97.8(3) . . . . yes Cu(1) N(9) C(36) C(38) 22.2(4) . . . . yes Cu(1) N(10) C(38) C(36) 22.5(4) . . . . yes Cu(1) N(10) C(38) C(39) -158.9(3) . . . . yes Cu(1) N(10) C(42) C(41) 154.3(3) . . . . yes Cu(2) N(4) C(14) O(2) -172.5(3) . . . . yes Cu(2) N(4) C(14) C(13) 12.7(4) . . . . yes Cu(2) N(4) C(15) C(16) -114.1(3) . . . . yes Cu(2) N(4) C(15) C(17) 7.0(3) . . . . yes Cu(2) N(5) C(17) C(15) 7.3(4) . . . . yes Cu(2) N(5) C(17) C(18) -175.2(3) . . . . yes Cu(2) N(5) C(21) C(20) 175.8(3) . . . . yes Cu(2) N(6) C(22) C(23) 169.8(3) . . . . yes Cu(2) N(6) C(26) C(25) -170.8(3) . . . . yes Cu(2) N(6) C(26) C(27) 11.8(4) . . . . yes Cu(2) N(7) C(27) C(26) 8.9(4) . . . . yes Cu(2) N(7) C(27) C(28) -111.2(3) . . . . yes Cu(2) N(7) C(29) O(3) -177.6(3) . . . . yes Cu(2) N(7) C(29) C(30) 4.9(4) . . . . yes O(1) C(8) N(2) C(6) 4.7(5) . . . . yes O(1) C(8) C(9) N(3) 153.1(3) . . . . yes O(1) C(8) C(9) C(10) -31.7(5) . . . . yes O(2) C(14) N(4) C(15) 4.0(5) . . . . yes O(2) C(14) C(13) N(3) 139.8(3) . . . . yes O(2) C(14) C(13) C(12) -46.4(5) . . . . yes O(3) C(29) N(7) C(27) -1.2(6) . . . . yes O(3) C(29) C(30) N(8) 148.4(3) . . . . yes O(3) C(29) C(30) C(31) -33.3(5) . . . . yes O(4) C(35) N(9) C(36) 1.0(5) . . . . yes O(4) C(35) C(34) N(8) 149.1(3) . . . . yes O(4) C(35) C(34) C(33) -36.9(5) . . . . yes N(1) Cu(1) N(2) C(6) -8.0(2) . . . . yes N(1) Cu(1) N(2) C(8) 171.8(3) . . . . yes N(1) Cu(1) N(9) C(35) -68.0(3) . . . . yes N(1) Cu(1) N(9) C(36) 110.9(2) . . . . yes N(1) Cu(1) N(10) C(38) -104.2(2) . . . . yes N(1) Cu(1) N(10) C(42) 98.3(3) . . . . yes N(1) C(1) C(2) C(3) 0.2(6) . . . . yes N(1) C(5) C(4) C(3) -0.5(6) . . . . yes N(1) C(5) C(6) N(2) -9.7(4) . . . . yes N(1) C(5) C(6) C(7) 110.9(3) . . . . yes N(2) Cu(1) N(1) C(1) -177.2(3) . . . . yes N(2) Cu(1) N(1) C(5) 2.0(2) . . . . yes N(2) Cu(1) N(9) C(35) 39(1) . . . . yes N(2) Cu(1) N(9) C(36) -141(1) . . . . yes N(2) Cu(1) N(10) C(38) 168.3(2) . . . . yes N(2) Cu(1) N(10) C(42) 10.8(3) . . . . yes N(2) C(6) C(5) C(4) 173.4(3) . . . . yes N(2) C(8) C(9) N(3) -30.2(4) . . . . yes N(2) C(8) C(9) C(10) 145.1(3) . . . . yes N(3) C(9) C(10) C(11) 3.7(5) . . . . yes N(3) C(13) C(12) C(11) 3.9(5) . . . . yes N(3) C(13) C(14) N(4) -44.8(4) . . . . yes N(4) Cu(2) N(5) C(17) -2.5(2) . . . . yes N(4) Cu(2) N(5) C(21) -179.1(3) . . . . yes N(4) Cu(2) N(6) C(22) -5.1(3) . . . . yes N(4) Cu(2) N(6) C(26) 166.7(2) . . . . yes N(4) Cu(2) N(7) C(27) -116.7(6) . . . . yes N(4) Cu(2) N(7) C(29) 59.8(8) . . . . yes N(4) C(14) C(13) C(12) 128.9(3) . . . . yes N(4) C(15) C(17) N(5) -9.3(4) . . . . yes N(4) C(15) C(17) C(18) 173.2(4) . . . . yes N(5) Cu(2) N(4) C(14) 173.6(3) . . . . yes N(5) Cu(2) N(4) C(15) -2.9(2) . . . . yes N(5) Cu(2) N(6) C(22) 81.8(3) . . . . yes N(5) Cu(2) N(6) C(26) -106.5(3) . . . . yes N(5) Cu(2) N(7) C(27) 114.9(2) . . . . yes N(5) Cu(2) N(7) C(29) -68.7(3) . . . . yes N(5) C(17) C(15) C(16) 112.4(4) . . . . yes N(5) C(17) C(18) C(19) -2.0(7) . . . . yes N(5) C(21) C(20) C(19) -0.3(7) . . . . yes N(6) Cu(2) N(4) C(14) -68.8(3) . . . . yes N(6) Cu(2) N(4) C(15) 114.7(2) . . . . yes N(6) Cu(2) N(5) C(17) -101.7(2) . . . . yes N(6) Cu(2) N(5) C(21) 81.7(3) . . . . yes N(6) Cu(2) N(7) C(27) -2.6(2) . . . . yes N(6) Cu(2) N(7) C(29) 173.9(3) . . . . yes N(6) C(22) C(23) C(24) 0.3(6) . . . . yes N(6) C(26) C(25) C(24) -0.4(6) . . . . yes N(6) C(26) C(27) N(7) -13.3(4) . . . . yes N(6) C(26) C(27) C(28) 108.6(3) . . . . yes N(7) Cu(2) N(4) C(14) 43.9(8) . . . . yes N(7) Cu(2) N(4) C(15) -132.6(6) . . . . yes N(7) Cu(2) N(5) C(17) 170.6(2) . . . . yes N(7) Cu(2) N(5) C(21) -6.0(3) . . . . yes N(7) Cu(2) N(6) C(22) -177.0(3) . . . . yes N(7) Cu(2) N(6) C(26) -5.2(3) . . . . yes N(7) C(27) C(26) C(25) 169.3(3) . . . . yes N(7) C(29) C(30) N(8) -33.9(5) . . . . yes N(7) C(29) C(30) C(31) 144.4(4) . . . . yes N(8) C(30) C(31) C(32) 3.7(6) . . . . yes N(8) C(34) C(33) C(32) 3.5(6) . . . . yes N(8) C(34) C(35) N(9) -35.2(5) . . . . yes N(9) Cu(1) N(1) C(1) -2.1(3) . . . . yes N(9) Cu(1) N(1) C(5) 177.2(2) . . . . yes N(9) Cu(1) N(2) C(6) -116(1) . . . . yes N(9) Cu(1) N(2) C(8) 63(1) . . . . yes N(9) Cu(1) N(10) C(38) -7.9(2) . . . . yes N(9) Cu(1) N(10) C(42) -165.3(3) . . . . yes N(9) C(35) C(34) C(33) 138.7(3) . . . . yes N(9) C(36) C(38) N(10) -29.4(4) . . . . yes N(9) C(36) C(38) C(39) 152.0(3) . . . . yes N(10) Cu(1) N(1) C(1) 82.5(3) . . . . yes N(10) Cu(1) N(1) C(5) -98.3(2) . . . . yes N(10) Cu(1) N(2) C(6) 111.7(2) . . . . yes N(10) Cu(1) N(2) C(8) -68.6(3) . . . . yes N(10) Cu(1) N(9) C(35) 172.3(3) . . . . yes N(10) Cu(1) N(9) C(36) -8.8(2) . . . . yes N(10) C(38) C(36) C(37) 91.7(4) . . . . yes N(10) C(38) C(39) C(40) 1.1(6) . . . . yes N(10) C(42) C(41) C(40) 0.5(6) . . . . yes C(1) N(1) C(5) C(4) 0.2(5) . . . . yes C(1) N(1) C(5) C(6) -176.7(3) . . . . yes C(1) C(2) C(3) C(4) -0.5(6) . . . . yes C(2) C(1) N(1) C(5) -0.1(6) . . . . yes C(2) C(3) C(4) C(5) 0.6(6) . . . . yes C(3) C(4) C(5) C(6) 176.3(4) . . . . yes C(4) C(5) C(6) C(7) -66.0(4) . . . . yes C(5) C(6) N(2) C(8) -168.2(3) . . . . yes C(6) N(2) C(8) C(9) -171.8(3) . . . . yes C(7) C(6) N(2) C(8) 71.7(3) . . . . yes C(8) C(9) N(3) C(13) 173.8(3) . . . . yes C(8) C(9) C(10) C(11) -171.3(3) . . . . yes C(9) N(3) C(13) C(12) -2.5(5) . . . . yes C(9) N(3) C(13) C(14) 171.2(3) . . . . yes C(9) C(10) C(11) C(12) -2.1(5) . . . . yes C(10) C(9) N(3) C(13) -1.4(5) . . . . yes C(10) C(11) C(12) C(13) -1.5(6) . . . . yes C(11) C(12) C(13) C(14) -169.5(3) . . . . yes C(13) C(14) N(4) C(15) -170.8(3) . . . . yes C(14) N(4) C(15) C(16) 69.2(4) . . . . yes C(14) N(4) C(15) C(17) -169.7(3) . . . . yes C(15) C(17) N(5) C(21) -175.8(3) . . . . yes C(15) C(17) C(18) C(19) 175.5(5) . . . . yes C(16) C(15) C(17) C(18) -65.1(4) . . . . yes C(17) N(5) C(21) C(20) -0.6(6) . . . . yes C(17) C(18) C(19) C(20) 1.1(8) . . . . yes C(18) C(17) N(5) C(21) 1.7(6) . . . . yes C(18) C(19) C(20) C(21) 0.1(8) . . . . yes C(22) N(6) C(26) C(25) 1.5(5) . . . . yes C(22) N(6) C(26) C(27) -175.9(3) . . . . yes C(22) C(23) C(24) C(25) 0.8(6) . . . . yes C(23) C(22) N(6) C(26) -1.5(6) . . . . yes C(23) C(24) C(25) C(26) -0.8(6) . . . . yes C(24) C(25) C(26) C(27) 176.9(4) . . . . yes C(25) C(26) C(27) C(28) -68.7(4) . . . . yes C(26) C(27) N(7) C(29) -167.8(3) . . . . yes C(27) N(7) C(29) C(30) -178.7(3) . . . . yes C(28) C(27) N(7) C(29) 72.1(4) . . . . yes C(29) C(30) N(8) C(34) 176.5(3) . . . . yes C(29) C(30) C(31) C(32) -174.4(4) . . . . yes C(30) N(8) C(34) C(33) -2.0(5) . . . . yes C(30) N(8) C(34) C(35) 171.8(3) . . . . yes C(30) C(31) C(32) C(33) -2.1(7) . . . . yes C(31) C(30) N(8) C(34) -1.7(5) . . . . yes C(31) C(32) C(33) C(34) -1.3(6) . . . . yes C(32) C(33) C(34) C(35) -170.1(4) . . . . yes C(34) C(35) N(9) C(36) -174.2(3) . . . . yes C(35) N(9) C(36) C(37) 81.2(4) . . . . yes C(35) N(9) C(36) C(38) -158.9(3) . . . . yes C(36) C(38) N(10) C(42) -177.8(3) . . . . yes C(36) C(38) C(39) C(40) 179.6(4) . . . . yes C(37) C(36) C(38) C(39) -86.9(4) . . . . yes C(38) N(10) C(42) C(41) -1.6(6) . . . . yes C(38) C(39) C(40) C(41) -2.2(6) . . . . yes C(39) C(38) N(10) C(42) 0.8(5) . . . . yes C(39) C(40) C(41) C(42) 1.5(6) . . . . yes C(39) C(40) C(41) C(42) 1.5(6) . . . . yes #------------------------------------------------------------------------------ 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 O(1) C(24) 3.395(4) . 2_467 ? O(1) C(41) 3.427(5) . 2_567 ? O(2) O(8) 2.807(3) . 2_557 ? O(2) C(12) 3.225(4) . 2_557 ? O(2) C(11) 3.429(4) . 2_557 ? O(4) O(6) 2.834(4) . 2_656 ? O(5) O(10) 2.776(3) . 1_645 ? O(5) O(8) 2.824(4) . 2_557 ? O(5) C(4) 3.340(6) . 1_545 ? O(5) C(3) 3.562(6) . 1_545 ? O(6) O(10) 2.817(5) . 2_566 ? O(6) O(7) 2.856(4) . 2_566 ? O(6) O(6) 3.434(6) . 2_656 ? O(6) C(19) 3.531(8) . 2_556 ? O(8) O(9) 2.876(5) . 2_467 ? O(10) C(2) 3.256(4) . 2_566 ? C(3) C(31) 3.477(6) . 2_566 ? C(3) C(28) 3.521(6) . 1_655 ? C(4) C(28) 3.558(6) . 1_655 ? C(7) C(11) 3.539(6) . 2_567 ? C(23) C(41) 3.371(6) . 1_455 ? C(23) C(42) 3.521(6) . 1_455 ? C(24) C(25) 3.444(6) . 2_467 ? C(24) C(42) 3.518(6) . 1_455 ? C(31) C(31) 3.370(8) . 2_566 ? C(40) C(40) 3.579(7) . 2_657 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_s-mono2 _database_code_CSD 182241 _audit_creation_date 'Mon Jan 28 16:44:46 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C21 H21 Br2 Cu N5 O2 ' _chemical_formula_moiety 'C21 H21 Br2 Cu N5 O2 ' _chemical_formula_weight 598.78 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 10.716(7) _cell_length_b 11.405(7) _cell_length_c 17.92(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2190(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6472 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 223.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'Block' _exptl_crystal_colour 'Green' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.816 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 4.686 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.253 _exptl_absorpt_correction_T_max 0.626 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 16671 _diffrn_reflns_av_R_equivalents 0.089 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). 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 4844 _reflns_number_gt 4496 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0725 _refine_ls_wR_factor_ref 0.1945 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4496 _refine_ls_number_parameters 280 _refine_ls_goodness_of_fit_ref 1.275 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack -0.02(2) _refine_diff_density_max 1.85 _refine_diff_density_min -1.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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) ; 'O' 'O' 0.011 0.006 ;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) ; 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br(1) Br 0.09093(8) -0.00673(7) 0.12213(4) 0.0409(2) Uani 1.00 d . . . Br(2) Br 0.43420(7) 0.13579(6) 0.15669(5) 0.0427(2) Uani 1.00 d . . . Cu(1) Cu 0.19802(9) 0.11619(7) 0.21001(5) 0.0324(2) Uani 1.00 d . . . O(1) O 0.2457(6) 0.2196(5) 0.4234(3) 0.044(1) Uani 1.00 d . . . O(2) O 0.1872(6) -0.2750(5) 0.2010(3) 0.047(1) Uani 1.00 d . . . N(1) N 0.1316(6) 0.2674(5) 0.1658(4) 0.035(1) Uani 1.00 d . . . N(2) N 0.2086(7) 0.2138(5) 0.2973(4) 0.033(1) Uani 1.00 d . . . N(3) N 0.2452(6) -0.0121(5) 0.2907(4) 0.034(1) Uani 1.00 d . . . N(4) N 0.3510(6) -0.1598(5) 0.1654(4) 0.036(1) Uani 1.00 d . . . N(5) N 0.3325(6) -0.3823(5) 0.0199(3) 0.031(1) Uani 1.00 d . . . C(1) C 0.0942(8) 0.2839(7) 0.0952(5) 0.041(2) Uani 1.00 d . . . C(2) C 0.057(1) 0.3932(9) 0.0672(5) 0.054(2) Uani 1.00 d . . . C(3) C 0.0574(10) 0.4853(8) 0.1157(6) 0.052(2) Uani 1.00 d . . . C(4) C 0.0943(8) 0.4701(7) 0.1900(5) 0.043(2) Uani 1.00 d . . . C(5) C 0.1362(7) 0.3595(7) 0.2119(4) 0.035(1) Uani 1.00 d . . . C(6) C 0.1830(8) 0.3394(6) 0.2903(5) 0.036(2) Uani 1.00 d . . . C(7) C 0.2990(10) 0.4133(7) 0.3053(5) 0.047(2) Uani 1.00 d . . . C(8) C 0.2335(8) 0.1685(6) 0.3614(4) 0.035(2) Uani 1.00 d . . . C(9) C 0.2482(6) 0.0357(6) 0.3593(4) 0.027(1) Uani 1.00 d . . . C(10) C 0.2641(8) -0.0267(7) 0.4243(5) 0.041(2) Uani 1.00 d . . . C(11) C 0.2651(9) -0.1498(7) 0.4187(5) 0.042(2) Uani 1.00 d . . . C(12) C 0.2608(9) -0.1981(6) 0.3500(5) 0.044(2) Uani 1.00 d . . . C(13) C 0.2539(7) -0.1292(6) 0.2873(4) 0.033(1) Uani 1.00 d . . . C(14) C 0.2569(8) -0.1930(6) 0.2131(5) 0.037(2) Uani 1.00 d . . . C(15) C 0.3528(8) -0.2036(6) 0.0902(4) 0.036(2) Uani 1.00 d . . . C(16) C 0.4571(9) -0.1473(7) 0.0472(5) 0.043(2) Uani 1.00 d . . . C(17) C 0.3665(7) -0.3348(6) 0.0855(4) 0.032(1) Uani 1.00 d . . . C(18) C 0.4200(8) -0.4057(7) 0.1410(5) 0.041(2) Uani 1.00 d . . . C(19) C 0.4307(9) -0.5243(7) 0.1258(5) 0.043(2) Uani 1.00 d . . . C(20) C 0.3927(9) -0.5702(7) 0.0584(6) 0.047(2) Uani 1.00 d . . . C(21) C 0.3441(8) -0.4997(7) 0.0054(5) 0.039(2) Uani 1.00 d . . . H(1) H 0.0885 0.2180 0.0480 0.0599 Uiso 1.00 calc . . . H(2) H 0.0296 0.4001 0.0161 0.0648 Uiso 1.00 calc . . . H(3) H 0.0324 0.5619 0.0993 0.0590 Uiso 1.00 calc . . . H(4) H 0.0922 0.5348 0.2251 0.0510 Uiso 1.00 calc . . . H(5) H 0.1192 0.3599 0.3250 0.0401 Uiso 1.00 calc . . . H(6) H 0.3704 0.3749 0.2869 0.0526 Uiso 1.00 calc . . . H(7) H 0.2898 0.4876 0.2824 0.0526 Uiso 1.00 calc . . . H(8) H 0.3078 0.4243 0.3583 0.0526 Uiso 1.00 calc . . . H(9) H 0.2739 0.0122 0.4718 0.0466 Uiso 1.00 calc . . . H(10) H 0.2674 -0.1991 0.4622 0.0475 Uiso 1.00 calc . . . H(11) H 0.2630 -0.2820 0.3453 0.0523 Uiso 1.00 calc . . . H(12) H 0.2747 -0.1824 0.0667 0.0417 Uiso 1.00 calc . . . H(13) H 0.5355 -0.1689 0.0709 0.0529 Uiso 1.00 calc . . . H(14) H 0.4585 -0.1740 -0.0023 0.0529 Uiso 1.00 calc . . . H(15) H 0.4502 -0.0647 0.0490 0.0529 Uiso 1.00 calc . . . H(16) H 0.4496 -0.3728 0.1867 0.0500 Uiso 1.00 calc . . . H(17) H 0.4633 -0.5764 0.1623 0.0480 Uiso 1.00 calc . . . H(18) H 0.4022 -0.6526 0.0502 0.0556 Uiso 1.00 calc . . . H(19) H 0.3184 -0.5313 -0.0419 0.0481 Uiso 1.00 calc . . . H(20) H 0.2990 -0.3325 -0.0175 0.0357 Uiso 1.00 calc . . . 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 Br(1) 0.0454(4) 0.0425(4) 0.0349(4) -0.0030(3) -0.0066(3) -0.0017(3) Br(2) 0.0437(4) 0.0333(4) 0.0511(5) -0.0021(3) 0.0060(4) 0.0028(3) Cu(1) 0.0419(5) 0.0297(4) 0.0258(4) 0.0021(3) -0.0019(4) 0.0007(3) O(1) 0.068(4) 0.035(3) 0.028(3) 0.004(3) 0.002(3) -0.005(2) O(2) 0.068(4) 0.035(3) 0.038(3) -0.016(3) 0.010(3) -0.005(2) N(1) 0.042(3) 0.029(3) 0.034(3) 0.003(2) 0.001(3) 0.001(2) N(2) 0.050(4) 0.025(3) 0.025(3) 0.005(2) 0.001(3) 0.001(2) N(3) 0.046(3) 0.027(3) 0.028(3) 0.000(2) 0.005(3) 0.001(2) N(4) 0.046(4) 0.032(3) 0.030(3) 0.003(2) 0.006(3) -0.004(2) N(5) 0.048(3) 0.022(2) 0.023(3) 0.003(2) 0.004(2) -0.004(2) C(1) 0.040(4) 0.043(4) 0.040(4) 0.008(3) -0.008(4) 0.004(3) C(2) 0.060(6) 0.057(5) 0.045(5) 0.005(5) -0.001(4) 0.026(4) C(3) 0.048(5) 0.050(5) 0.057(6) 0.010(4) -0.011(4) 0.018(4) C(4) 0.044(5) 0.035(4) 0.050(5) 0.007(3) -0.003(4) 0.011(3) C(5) 0.038(4) 0.035(3) 0.031(4) -0.001(3) 0.004(3) 0.011(3) C(6) 0.050(4) 0.026(3) 0.032(4) 0.003(3) 0.003(4) -0.002(3) C(7) 0.058(5) 0.041(4) 0.042(5) -0.008(4) -0.009(4) 0.004(3) C(8) 0.047(4) 0.034(3) 0.024(4) 0.004(3) 0.009(3) -0.002(3) C(9) 0.030(3) 0.032(3) 0.017(3) -0.004(2) 0.002(2) -0.001(2) C(10) 0.050(4) 0.038(4) 0.036(4) 0.003(3) 0.004(4) 0.007(3) C(11) 0.058(5) 0.031(3) 0.037(4) 0.013(3) -0.003(4) 0.011(3) C(12) 0.060(5) 0.023(3) 0.050(5) 0.000(3) -0.006(4) 0.009(3) C(13) 0.042(4) 0.025(3) 0.032(4) -0.003(3) -0.001(3) -0.003(3) C(14) 0.049(4) 0.032(3) 0.032(4) 0.005(3) 0.001(3) -0.010(3) C(15) 0.050(4) 0.032(3) 0.027(4) -0.005(3) 0.000(3) -0.002(3) C(16) 0.056(5) 0.044(4) 0.031(4) -0.015(4) 0.006(4) 0.006(3) C(17) 0.041(4) 0.028(3) 0.027(4) -0.002(3) 0.005(3) 0.002(3) C(18) 0.048(4) 0.039(4) 0.036(4) 0.008(3) 0.009(4) 0.011(3) C(19) 0.049(4) 0.033(4) 0.047(5) 0.006(3) 0.014(4) 0.007(3) C(20) 0.049(5) 0.033(4) 0.058(5) 0.006(3) 0.027(4) 0.005(3) C(21) 0.047(4) 0.028(3) 0.043(4) -0.002(3) 0.007(3) -0.007(3) #------------------------------------------------------------------------------ _computing_data_collection 'CRYSTALCLEAR' _computing_cell_refinement 'CRYSTALCLEAR' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 Br(1) Cu(1) 2.401(1) . . yes Br(2) Cu(1) 2.715(2) . . yes Cu(1) N(1) 2.027(6) . . yes Cu(1) N(2) 1.923(6) . . yes Cu(1) N(3) 2.118(6) . . yes O(1) C(8) 1.261(10) . . yes O(2) C(14) 1.216(10) . . yes N(1) C(1) 1.34(1) . . yes N(1) C(5) 1.337(10) . . yes N(2) C(6) 1.464(9) . . yes N(2) C(8) 1.288(10) . . yes N(3) C(9) 1.347(9) . . yes N(3) C(13) 1.340(9) . . yes N(4) C(14) 1.38(1) . . yes N(4) C(15) 1.44(1) . . yes N(5) C(17) 1.346(9) . . yes N(5) C(21) 1.369(9) . . yes C(1) C(2) 1.40(1) . . yes C(2) C(3) 1.36(1) . . yes C(3) C(4) 1.40(1) . . yes C(4) C(5) 1.39(1) . . yes C(5) C(6) 1.51(1) . . yes C(6) C(7) 1.53(1) . . yes C(8) C(9) 1.523(10) . . yes C(9) C(10) 1.37(1) . . yes C(10) C(11) 1.41(1) . . yes C(11) C(12) 1.35(1) . . yes C(12) C(13) 1.37(1) . . yes C(13) C(14) 1.51(1) . . yes C(15) C(16) 1.50(1) . . yes C(15) C(17) 1.505(10) . . yes C(17) C(18) 1.40(1) . . yes C(18) C(19) 1.39(1) . . yes C(19) C(20) 1.38(1) . . yes C(20) C(21) 1.35(1) . . yes #------------------------------------------------------------------------------ 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) Cu(1) Br(2) 105.24(5) . . . yes Br(1) Cu(1) N(1) 94.1(2) . . . yes Br(1) Cu(1) N(2) 154.1(2) . . . yes Br(1) Cu(1) N(3) 99.1(2) . . . yes Br(2) Cu(1) N(1) 96.9(2) . . . yes Br(2) Cu(1) N(2) 100.6(2) . . . yes Br(2) Cu(1) N(3) 94.3(2) . . . yes N(1) Cu(1) N(2) 81.2(3) . . . yes N(1) Cu(1) N(3) 159.8(3) . . . yes N(2) Cu(1) N(3) 80.3(2) . . . yes Cu(1) N(1) C(1) 126.4(5) . . . yes Cu(1) N(1) C(5) 114.4(5) . . . yes C(1) N(1) C(5) 118.9(7) . . . yes Cu(1) N(2) C(6) 119.1(5) . . . yes Cu(1) N(2) C(8) 120.4(5) . . . yes C(6) N(2) C(8) 120.5(6) . . . yes Cu(1) N(3) C(9) 110.5(4) . . . yes Cu(1) N(3) C(13) 132.4(5) . . . yes C(9) N(3) C(13) 116.3(6) . . . yes C(14) N(4) C(15) 119.8(7) . . . yes C(17) N(5) C(21) 122.3(6) . . . yes N(1) C(1) C(2) 123.3(8) . . . yes C(1) C(2) C(3) 117.0(9) . . . yes C(2) C(3) C(4) 120.9(8) . . . yes C(3) C(4) C(5) 118.0(8) . . . yes N(1) C(5) C(4) 121.7(7) . . . yes N(1) C(5) C(6) 117.9(7) . . . yes C(4) C(5) C(6) 120.4(7) . . . yes N(2) C(6) C(5) 106.9(6) . . . yes N(2) C(6) C(7) 111.9(7) . . . yes C(5) C(6) C(7) 110.6(7) . . . yes O(1) C(8) N(2) 128.5(7) . . . yes O(1) C(8) C(9) 118.1(6) . . . yes N(2) C(8) C(9) 113.5(6) . . . yes N(3) C(9) C(8) 115.0(6) . . . yes N(3) C(9) C(10) 124.6(6) . . . yes C(8) C(9) C(10) 120.4(6) . . . yes C(9) C(10) C(11) 117.2(7) . . . yes C(10) C(11) C(12) 118.1(8) . . . yes C(11) C(12) C(13) 121.0(7) . . . yes N(3) C(13) C(12) 122.5(7) . . . yes N(3) C(13) C(14) 121.3(7) . . . yes C(12) C(13) C(14) 116.2(6) . . . yes O(2) C(14) N(4) 123.4(8) . . . yes O(2) C(14) C(13) 120.9(7) . . . yes N(4) C(14) C(13) 115.3(6) . . . yes N(4) C(15) C(16) 110.0(6) . . . yes N(4) C(15) C(17) 113.5(6) . . . yes C(16) C(15) C(17) 108.9(7) . . . yes N(5) C(17) C(15) 114.9(6) . . . yes N(5) C(17) C(18) 119.9(6) . . . yes C(15) C(17) C(18) 125.0(7) . . . yes C(17) C(18) C(19) 117.2(7) . . . yes C(18) C(19) C(20) 121.3(8) . . . yes C(19) C(20) C(21) 120.3(7) . . . yes N(5) C(21) C(20) 119.0(7) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br(1) Cu(1) N(1) C(1) -25.7(7) . . . . yes Br(1) Cu(1) N(1) C(5) 159.7(5) . . . . yes Br(1) Cu(1) N(2) C(6) -88.3(7) . . . . yes Br(1) Cu(1) N(2) C(8) 89.3(8) . . . . yes Br(1) Cu(1) N(3) C(9) -148.9(5) . . . . yes Br(1) Cu(1) N(3) C(13) 20.1(7) . . . . yes Br(2) Cu(1) N(1) C(1) 80.2(7) . . . . yes Br(2) Cu(1) N(1) C(5) -94.4(5) . . . . yes Br(2) Cu(1) N(2) C(6) 88.3(6) . . . . yes Br(2) Cu(1) N(2) C(8) -94.1(6) . . . . yes Br(2) Cu(1) N(3) C(9) 104.9(5) . . . . yes Br(2) Cu(1) N(3) C(13) -86.1(7) . . . . yes Cu(1) N(1) C(1) C(2) -175.8(7) . . . . yes Cu(1) N(1) C(5) C(4) 179.9(6) . . . . yes Cu(1) N(1) C(5) C(6) -2.8(9) . . . . yes Cu(1) N(2) C(6) C(5) 7.1(8) . . . . yes Cu(1) N(2) C(6) C(7) -114.0(7) . . . . yes Cu(1) N(2) C(8) O(1) 178.8(7) . . . . yes Cu(1) N(2) C(8) C(9) -1.8(9) . . . . yes Cu(1) N(3) C(9) C(8) -7.0(7) . . . . yes Cu(1) N(3) C(9) C(10) 173.4(6) . . . . yes Cu(1) N(3) C(13) C(12) -166.0(6) . . . . yes Cu(1) N(3) C(13) C(14) 13(1) . . . . yes O(1) C(8) N(2) C(6) -3(1) . . . . yes O(1) C(8) C(9) N(3) -174.4(7) . . . . yes O(1) C(8) C(9) C(10) 5(1) . . . . yes O(2) C(14) N(4) C(15) 14(1) . . . . yes O(2) C(14) C(13) N(3) -129.3(8) . . . . yes O(2) C(14) C(13) C(12) 50(1) . . . . yes N(1) Cu(1) N(2) C(6) -7.1(6) . . . . yes N(1) Cu(1) N(2) C(8) 170.5(7) . . . . yes N(1) Cu(1) N(3) C(9) -18(1) . . . . yes N(1) Cu(1) N(3) C(13) 150.4(7) . . . . yes N(1) C(1) C(2) C(3) 0(1) . . . . yes N(1) C(5) C(4) C(3) -5(1) . . . . yes N(1) C(5) C(6) N(2) -2.4(10) . . . . yes N(1) C(5) C(6) C(7) 119.6(8) . . . . yes N(2) Cu(1) N(1) C(1) 179.9(7) . . . . yes N(2) Cu(1) N(1) C(5) 5.3(6) . . . . yes N(2) Cu(1) N(3) C(9) 4.8(5) . . . . yes N(2) Cu(1) N(3) C(13) 173.9(7) . . . . yes N(2) C(6) C(5) C(4) 174.9(7) . . . . yes N(2) C(8) C(9) N(3) 6.1(10) . . . . yes N(2) C(8) C(9) C(10) -174.3(7) . . . . yes N(3) Cu(1) N(1) C(1) -156.8(7) . . . . yes N(3) Cu(1) N(1) C(5) 28(1) . . . . yes N(3) Cu(1) N(2) C(6) -179.1(6) . . . . yes N(3) Cu(1) N(2) C(8) -1.6(6) . . . . yes N(3) C(9) C(10) C(11) -6(1) . . . . yes N(3) C(13) C(12) C(11) -3(1) . . . . yes N(3) C(13) C(14) N(4) 57.3(10) . . . . yes N(4) C(14) C(13) C(12) -122.7(8) . . . . yes N(4) C(15) C(17) N(5) 161.4(7) . . . . yes N(4) C(15) C(17) C(18) -23(1) . . . . yes N(5) C(17) C(15) C(16) -75.8(9) . . . . yes N(5) C(17) C(18) C(19) -2(1) . . . . yes N(5) C(21) C(20) C(19) 0(1) . . . . yes C(1) N(1) C(5) C(4) 4(1) . . . . yes C(1) N(1) C(5) C(6) -177.8(7) . . . . yes C(1) C(2) C(3) C(4) 0(1) . . . . yes C(2) C(1) N(1) C(5) -1(1) . . . . yes C(2) C(3) C(4) C(5) 3(1) . . . . yes C(3) C(4) C(5) C(6) 177.1(8) . . . . yes C(4) C(5) C(6) C(7) -63.0(10) . . . . yes C(5) C(6) N(2) C(8) -170.4(7) . . . . yes C(6) N(2) C(8) C(9) 175.7(7) . . . . yes C(7) C(6) N(2) C(8) 68.4(10) . . . . yes C(8) C(9) N(3) C(13) -178.0(6) . . . . yes C(8) C(9) C(10) C(11) 174.1(7) . . . . yes C(9) N(3) C(13) C(12) 2(1) . . . . yes C(9) N(3) C(13) C(14) -177.5(7) . . . . yes C(9) C(10) C(11) C(12) 5(1) . . . . yes C(10) C(9) N(3) C(13) 2(1) . . . . yes C(10) C(11) C(12) C(13) 0(1) . . . . yes C(11) C(12) C(13) C(14) 176.8(8) . . . . yes C(13) C(14) N(4) C(15) -172.0(6) . . . . yes C(14) N(4) C(15) C(16) 175.0(7) . . . . yes C(14) N(4) C(15) C(17) -62.7(9) . . . . yes C(15) C(17) N(5) C(21) 177.2(7) . . . . yes C(15) C(17) C(18) C(19) -176.9(8) . . . . yes C(16) C(15) C(17) C(18) 98.9(9) . . . . yes C(17) N(5) C(21) C(20) 0(1) . . . . yes C(17) C(18) C(19) C(20) 1(1) . . . . yes C(18) C(17) N(5) C(21) 2(1) . . . . yes C(18) C(19) C(20) C(21) 0(1) . . . . yes C(18) C(19) C(20) C(21) 0(1) . . . . yes #------------------------------------------------------------------------------ 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 Br(2) Cu(1) 2.715(2) . . ? Br(1) C(21) 3.496(8) . 3_445 ? O(1) N(5) 2.670(8) . 2_555 ? O(1) C(15) 3.17(1) . 2_555 ? O(1) C(16) 3.21(1) . 2_555 ? O(1) C(17) 3.408(10) . 2_555 ? O(1) C(16) 3.57(1) . 4_655 ? O(2) C(4) 3.079(10) . 1_545 ? O(2) C(3) 3.43(1) . 1_545 ? C(2) C(11) 3.49(1) . 4_555 ? C(2) C(21) 3.49(1) . 1_565 ? C(2) C(10) 3.56(1) . 4_555 ? C(3) C(9) 3.35(1) . 4_555 ? C(3) C(10) 3.52(1) . 4_555 ? C(7) C(19) 3.58(1) . 1_565 ? C(9) C(19) 3.52(1) . 4_655 ? C(10) C(19) 3.39(1) . 4_655 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------