Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global #=================================================== _audit_creation_date '15 June 2001' _audit_creation_method SHELXL-97 #=================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Professor Hans-Conrad Zur Loye' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of South Carolina 631 Sumter Street Columbia SC 29208 USA ; _publ_contact_author_phone '803 777 6916' _publ_contact_author_fax '803 777 8508' _publ_contact_author_email zurloye@sc.edu _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' #===================================================================== # 2. AUTHOR LIST loop_ _publ_author_name _publ_author_address 'Zaman, Md. Badruz' ; Department of Chemistry and Biochemistry University of South Carolina Columbia, South Carolina, 29208 USA ; 'Smith, Mark D.' ; Department of Chemistry and Biochemistry University of South Carolina Columbia, South Carolina, 29208 USA ; 'zur Loye, Hans-Conrad' ; Department of Chemistry and Biochemistry University of South Carolina Columbia, South Carolina, 29208 USA ; _publ_section_title ; Two Different One-Dimensional Structural Motifs in the Same Coordination Polymer: A Novel Interpenetration of Infinite Ladders by Infinite Chains ; #===================================================================== # 3. CHEMICAL DATA data_2 _database_code_CSD 167941 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? ; [Cu(dpdaB)(EtOH)(NO3)2][Cu(dpdaB)1.5(NO3)2] 2EtOH ; _chemical_formula_sum 'C56 H48 Cu2 N9 O15' _chemical_formula_weight 1214.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.248(2) _cell_length_b 13.771(3) _cell_length_c 18.257(4) _cell_angle_alpha 108.078(4) _cell_angle_beta 97.890(4) _cell_angle_gamma 103.139(5) _cell_volume 2778.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3039 _cell_measurement_theta_min 2.256 _cell_measurement_theta_max 24.481 _exptl_crystal_description bar _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1250 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 16659 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.2239 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 25.09 _reflns_number_total 9758 _reflns_number_gt 4024 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.619 (Bruker, 2000)' _computing_cell_refinement 'SAINT+ NT V6.02a (Bruker, 1998)' _computing_data_reduction 'SAINT+ NT V6.02a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL V5.1' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [0.00000+1.00000exp(3.50(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0010*P+(0.0207P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9758 _refine_ls_number_parameters 745 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1389 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.0936 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Cu1 Cu 0.39534(7) 0.27529(6) 0.15349(5) 0.0361(2) Uani 1 1 d . . . Cu2 Cu 0.60024(6) 0.71051(5) 0.37328(4) 0.0283(2) Uani 1 1 d . . . C1 C 0.2240(5) 0.3550(5) 0.0838(4) 0.0388(17) Uani 1 1 d . . . H1 H 0.2273 0.3040 0.0374 0.047 Uiso 1 1 calc R . . C2 C 0.1542(5) 0.4194(5) 0.0799(4) 0.0396(17) Uani 1 1 d . . . H2 H 0.1119 0.4118 0.0310 0.047 Uiso 1 1 calc R . . C3 C 0.1462(5) 0.4953(4) 0.1477(4) 0.0286(14) Uani 1 1 d . . . C4 C 0.2093(5) 0.5004(4) 0.2182(4) 0.0330(15) Uani 1 1 d . . . H4 H 0.2051 0.5486 0.2657 0.040 Uiso 1 1 calc R . . C5 C 0.2781(5) 0.4346(4) 0.2183(4) 0.0323(16) Uani 1 1 d . . . H5 H 0.3203 0.4397 0.2665 0.039 Uiso 1 1 calc R . . C6 C 0.0748(5) 0.5637(4) 0.1434(3) 0.0339(16) Uani 1 1 d . . . C7 C 0.0164(5) 0.6199(5) 0.1410(3) 0.0341(16) Uani 1 1 d . . . C8 C -0.0547(5) 0.6896(4) 0.1383(3) 0.0297(15) Uani 1 1 d . . . C9 C -0.1720(5) 0.6539(5) 0.1288(4) 0.0379(17) Uani 1 1 d . . . H9 H -0.2060 0.5841 0.1245 0.046 Uiso 1 1 calc R . . C10 C -0.2397(5) 0.7207(5) 0.1256(4) 0.0381(16) Uani 1 1 d . . . H10 H -0.3191 0.6948 0.1174 0.046 Uiso 1 1 calc R . . C11 C -0.1908(5) 0.8255(4) 0.1343(3) 0.0325(15) Uani 1 1 d . . . C12 C -0.0730(5) 0.8617(5) 0.1450(4) 0.051(2) Uani 1 1 d . . . H12 H -0.0388 0.9322 0.1512 0.061 Uiso 1 1 calc R . . C13 C -0.0057(5) 0.7949(5) 0.1466(4) 0.051(2) Uani 1 1 d . . . H13 H 0.0734 0.8204 0.1533 0.062 Uiso 1 1 calc R . . C14 C -0.2604(5) 0.8959(4) 0.1321(4) 0.0355(16) Uani 1 1 d . . . C15 C -0.3165(5) 0.9547(5) 0.1310(4) 0.0389(17) Uani 1 1 d . . . C16 C -0.5583(5) 1.0662(5) 0.0945(4) 0.0403(17) Uani 1 1 d . . . H16 H -0.6353 1.0420 0.0683 0.048 Uiso 1 1 calc R . . C17 C -0.4981(5) 0.9926(5) 0.0922(4) 0.0392(17) Uani 1 1 d . . . H17 H -0.5341 0.9203 0.0654 0.047 Uiso 1 1 calc R . . C18 C -0.3829(5) 1.0282(5) 0.1305(4) 0.0344(16) Uani 1 1 d . . . C19 C -0.3349(5) 1.1369(5) 0.1687(4) 0.0424(18) Uani 1 1 d . . . H19 H -0.2577 1.1638 0.1947 0.051 Uiso 1 1 calc R . . C20 C -0.3999(5) 1.2048(5) 0.1684(4) 0.0363(16) Uani 1 1 d . . . H20 H -0.3653 1.2775 0.1942 0.044 Uiso 1 1 calc R . . C21 C 0.4945(7) 0.3425(6) 0.3511(4) 0.063(2) Uani 1 1 d . . . H21A H 0.4333 0.2794 0.3438 0.075 Uiso 1 1 calc R . . H21B H 0.4816 0.4022 0.3904 0.075 Uiso 1 1 calc R . . C22 C 0.6061(8) 0.3277(7) 0.3822(5) 0.107(4) Uani 1 1 d . . . H22A H 0.6196 0.2684 0.3440 0.161 Uiso 1 1 calc R . . H22B H 0.6035 0.3143 0.4305 0.161 Uiso 1 1 calc R . . H22C H 0.6672 0.3911 0.3921 0.161 Uiso 1 1 calc R . . C31 C 0.4248(5) 0.7609(4) 0.2788(3) 0.0343(16) Uani 1 1 d . . . H31 H 0.4208 0.8026 0.3288 0.041 Uiso 1 1 calc R . . C32 C 0.3572(5) 0.7657(5) 0.2143(4) 0.0366(16) Uani 1 1 d . . . H32 H 0.3087 0.8093 0.2210 0.044 Uiso 1 1 calc R . . C33 C 0.3620(5) 0.7054(5) 0.1395(4) 0.0329(16) Uani 1 1 d . . . C34 C 0.4332(5) 0.6390(4) 0.1332(3) 0.0321(15) Uani 1 1 d . . . H34 H 0.4371 0.5953 0.0838 0.039 Uiso 1 1 calc R . . C35 C 0.4982(5) 0.6387(4) 0.2014(3) 0.0294(15) Uani 1 1 d . . . H35 H 0.5454 0.5940 0.1965 0.035 Uiso 1 1 calc R . . C36 C 0.2952(5) 0.7114(4) 0.0701(3) 0.0324(15) Uani 1 1 d . . . C37 C 0.2401(5) 0.7219(4) 0.0165(3) 0.0325(15) Uani 1 1 d . . . C38 C 0.1692(5) 0.7262(5) -0.0524(4) 0.0322(15) Uani 1 1 d . . . C39 C 0.1183(5) 0.8069(5) -0.0472(4) 0.0352(16) Uani 1 1 d . . . H39 H 0.1293 0.8602 0.0015 0.042 Uiso 1 1 calc R . . C40 C 0.0510(5) 0.8097(5) -0.1136(4) 0.0369(17) Uani 1 1 d . . . H40 H 0.0172 0.8647 -0.1094 0.044 Uiso 1 1 calc R . . C41 C 0.0339(5) 0.7293(5) -0.1872(4) 0.0325(16) Uani 1 1 d . . . C42 C 0.0855(5) 0.6482(4) -0.1922(3) 0.0294(15) Uani 1 1 d . . . H42 H 0.0744 0.5941 -0.2405 0.035 Uiso 1 1 calc R . . C43 C 0.1534(5) 0.6480(4) -0.1254(4) 0.0321(16) Uani 1 1 d . . . H43 H 0.1891 0.5943 -0.1294 0.039 Uiso 1 1 calc R . . C44 C -0.0374(5) 0.7295(4) -0.2572(3) 0.0297(15) Uani 1 1 d . . . C45 C -0.0935(5) 0.7249(5) -0.3160(4) 0.0367(17) Uani 1 1 d . . . C46 C -0.2130(5) 0.8050(5) -0.4802(4) 0.0457(19) Uani 1 1 d . . . H46 H -0.1979 0.8649 -0.4947 0.055 Uiso 1 1 calc R . . C47 C -0.1456(6) 0.8081(5) -0.4117(4) 0.050(2) Uani 1 1 d . . . H47 H -0.0875 0.8701 -0.3812 0.060 Uiso 1 1 calc R . . C48 C -0.1624(5) 0.7218(5) -0.3877(3) 0.0302(15) Uani 1 1 d . . . C49 C -0.2484(5) 0.6315(5) -0.4379(4) 0.0403(17) Uani 1 1 d . . . H49 H -0.2617 0.5691 -0.4265 0.048 Uiso 1 1 calc R . . C50 C -0.3137(5) 0.6343(4) -0.5041(3) 0.0369(17) Uani 1 1 d . . . H50 H -0.3721 0.5732 -0.5358 0.044 Uiso 1 1 calc R . . C51 C 0.6466(5) 0.9450(4) 0.4392(4) 0.0362(16) Uani 1 1 d . . . H51 H 0.5929 0.9285 0.4681 0.043 Uiso 1 1 calc R . . C52 C 0.6954(5) 1.0506(5) 0.4515(4) 0.0393(17) Uani 1 1 d . . . H52 H 0.6745 1.1035 0.4876 0.047 Uiso 1 1 calc R . . C53 C 0.7755(6) 1.0772(4) 0.4100(4) 0.0363(16) Uani 1 1 d . . . C54 C 0.8004(6) 0.9958(5) 0.3549(4) 0.0496(19) Uani 1 1 d . . . H54 H 0.8525 1.0102 0.3245 0.060 Uiso 1 1 calc R . . C55 C 0.7451(6) 0.8917(5) 0.3463(4) 0.0439(18) Uani 1 1 d . . . H55 H 0.7608 0.8369 0.3084 0.053 Uiso 1 1 calc R . . C56 C 0.8350(6) 1.1873(5) 0.4265(4) 0.0409(17) Uani 1 1 d . . . C57 C 0.8842(6) 1.2804(5) 0.4465(4) 0.0421(17) Uani 1 1 d . . . C58 C 0.9435(5) 1.3921(4) 0.4734(4) 0.0367(16) Uani 1 1 d . . . C59 C 1.0155(6) 1.4406(5) 0.5468(4) 0.050(2) Uani 1 1 d . . . H59 H 1.0265 1.4011 0.5789 0.061 Uiso 1 1 calc R . . C60 C 1.0727(6) 1.5496(5) 0.5735(4) 0.053(2) Uani 1 1 d . . . H60 H 1.1219 1.5825 0.6233 0.064 Uiso 1 1 calc R . . C1S C 0.3707(9) 0.0407(7) 0.3438(6) 0.108(4) Uani 1 1 d . . . H1S1 H 0.3708 0.1101 0.3788 0.129 Uiso 1 1 calc R . . H1S2 H 0.3842 -0.0026 0.3751 0.129 Uiso 1 1 calc R . . C2S C 0.4575(9) 0.0512(7) 0.2971(7) 0.128(4) Uani 1 1 d . . . H2S1 H 0.4596 -0.0183 0.2657 0.193 Uiso 1 1 calc R . . H2S2 H 0.5314 0.0903 0.3318 0.193 Uiso 1 1 calc R . . H2S3 H 0.4384 0.0887 0.2630 0.193 Uiso 1 1 calc R . . C3S C 0.9588(7) 0.1589(6) 0.6316(5) 0.075(3) Uani 1 1 d . . . H3S1 H 0.9938 0.1665 0.5884 0.090 Uiso 1 1 calc R . . H3S2 H 1.0202 0.1743 0.6769 0.090 Uiso 1 1 calc R . . C4S C 0.8920(7) 0.2372(6) 0.6518(5) 0.086(3) Uani 1 1 d . . . H4S1 H 0.8378 0.2283 0.6052 0.130 Uiso 1 1 calc R . . H4S2 H 0.9434 0.3081 0.6720 0.130 Uiso 1 1 calc R . . H4S3 H 0.8514 0.2256 0.6911 0.130 Uiso 1 1 calc R . . N1 N 0.2867(4) 0.3634(4) 0.1519(3) 0.0312(12) Uani 1 1 d . . . N2 N -0.5104(4) 1.1719(4) 0.1332(3) 0.0339(13) Uani 1 1 d . . . N3 N 0.4964(4) 0.6994(3) 0.2739(3) 0.0278(12) Uani 1 1 d . . . N4 N -0.2983(4) 0.7200(4) -0.5259(3) 0.0289(12) Uani 1 1 d . . . N5 N 0.6717(4) 0.8653(4) 0.3885(3) 0.0306(12) Uani 1 1 d . . . N11 N 0.5180(4) 0.3814(4) 0.0700(3) 0.0360(13) Uani 1 1 d . . . N12 N 0.2086(6) 0.1086(6) 0.1390(6) 0.077(3) Uani 1 1 d . . . N13 N 0.7310(5) 0.5732(4) 0.3024(3) 0.0401(14) Uani 1 1 d . . . N14 N 0.3955(5) 0.6662(4) 0.4248(3) 0.0390(13) Uani 1 1 d . . . O1 O 0.5174(3) 0.3883(3) 0.1422(2) 0.0366(11) Uani 1 1 d . . . O2 O 0.4494(4) 0.3035(3) 0.0166(3) 0.0548(14) Uani 1 1 d . . . O3 O 0.5857(4) 0.4534(4) 0.0596(3) 0.0537(13) Uani 1 1 d . . . O4 O 0.2912(4) 0.1775(4) 0.1930(3) 0.0652(16) Uani 1 1 d . . . O5 O 0.1962(5) 0.1136(5) 0.0712(4) 0.086(2) Uani 1 1 d . . . O6 O 0.1447(5) 0.0380(4) 0.1526(5) 0.124(3) Uani 1 1 d . . . O7 O 0.6287(3) 0.5618(3) 0.3171(2) 0.0317(10) Uani 1 1 d . . . O8 O 0.7886(4) 0.6631(4) 0.3117(3) 0.0625(15) Uani 1 1 d . . . O9 O 0.7645(4) 0.4935(4) 0.2804(3) 0.0542(14) Uani 1 1 d . . . O10 O 0.4527(4) 0.6056(3) 0.3924(2) 0.0417(12) Uani 1 1 d . . . O11 O 0.4416(4) 0.7642(3) 0.4517(3) 0.0521(13) Uani 1 1 d . . . O12 O 0.2955(4) 0.6259(4) 0.4253(3) 0.0636(15) Uani 1 1 d . . . O1E O 0.4875(4) 0.3608(3) 0.2797(3) 0.0412(12) Uani 1 1 d D . . H1E H 0.537(4) 0.421(3) 0.292(4) 0.062 Uiso 1 1 d D . . O1S O 0.2544(5) -0.0149(4) 0.2807(4) 0.114(2) Uani 1 1 d . . . H1S H 0.2012 -0.0234 0.3030 0.172 Uiso 1 1 calc R . . O2S O 0.8920(5) 0.0559(4) 0.6102(4) 0.110(2) Uani 1 1 d . . . H2S H 0.8535 0.0515 0.6431 0.165 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0318(5) 0.0275(4) 0.0521(6) 0.0138(4) 0.0095(4) 0.0146(4) Cu2 0.0332(5) 0.0223(4) 0.0257(4) 0.0097(3) -0.0053(3) 0.0066(3) C1 0.038(4) 0.031(3) 0.043(4) 0.004(3) 0.000(3) 0.018(3) C2 0.036(4) 0.044(4) 0.042(4) 0.014(3) 0.003(3) 0.022(3) C3 0.022(3) 0.022(3) 0.044(4) 0.013(3) 0.009(3) 0.007(3) C4 0.029(4) 0.031(3) 0.037(4) 0.007(3) 0.005(3) 0.013(3) C5 0.027(4) 0.033(3) 0.035(4) 0.011(3) 0.000(3) 0.012(3) C6 0.032(4) 0.029(3) 0.040(4) 0.012(3) 0.006(3) 0.010(3) C7 0.038(4) 0.032(3) 0.037(4) 0.016(3) 0.010(3) 0.014(3) C8 0.029(4) 0.029(3) 0.031(4) 0.009(3) 0.001(3) 0.014(3) C9 0.028(4) 0.032(3) 0.059(5) 0.022(3) 0.009(3) 0.012(3) C10 0.030(4) 0.040(4) 0.051(4) 0.021(3) 0.009(3) 0.016(3) C11 0.039(4) 0.024(3) 0.039(4) 0.009(3) 0.010(3) 0.019(3) C12 0.029(4) 0.031(4) 0.091(6) 0.025(4) 0.007(4) 0.009(3) C13 0.020(4) 0.037(4) 0.100(6) 0.028(4) 0.011(4) 0.011(3) C14 0.034(4) 0.030(3) 0.047(4) 0.014(3) 0.008(3) 0.016(3) C15 0.034(4) 0.035(4) 0.055(5) 0.021(3) 0.013(3) 0.016(3) C16 0.030(4) 0.040(4) 0.049(5) 0.012(3) 0.003(3) 0.015(3) C17 0.044(4) 0.026(3) 0.045(4) 0.005(3) 0.007(3) 0.017(3) C18 0.034(4) 0.032(4) 0.043(4) 0.015(3) 0.012(3) 0.016(3) C19 0.022(4) 0.035(4) 0.073(5) 0.019(4) 0.009(3) 0.015(3) C20 0.031(4) 0.024(3) 0.053(5) 0.010(3) 0.013(3) 0.010(3) C21 0.076(6) 0.042(4) 0.068(6) 0.020(4) 0.024(5) 0.010(4) C22 0.140(10) 0.124(8) 0.075(7) 0.055(6) -0.003(7) 0.060(8) C31 0.037(4) 0.030(3) 0.031(4) 0.004(3) -0.002(3) 0.015(3) C32 0.037(4) 0.037(4) 0.037(4) 0.011(3) 0.002(3) 0.020(3) C33 0.022(4) 0.037(4) 0.040(4) 0.020(3) -0.003(3) 0.006(3) C34 0.030(4) 0.040(4) 0.021(3) 0.011(3) -0.005(3) 0.006(3) C35 0.023(4) 0.034(3) 0.032(4) 0.013(3) 0.004(3) 0.011(3) C36 0.032(4) 0.036(4) 0.032(4) 0.017(3) 0.004(3) 0.010(3) C37 0.030(4) 0.036(4) 0.032(4) 0.014(3) 0.003(3) 0.010(3) C38 0.023(4) 0.039(4) 0.035(4) 0.019(3) -0.004(3) 0.008(3) C39 0.031(4) 0.040(4) 0.033(4) 0.010(3) 0.002(3) 0.012(3) C40 0.035(4) 0.046(4) 0.041(4) 0.022(3) 0.007(3) 0.023(3) C41 0.020(3) 0.046(4) 0.036(4) 0.025(3) -0.002(3) 0.007(3) C42 0.029(4) 0.031(3) 0.024(3) 0.011(3) -0.001(3) 0.003(3) C43 0.025(4) 0.031(3) 0.044(4) 0.019(3) 0.002(3) 0.011(3) C44 0.018(3) 0.035(3) 0.036(4) 0.013(3) -0.001(3) 0.010(3) C45 0.036(4) 0.039(4) 0.040(4) 0.016(3) 0.004(3) 0.019(3) C46 0.047(4) 0.033(4) 0.048(5) 0.018(3) -0.013(4) 0.004(3) C47 0.049(5) 0.039(4) 0.045(5) 0.011(3) -0.019(4) 0.004(3) C48 0.025(4) 0.042(4) 0.033(4) 0.020(3) 0.006(3) 0.017(3) C49 0.044(4) 0.042(4) 0.044(4) 0.026(3) 0.002(3) 0.018(3) C50 0.040(4) 0.030(3) 0.036(4) 0.012(3) -0.004(3) 0.007(3) C51 0.037(4) 0.032(4) 0.036(4) 0.011(3) 0.005(3) 0.006(3) C52 0.040(4) 0.024(3) 0.048(5) 0.007(3) 0.006(3) 0.009(3) C53 0.044(4) 0.021(3) 0.037(4) 0.007(3) 0.004(3) 0.002(3) C54 0.064(5) 0.034(4) 0.051(5) 0.016(4) 0.025(4) 0.005(4) C55 0.056(5) 0.023(3) 0.043(5) 0.000(3) 0.008(4) 0.009(3) C56 0.048(4) 0.030(4) 0.045(4) 0.013(3) 0.013(3) 0.009(3) C57 0.048(4) 0.030(4) 0.048(5) 0.014(3) 0.013(3) 0.010(3) C58 0.041(4) 0.020(3) 0.045(4) 0.011(3) 0.010(3) 0.002(3) C59 0.065(5) 0.036(4) 0.053(5) 0.025(4) 0.006(4) 0.011(4) C60 0.067(5) 0.030(4) 0.049(5) 0.010(3) 0.002(4) 0.001(4) C1S 0.109(9) 0.068(7) 0.130(10) 0.010(6) 0.075(8) 0.003(6) C2S 0.159(12) 0.081(7) 0.174(13) 0.066(8) 0.073(10) 0.040(7) C3S 0.082(7) 0.052(5) 0.085(7) 0.022(5) 0.019(5) 0.010(5) C4S 0.104(8) 0.072(6) 0.080(7) 0.018(5) 0.019(6) 0.032(6) N1 0.027(3) 0.028(3) 0.037(3) 0.009(2) 0.002(2) 0.010(2) N2 0.026(3) 0.029(3) 0.048(4) 0.012(3) 0.008(3) 0.011(2) N3 0.030(3) 0.022(3) 0.032(3) 0.009(2) 0.005(2) 0.011(2) N4 0.026(3) 0.030(3) 0.029(3) 0.010(2) -0.001(2) 0.010(2) N5 0.036(3) 0.028(3) 0.028(3) 0.013(2) 0.002(2) 0.009(2) N11 0.033(3) 0.034(3) 0.040(4) 0.012(3) 0.006(3) 0.011(3) N12 0.030(4) 0.047(5) 0.154(9) 0.030(6) 0.025(5) 0.016(4) N13 0.046(4) 0.036(3) 0.036(4) 0.011(3) 0.000(3) 0.016(3) N14 0.034(4) 0.045(4) 0.040(4) 0.017(3) 0.009(3) 0.010(3) O1 0.042(3) 0.028(2) 0.037(3) 0.009(2) 0.004(2) 0.010(2) O2 0.048(3) 0.048(3) 0.047(3) 0.004(2) -0.004(2) -0.002(2) O3 0.058(3) 0.046(3) 0.054(3) 0.021(3) 0.018(3) 0.001(3) O4 0.040(3) 0.046(3) 0.113(5) 0.026(3) 0.027(3) 0.017(3) O5 0.051(4) 0.058(4) 0.135(6) 0.017(4) 0.003(4) 0.025(3) O6 0.057(4) 0.055(4) 0.268(10) 0.068(5) 0.060(5) 0.003(3) O7 0.030(3) 0.029(2) 0.031(3) 0.0056(19) 0.000(2) 0.011(2) O8 0.069(4) 0.034(3) 0.083(4) 0.018(3) 0.034(3) 0.007(3) O9 0.062(3) 0.050(3) 0.053(3) 0.007(2) 0.011(3) 0.037(3) O10 0.048(3) 0.040(3) 0.036(3) 0.010(2) 0.004(2) 0.019(2) O11 0.070(4) 0.032(3) 0.046(3) 0.011(2) 0.008(3) 0.005(2) O12 0.040(3) 0.075(4) 0.077(4) 0.028(3) 0.017(3) 0.012(3) O1E 0.044(3) 0.035(3) 0.045(3) 0.016(2) 0.005(2) 0.013(2) O1S 0.089(5) 0.068(4) 0.171(7) 0.021(4) 0.046(5) 0.014(4) O2S 0.121(6) 0.063(4) 0.138(6) 0.027(4) 0.049(5) 0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.981(4) . ? Cu1 N1 1.997(4) . ? Cu1 N2 2.009(5) 1_645 ? Cu1 O4 2.010(5) . ? Cu1 O1E 2.229(4) . ? Cu2 N3 2.009(4) . ? Cu2 N4 2.023(4) 1_656 ? Cu2 N5 2.026(5) . ? Cu2 O7 2.118(4) . ? Cu2 O10 2.185(5) . ? C1 N1 1.325(7) . ? C1 C2 1.375(7) . ? C2 C3 1.383(8) . ? C3 C4 1.380(7) . ? C3 C6 1.436(7) . ? C4 C5 1.371(7) . ? C5 N1 1.337(7) . ? C6 C7 1.173(7) . ? C7 C8 1.442(7) . ? C8 C9 1.377(8) . ? C8 C13 1.388(8) . ? C9 C10 1.380(7) . ? C10 C11 1.380(8) . ? C11 C12 1.380(8) . ? C11 C14 1.435(7) . ? C12 C13 1.372(8) . ? C14 C15 1.177(7) . ? C15 C18 1.436(7) . ? C16 N2 1.350(7) . ? C16 C17 1.376(7) . ? C17 C18 1.386(8) . ? C18 C19 1.384(8) . ? C19 C20 1.359(7) . ? C20 N2 1.323(7) . ? C21 O1E 1.397(8) . ? C21 C22 1.489(9) . ? C31 N3 1.344(6) . ? C31 C32 1.372(7) . ? C32 C33 1.378(8) . ? C33 C34 1.392(7) . ? C33 C36 1.447(7) . ? C34 C35 1.385(7) . ? C35 N3 1.334(7) . ? C36 C37 1.176(7) . ? C37 C38 1.452(7) . ? C38 C39 1.379(7) . ? C38 C43 1.384(8) . ? C39 C40 1.386(7) . ? C40 C41 1.403(8) . ? C41 C42 1.390(7) . ? C41 C44 1.446(7) . ? C42 C43 1.380(7) . ? C44 C45 1.168(7) . ? C45 C48 1.441(7) . ? C46 N4 1.325(6) . ? C46 C47 1.384(7) . ? C47 C48 1.371(8) . ? C48 C49 1.388(7) . ? C49 C50 1.372(7) . ? C50 N4 1.341(6) . ? C51 N5 1.326(7) . ? C51 C52 1.374(7) . ? C52 C53 1.373(9) . ? C53 C54 1.378(8) . ? C53 C56 1.440(8) . ? C54 C55 1.389(8) . ? C55 N5 1.322(8) . ? C56 C57 1.200(8) . ? C57 C58 1.434(8) . ? C58 C60 1.367(8) 2_786 ? C58 C59 1.369(8) . ? C59 C60 1.399(8) . ? C60 C58 1.367(8) 2_786 ? C1S C2S 1.461(12) . ? C1S O1S 1.565(11) . ? C3S O2S 1.369(8) . ? C3S C4S 1.486(9) . ? N2 Cu1 2.009(5) 1_465 ? N4 Cu2 2.023(4) 1_454 ? N11 O3 1.222(6) . ? N11 O2 1.234(6) . ? N11 O1 1.294(6) . ? N12 O6 1.215(8) . ? N12 O5 1.251(9) . ? N12 O4 1.267(8) . ? N13 O8 1.224(6) . ? N13 O9 1.229(6) . ? N13 O7 1.303(6) . ? N14 O12 1.227(6) . ? N14 O11 1.244(6) . ? N14 O10 1.269(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N1 89.69(18) . . ? O1 Cu1 N2 91.99(18) . 1_645 ? N1 Cu1 N2 169.0(2) . 1_645 ? O1 Cu1 O4 165.9(2) . . ? N1 Cu1 O4 92.42(19) . . ? N2 Cu1 O4 88.58(19) 1_645 . ? O1 Cu1 O1E 80.00(17) . . ? N1 Cu1 O1E 96.78(18) . . ? N2 Cu1 O1E 94.19(18) 1_645 . ? O4 Cu1 O1E 86.0(2) . . ? N3 Cu2 N4 178.7(2) . 1_656 ? N3 Cu2 N5 87.45(17) . . ? N4 Cu2 N5 93.44(18) 1_656 . ? N3 Cu2 O7 91.91(16) . . ? N4 Cu2 O7 88.09(16) 1_656 . ? N5 Cu2 O7 137.1(2) . . ? N3 Cu2 O10 87.11(17) . . ? N4 Cu2 O10 91.60(17) 1_656 . ? N5 Cu2 O10 141.83(19) . . ? O7 Cu2 O10 80.87(17) . . ? N1 C1 C2 121.9(6) . . ? C1 C2 C3 120.7(6) . . ? C4 C3 C2 116.5(5) . . ? C4 C3 C6 122.8(6) . . ? C2 C3 C6 120.7(5) . . ? C5 C4 C3 120.1(6) . . ? N1 C5 C4 122.5(5) . . ? C7 C6 C3 179.1(7) . . ? C6 C7 C8 179.6(8) . . ? C9 C8 C13 118.6(5) . . ? C9 C8 C7 120.8(5) . . ? C13 C8 C7 120.6(5) . . ? C8 C9 C10 120.6(5) . . ? C11 C10 C9 120.7(6) . . ? C12 C11 C10 118.7(5) . . ? C12 C11 C14 120.3(5) . . ? C10 C11 C14 121.1(6) . . ? C13 C12 C11 120.8(6) . . ? C12 C13 C8 120.7(6) . . ? C15 C14 C11 179.2(7) . . ? C14 C15 C18 178.8(7) . . ? N2 C16 C17 122.9(6) . . ? C16 C17 C18 118.9(5) . . ? C19 C18 C17 117.4(5) . . ? C19 C18 C15 121.4(5) . . ? C17 C18 C15 121.2(5) . . ? C20 C19 C18 120.3(6) . . ? N2 C20 C19 123.0(5) . . ? O1E C21 C22 114.6(7) . . ? N3 C31 C32 123.8(6) . . ? C31 C32 C33 119.4(6) . . ? C32 C33 C34 117.7(5) . . ? C32 C33 C36 120.9(6) . . ? C34 C33 C36 121.4(6) . . ? C35 C34 C33 119.1(6) . . ? N3 C35 C34 123.3(6) . . ? C37 C36 C33 176.0(7) . . ? C36 C37 C38 175.7(6) . . ? C39 C38 C43 119.0(5) . . ? C39 C38 C37 121.7(6) . . ? C43 C38 C37 119.3(5) . . ? C38 C39 C40 120.9(6) . . ? C39 C40 C41 119.8(6) . . ? C42 C41 C40 119.1(5) . . ? C42 C41 C44 120.0(6) . . ? C40 C41 C44 120.9(5) . . ? C43 C42 C41 120.0(6) . . ? C42 C43 C38 121.2(5) . . ? C45 C44 C41 176.4(7) . . ? C44 C45 C48 178.7(7) . . ? N4 C46 C47 122.7(6) . . ? C48 C47 C46 121.5(6) . . ? C47 C48 C49 115.5(5) . . ? C47 C48 C45 121.8(6) . . ? C49 C48 C45 122.7(5) . . ? C50 C49 C48 120.1(5) . . ? N4 C50 C49 123.8(5) . . ? N5 C51 C52 123.7(6) . . ? C53 C52 C51 119.3(6) . . ? C52 C53 C54 118.2(6) . . ? C52 C53 C56 120.4(6) . . ? C54 C53 C56 121.4(6) . . ? C53 C54 C55 118.0(7) . . ? N5 C55 C54 124.4(6) . . ? C57 C56 C53 174.8(7) . . ? C56 C57 C58 177.9(7) . . ? C60 C58 C59 119.9(5) 2_786 . ? C60 C58 C57 120.4(6) 2_786 . ? C59 C58 C57 119.7(6) . . ? C58 C59 C60 119.8(6) . . ? C58 C60 C59 120.3(6) 2_786 . ? C2S C1S O1S 104.2(9) . . ? O2S C3S C4S 112.4(7) . . ? C1 N1 C5 118.3(5) . . ? C1 N1 Cu1 120.2(4) . . ? C5 N1 Cu1 121.5(4) . . ? C20 N2 C16 117.5(5) . . ? C20 N2 Cu1 119.3(4) . 1_465 ? C16 N2 Cu1 122.4(4) . 1_465 ? C35 N3 C31 116.7(5) . . ? C35 N3 Cu2 124.1(4) . . ? C31 N3 Cu2 119.1(4) . . ? C46 N4 C50 116.3(5) . . ? C46 N4 Cu2 124.5(4) . 1_454 ? C50 N4 Cu2 119.1(4) . 1_454 ? C55 N5 C51 116.4(5) . . ? C55 N5 Cu2 120.9(4) . . ? C51 N5 Cu2 122.7(5) . . ? O3 N11 O2 124.8(6) . . ? O3 N11 O1 117.4(5) . . ? O2 N11 O1 117.8(5) . . ? O6 N12 O5 121.0(9) . . ? O6 N12 O4 120.5(10) . . ? O5 N12 O4 118.4(8) . . ? O8 N13 O9 123.7(6) . . ? O8 N13 O7 117.9(5) . . ? O9 N13 O7 118.3(5) . . ? O12 N14 O11 122.8(6) . . ? O12 N14 O10 118.6(6) . . ? O11 N14 O10 118.6(6) . . ? N11 O1 Cu1 114.6(3) . . ? N12 O4 Cu1 113.1(6) . . ? N13 O7 Cu2 111.9(3) . . ? N14 O10 Cu2 105.4(4) . . ? C21 O1E Cu1 138.1(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1E H1E O7 0.850(5) 1.886(12) 2.729(6) 171(6) . O1S H1S O2S 0.82 2.17 2.952(9) 159.3 2_656 O2S H2S O1S 0.82 2.14 2.952(9) 171.5 2_656 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.394 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.070 #===END data_3 _database_code_CSD 167942 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; [Cu(dpdaB)(MeOH)(NO3)2][Cu(dpdaB)1.5(NO3)2] 2(EtOH) ; _chemical_formula_sum 'C53 H42 Cu2 N9 O15' _chemical_formula_weight 1172.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1363(18) _cell_length_b 13.738(2) _cell_length_c 17.563(3) _cell_angle_alpha 107.663(3) _cell_angle_beta 94.805(4) _cell_angle_gamma 104.021(4) _cell_volume 2667.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2484 _cell_measurement_theta_min 2.459 _cell_measurement_theta_max 22.633 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1202 _exptl_absorpt_coefficient_mu 0.874 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 14780 _diffrn_reflns_av_R_equivalents 0.0846 _diffrn_reflns_av_sigmaI/netI 0.2154 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 23.30 _reflns_number_total 7669 _reflns_number_gt 3403 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.619 (Bruker, 2000)' _computing_cell_refinement 'SAINT+ NT V6.02a (Bruker, 1998)' _computing_data_reduction 'SAINT+ NT V6.02a' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V5.1 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL V5.1' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [0.00000+1.00000exp(4.70(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0119P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7669 _refine_ls_number_parameters 719 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1232 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1125 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2322(6) 0.3441(6) 0.0993(4) 0.0386(19) Uani 1 1 d . . . H1 H 0.2343 0.2885 0.0519 0.046 Uiso 1 1 calc R . . C2 C 0.1604(5) 0.4071(6) 0.0935(4) 0.0381(19) Uani 1 1 d . . . H2 H 0.1137 0.3939 0.0432 0.046 Uiso 1 1 calc R . . C3 C 0.1574(5) 0.4891(5) 0.1614(4) 0.0301(17) Uani 1 1 d . . . C4 C 0.2235(5) 0.5012(5) 0.2341(4) 0.0363(18) Uani 1 1 d . . . H4 H 0.2209 0.5547 0.2826 0.044 Uiso 1 1 calc R . . C5 C 0.2934(5) 0.4348(5) 0.2355(4) 0.0330(18) Uani 1 1 d . . . H5 H 0.3386 0.4441 0.2854 0.040 Uiso 1 1 calc R . . C6 C 0.0846(6) 0.5579(6) 0.1572(4) 0.041(2) Uani 1 1 d . . . C7 C 0.0251(6) 0.6118(5) 0.1505(4) 0.0366(18) Uani 1 1 d . . . C8 C -0.0466(6) 0.6796(6) 0.1431(4) 0.0339(18) Uani 1 1 d . . . C9 C -0.1653(6) 0.6366(5) 0.1195(4) 0.0375(18) Uani 1 1 d . . . H9 H -0.1988 0.5625 0.1075 0.045 Uiso 1 1 calc R . . C10 C -0.2344(5) 0.7005(5) 0.1133(4) 0.0327(17) Uani 1 1 d . . . H10 H -0.3151 0.6701 0.0956 0.039 Uiso 1 1 calc R . . C11 C -0.1866(6) 0.8092(5) 0.1327(4) 0.0308(17) Uani 1 1 d . . . C12 C -0.0681(6) 0.8522(6) 0.1560(4) 0.044(2) Uani 1 1 d . . . H12 H -0.0344 0.9264 0.1681 0.053 Uiso 1 1 calc R . . C13 C 0.0008(6) 0.7869(6) 0.1614(4) 0.042(2) Uani 1 1 d . . . H13 H 0.0818 0.8168 0.1779 0.051 Uiso 1 1 calc R . . C14 C -0.2564(6) 0.8796(6) 0.1307(4) 0.0357(18) Uani 1 1 d . . . C15 C -0.3115(6) 0.9400(5) 0.1328(4) 0.0362(18) Uani 1 1 d . . . C16 C -0.5474(6) 1.0618(5) 0.1054(4) 0.0383(19) Uani 1 1 d . . . H16 H -0.6247 1.0400 0.0780 0.046 Uiso 1 1 calc R . . C17 C -0.4897(6) 0.9854(6) 0.0976(4) 0.0402(19) Uani 1 1 d . . . H17 H -0.5257 0.9135 0.0648 0.048 Uiso 1 1 calc R . . C18 C -0.3770(6) 1.0162(5) 0.1392(4) 0.0329(18) Uani 1 1 d . . . C19 C -0.3282(6) 1.1236(6) 0.1823(4) 0.042(2) Uani 1 1 d . . . H19 H -0.2505 1.1482 0.2094 0.050 Uiso 1 1 calc R . . C20 C -0.3915(5) 1.1936(6) 0.1859(4) 0.0391(19) Uani 1 1 d . . . H20 H -0.3557 1.2666 0.2161 0.047 Uiso 1 1 calc R . . C31 C 0.4291(6) 0.7632(5) 0.2874(4) 0.0355(18) Uani 1 1 d . . . H31 H 0.4254 0.8068 0.3401 0.043 Uiso 1 1 calc R . . C32 C 0.3639(5) 0.7682(5) 0.2225(4) 0.0341(18) Uani 1 1 d . . . H32 H 0.3150 0.8136 0.2311 0.041 Uiso 1 1 calc R . . C33 C 0.3679(5) 0.7077(5) 0.1442(4) 0.0301(17) Uani 1 1 d . . . C34 C 0.4385(5) 0.6407(5) 0.1359(4) 0.0314(18) Uani 1 1 d . . . H34 H 0.4439 0.5971 0.0836 0.038 Uiso 1 1 calc R . . C35 C 0.5015(5) 0.6380(5) 0.2049(3) 0.0267(16) Uani 1 1 d . . . H35 H 0.5483 0.5907 0.1982 0.032 Uiso 1 1 calc R . . C36 C 0.3027(6) 0.7161(5) 0.0760(4) 0.0344(18) Uani 1 1 d . . . C37 C 0.2472(6) 0.7292(6) 0.0228(4) 0.0368(18) Uani 1 1 d . . . C38 C 0.1790(5) 0.7380(5) -0.0449(4) 0.0308(17) Uani 1 1 d . . . C39 C 0.1257(5) 0.8190(6) -0.0345(4) 0.0390(19) Uani 1 1 d . . . H39 H 0.1357 0.8711 0.0175 0.047 Uiso 1 1 calc R . . C40 C 0.0579(6) 0.8233(6) -0.1004(4) 0.0367(18) Uani 1 1 d . . . H40 H 0.0227 0.8793 -0.0938 0.044 Uiso 1 1 calc R . . C41 C 0.0413(5) 0.7457(6) -0.1761(4) 0.0308(17) Uani 1 1 d . . . C42 C 0.0937(5) 0.6654(5) -0.1857(4) 0.0296(17) Uani 1 1 d . . . H42 H 0.0819 0.6123 -0.2374 0.036 Uiso 1 1 calc R . . C43 C 0.1635(5) 0.6611(5) -0.1208(4) 0.0310(17) Uani 1 1 d . . . H43 H 0.2004 0.6061 -0.1281 0.037 Uiso 1 1 calc R . . C44 C -0.0309(5) 0.7468(6) -0.2450(4) 0.0334(18) Uani 1 1 d . . . C45 C -0.0899(6) 0.7407(6) -0.3046(4) 0.0344(18) Uani 1 1 d . . . C46 C -0.2180(7) 0.8140(6) -0.4712(4) 0.066(3) Uani 1 1 d . . . H46 H -0.2093 0.8759 -0.4863 0.080 Uiso 1 1 calc R . . C47 C -0.1501(7) 0.8221(6) -0.4018(4) 0.062(3) Uani 1 1 d . . . H47 H -0.0962 0.8881 -0.3704 0.074 Uiso 1 1 calc R . . C48 C -0.1603(6) 0.7346(6) -0.3780(4) 0.0344(18) Uani 1 1 d . . . C49 C -0.2377(6) 0.6417(6) -0.4265(4) 0.045(2) Uani 1 1 d . . . H49 H -0.2468 0.5785 -0.4133 0.054 Uiso 1 1 calc R . . C50 C -0.3029(6) 0.6412(6) -0.4954(4) 0.043(2) Uani 1 1 d . . . H50 H -0.3568 0.5759 -0.5283 0.051 Uiso 1 1 calc R . . C51 C 0.6438(6) 0.9450(5) 0.4387(4) 0.0402(19) Uani 1 1 d . . . H51 H 0.5877 0.9278 0.4707 0.048 Uiso 1 1 calc R . . C52 C 0.6895(6) 1.0507(6) 0.4469(4) 0.047(2) Uani 1 1 d . . . H52 H 0.6634 1.1044 0.4824 0.056 Uiso 1 1 calc R . . C53 C 0.7745(6) 1.0776(6) 0.4022(4) 0.0398(19) Uani 1 1 d . . . C54 C 0.8024(7) 0.9952(6) 0.3481(4) 0.052(2) Uani 1 1 d . . . H54 H 0.8562 1.0100 0.3139 0.062 Uiso 1 1 calc R . . C55 C 0.7527(6) 0.8906(5) 0.3428(4) 0.0369(18) Uani 1 1 d . . . H55 H 0.7748 0.8349 0.3060 0.044 Uiso 1 1 calc R . . C56 C 0.8338(6) 1.1879(6) 0.4174(4) 0.043(2) Uani 1 1 d . . . C57 C 0.8820(7) 1.2799(6) 0.4401(4) 0.046(2) Uani 1 1 d . . . C58 C 0.9423(6) 1.3919(5) 0.4695(4) 0.0406(19) Uani 1 1 d . . . C59 C 0.9195(7) 1.4604(6) 0.4312(5) 0.055(2) Uani 1 1 d . . . H59 H 0.8637 1.4331 0.3830 0.065 Uiso 1 1 calc R . . C60 C 0.9752(7) 1.5669(6) 0.4610(4) 0.054(2) Uani 1 1 d . . . H60 H 0.9573 1.6127 0.4338 0.04(2) Uiso 1 1 calc R . . C1M C 0.5262(8) 0.3346(7) 0.3688(5) 0.075(3) Uani 1 1 d . . . H1M1 H 0.4810 0.2615 0.3604 0.112 Uiso 1 1 calc R . . H1M2 H 0.5076 0.3834 0.4162 0.112 Uiso 1 1 calc R . . H1M3 H 0.6085 0.3399 0.3779 0.112 Uiso 1 1 calc R . . Cu1 Cu 0.40657(7) 0.26992(7) 0.17135(5) 0.0309(2) Uani 1 1 d . . . Cu2 Cu 0.60363(7) 0.71216(7) 0.37973(5) 0.0295(2) Uani 1 1 d . . . N1 N 0.2987(4) 0.3583(4) 0.1686(3) 0.0283(13) Uani 1 1 d . . . N2 N -0.5012(4) 1.1657(4) 0.1495(3) 0.0319(14) Uani 1 1 d . . . N3 N 0.4993(4) 0.6985(4) 0.2799(3) 0.0257(13) Uani 1 1 d . . . N4 N -0.2951(5) 0.7251(4) -0.5185(3) 0.0336(15) Uani 1 1 d . . . N5 N 0.6744(5) 0.8665(4) 0.3884(3) 0.0304(14) Uani 1 1 d . . . N11 N 0.5219(5) 0.3752(5) 0.0760(3) 0.0332(14) Uani 1 1 d . . . N12 N 0.2179(6) 0.1061(5) 0.1640(5) 0.054(2) Uani 1 1 d . . . N13 N 0.7359(6) 0.5732(6) 0.3051(3) 0.0414(17) Uani 1 1 d . . . N14 N 0.4015(5) 0.6666(5) 0.4430(3) 0.0385(15) Uani 1 1 d . . . O1 O 0.5295(4) 0.3789(3) 0.1509(2) 0.0311(11) Uani 1 1 d . . . O2 O 0.4524(4) 0.2978(4) 0.0240(3) 0.0471(14) Uani 1 1 d . . . O3 O 0.5847(4) 0.4496(4) 0.0612(3) 0.0475(14) Uani 1 1 d . . . O4 O 0.3012(4) 0.1755(4) 0.2174(3) 0.0454(14) Uani 1 1 d . . . O5 O 0.2058(5) 0.1089(5) 0.0941(4) 0.0679(19) Uani 1 1 d . . . O6 O 0.1533(5) 0.0382(5) 0.1841(5) 0.096(2) Uani 1 1 d . . . O7 O 0.6344(4) 0.5640(4) 0.3225(2) 0.0332(12) Uani 1 1 d . . . O8 O 0.7939(5) 0.6617(5) 0.3104(3) 0.0654(17) Uani 1 1 d . . . O9 O 0.7701(4) 0.4940(4) 0.2825(3) 0.0585(17) Uani 1 1 d . . . O10 O 0.4574(4) 0.6060(4) 0.4071(3) 0.0453(14) Uani 1 1 d . . . O11 O 0.4491(4) 0.7647(4) 0.4667(3) 0.0533(15) Uani 1 1 d . . . O12 O 0.3043(5) 0.6305(5) 0.4534(3) 0.079(2) Uani 1 1 d . . . O1M O 0.4994(4) 0.3619(4) 0.2997(3) 0.0374(12) Uani 1 1 d D . . H1M H 0.555(5) 0.415(5) 0.295(5) 0.10(4) Uiso 1 1 d D . . C1S C 0.3975(11) 0.0397(8) 0.3383(7) 0.130(5) Uani 1 1 d D . . H1S1 H 0.3989 0.1147 0.3604 0.196 Uiso 1 1 calc R . . H1S2 H 0.4286 0.0273 0.2876 0.196 Uiso 1 1 calc R . . H1S3 H 0.4446 0.0221 0.3775 0.196 Uiso 1 1 calc R . . O1S O 0.2869(11) -0.0231(8) 0.3236(8) 0.293(10) Uani 1 1 d D . . H1S H 0.2517 -0.0071 0.2873 0.440 Uiso 1 1 d R . . O2S O 0.9378(12) 0.0879(11) 0.5837(9) 0.389(13) Uani 1 1 d D . . H2S H 0.9030 0.0462 0.6060 0.583 Uiso 1 1 calc R . . C2S C 0.9299(11) 0.1887(10) 0.6218(8) 0.217(11) Uani 1 1 d D . . H2S1 H 0.9962 0.2277 0.6654 0.326 Uiso 1 1 calc R . . H2S2 H 0.8586 0.1841 0.6446 0.326 Uiso 1 1 calc R . . H2S3 H 0.9291 0.2262 0.5824 0.326 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.037(4) 0.040(5) 0.036(4) 0.007(4) -0.004(3) 0.016(4) C2 0.033(4) 0.050(5) 0.037(4) 0.015(4) 0.002(3) 0.025(4) C3 0.019(4) 0.035(4) 0.046(4) 0.021(4) 0.008(3) 0.013(3) C4 0.038(4) 0.028(4) 0.043(4) 0.009(4) -0.002(3) 0.018(4) C5 0.032(4) 0.033(4) 0.039(4) 0.018(4) 0.001(3) 0.013(4) C6 0.031(4) 0.039(5) 0.059(5) 0.018(4) 0.009(4) 0.014(4) C7 0.039(4) 0.029(4) 0.048(4) 0.016(4) 0.008(4) 0.016(4) C8 0.026(4) 0.035(4) 0.046(4) 0.018(4) 0.004(3) 0.013(4) C9 0.043(5) 0.023(4) 0.050(4) 0.016(4) 0.002(4) 0.015(4) C10 0.026(4) 0.031(4) 0.042(4) 0.013(3) -0.003(3) 0.010(3) C11 0.035(4) 0.028(4) 0.034(4) 0.010(3) 0.002(3) 0.018(4) C12 0.035(4) 0.026(4) 0.073(6) 0.018(4) 0.006(4) 0.012(4) C13 0.024(4) 0.032(4) 0.070(5) 0.018(4) 0.002(4) 0.006(4) C14 0.036(4) 0.030(4) 0.042(4) 0.007(4) -0.001(3) 0.020(4) C15 0.040(4) 0.024(4) 0.043(4) 0.011(4) 0.000(3) 0.011(4) C16 0.041(4) 0.033(4) 0.042(4) 0.005(4) 0.005(3) 0.021(4) C17 0.038(4) 0.030(4) 0.052(5) 0.010(4) -0.001(4) 0.015(4) C18 0.039(4) 0.026(4) 0.046(4) 0.020(4) 0.014(4) 0.019(4) C19 0.026(4) 0.032(4) 0.067(5) 0.020(4) -0.002(4) 0.006(4) C20 0.024(4) 0.032(4) 0.061(5) 0.011(4) 0.009(4) 0.012(4) C31 0.048(5) 0.028(4) 0.029(4) 0.004(3) 0.000(3) 0.016(4) C32 0.034(4) 0.034(4) 0.040(4) 0.015(4) -0.006(3) 0.020(4) C33 0.033(4) 0.025(4) 0.034(4) 0.015(3) -0.006(3) 0.008(3) C34 0.036(4) 0.039(4) 0.017(3) 0.009(3) -0.004(3) 0.009(4) C35 0.029(4) 0.023(4) 0.029(4) 0.010(3) 0.002(3) 0.009(3) C36 0.037(4) 0.029(4) 0.032(4) 0.009(3) -0.007(3) 0.006(4) C37 0.042(4) 0.034(4) 0.036(4) 0.012(4) 0.000(4) 0.014(4) C38 0.030(4) 0.036(4) 0.030(4) 0.018(3) 0.000(3) 0.007(4) C39 0.033(4) 0.045(5) 0.038(4) 0.011(4) 0.000(3) 0.016(4) C40 0.038(4) 0.042(5) 0.040(4) 0.022(4) -0.002(3) 0.020(4) C41 0.027(4) 0.039(4) 0.030(4) 0.019(3) -0.001(3) 0.008(4) C42 0.035(4) 0.028(4) 0.024(3) 0.008(3) 0.001(3) 0.008(3) C43 0.031(4) 0.032(4) 0.037(4) 0.022(3) -0.004(3) 0.013(3) C44 0.027(4) 0.045(5) 0.033(4) 0.014(4) 0.007(3) 0.017(4) C45 0.036(4) 0.041(5) 0.031(4) 0.011(3) 0.003(3) 0.020(4) C46 0.088(7) 0.034(5) 0.062(5) 0.017(4) -0.039(5) 0.007(5) C47 0.071(6) 0.041(5) 0.054(5) 0.018(4) -0.043(5) -0.004(5) C48 0.032(4) 0.043(5) 0.032(4) 0.019(4) -0.004(3) 0.014(4) C49 0.066(5) 0.031(4) 0.037(4) 0.019(4) -0.011(4) 0.011(4) C50 0.053(5) 0.038(5) 0.031(4) 0.012(4) -0.007(4) 0.006(4) C51 0.045(5) 0.031(4) 0.042(4) 0.009(4) 0.009(4) 0.008(4) C52 0.047(5) 0.030(5) 0.059(5) 0.011(4) 0.016(4) 0.007(4) C53 0.046(5) 0.029(4) 0.041(4) 0.012(4) -0.006(4) 0.009(4) C54 0.070(6) 0.033(5) 0.043(5) 0.011(4) 0.016(4) -0.001(5) C55 0.055(5) 0.022(4) 0.033(4) 0.007(3) 0.012(4) 0.010(4) C56 0.054(5) 0.031(5) 0.050(5) 0.018(4) 0.009(4) 0.017(4) C57 0.055(5) 0.028(5) 0.053(5) 0.009(4) 0.012(4) 0.011(4) C58 0.042(5) 0.023(4) 0.054(5) 0.008(4) 0.015(4) 0.008(4) C59 0.072(6) 0.034(5) 0.054(5) 0.015(4) -0.011(4) 0.014(5) C60 0.067(6) 0.035(5) 0.058(5) 0.022(4) -0.015(4) 0.009(5) C1M 0.096(7) 0.067(7) 0.058(6) 0.030(5) 0.004(5) 0.009(6) Cu1 0.0306(5) 0.0254(5) 0.0407(5) 0.0123(4) 0.0041(4) 0.0140(4) Cu2 0.0368(5) 0.0236(5) 0.0263(4) 0.0086(4) -0.0074(4) 0.0092(4) N1 0.029(3) 0.025(3) 0.035(3) 0.009(3) 0.011(3) 0.014(3) N2 0.030(3) 0.029(3) 0.042(3) 0.012(3) 0.007(3) 0.017(3) N3 0.026(3) 0.020(3) 0.028(3) 0.008(3) -0.003(2) 0.002(3) N4 0.047(4) 0.025(3) 0.028(3) 0.010(3) -0.007(3) 0.012(3) N5 0.040(3) 0.030(3) 0.021(3) 0.008(3) -0.001(3) 0.012(3) N11 0.038(4) 0.027(4) 0.035(4) 0.007(3) 0.001(3) 0.015(3) N12 0.037(4) 0.032(4) 0.091(6) 0.013(5) 0.012(4) 0.013(4) N13 0.056(5) 0.040(4) 0.032(4) 0.011(3) 0.001(3) 0.024(4) N14 0.036(4) 0.045(4) 0.037(4) 0.017(3) 0.008(3) 0.012(4) O1 0.040(3) 0.031(3) 0.023(2) 0.010(2) -0.004(2) 0.012(2) O2 0.048(3) 0.042(3) 0.035(3) 0.000(3) -0.003(2) 0.004(3) O3 0.057(4) 0.038(3) 0.046(3) 0.018(3) 0.005(3) 0.007(3) O4 0.030(3) 0.037(3) 0.073(4) 0.022(3) 0.012(3) 0.011(3) O5 0.062(4) 0.049(4) 0.081(4) 0.002(4) -0.009(4) 0.026(3) O6 0.065(4) 0.046(4) 0.170(7) 0.040(5) 0.031(4) -0.005(4) O7 0.035(3) 0.033(3) 0.029(3) 0.006(2) -0.002(2) 0.014(3) O8 0.068(4) 0.057(4) 0.079(4) 0.029(4) 0.031(3) 0.015(4) O9 0.060(4) 0.056(4) 0.061(4) 0.008(3) -0.004(3) 0.038(3) O10 0.052(3) 0.047(3) 0.042(3) 0.016(3) 0.004(3) 0.023(3) O11 0.070(4) 0.036(3) 0.047(3) 0.010(3) -0.001(3) 0.010(3) O12 0.044(4) 0.099(5) 0.089(5) 0.027(4) 0.032(3) 0.013(4) O1M 0.046(3) 0.032(3) 0.039(3) 0.019(3) 0.000(2) 0.013(3) C1S 0.206(15) 0.053(7) 0.105(9) 0.016(7) -0.011(10) 0.013(9) O1S 0.280(14) 0.087(8) 0.396(19) -0.085(10) 0.216(14) 0.000(9) O2S 0.331(19) 0.271(17) 0.42(2) 0.172(16) -0.331(17) -0.115(15) C2S 0.218(17) 0.198(17) 0.131(11) 0.123(12) -0.089(11) -0.179(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.336(7) . ? C1 C2 1.388(9) . ? C2 C3 1.381(8) . ? C3 C4 1.390(8) . ? C3 C6 1.455(9) . ? C4 C5 1.394(8) . ? C5 N1 1.336(7) . ? C6 C7 1.174(9) . ? C7 C8 1.446(9) . ? C8 C13 1.370(9) . ? C8 C9 1.391(8) . ? C9 C10 1.372(8) . ? C10 C11 1.385(9) . ? C11 C12 1.389(8) . ? C11 C14 1.437(9) . ? C12 C13 1.384(9) . ? C14 C15 1.180(8) . ? C15 C18 1.444(9) . ? C16 N2 1.349(8) . ? C16 C17 1.377(9) . ? C17 C18 1.395(8) . ? C18 C19 1.388(9) . ? C19 C20 1.359(9) . ? C20 N2 1.339(7) . ? C31 N3 1.359(8) . ? C31 C32 1.359(8) . ? C32 C33 1.386(8) . ? C33 C34 1.388(9) . ? C33 C36 1.428(8) . ? C34 C35 1.393(8) . ? C35 N3 1.333(7) . ? C36 C37 1.190(8) . ? C37 C38 1.444(8) . ? C38 C43 1.390(8) . ? C38 C39 1.392(9) . ? C39 C40 1.388(8) . ? C40 C41 1.391(8) . ? C41 C42 1.377(9) . ? C41 C44 1.440(8) . ? C42 C43 1.387(8) . ? C44 C45 1.186(8) . ? C45 C48 1.455(8) . ? C46 N4 1.326(8) . ? C46 C47 1.372(9) . ? C47 C48 1.370(10) . ? C48 C49 1.364(9) . ? C49 C50 1.386(8) . ? C50 N4 1.319(9) . ? C51 N5 1.324(7) . ? C51 C52 1.382(10) . ? C52 C53 1.393(10) . ? C53 C54 1.373(9) . ? C53 C56 1.442(10) . ? C54 C55 1.389(10) . ? C55 N5 1.338(8) . ? C56 C57 1.181(9) . ? C57 C58 1.442(10) . ? C58 C59 1.377(10) . ? C58 C60 1.384(9) 2_786 ? C59 C60 1.367(10) . ? C60 C58 1.384(9) 2_786 ? C1M O1M 1.411(9) . ? Cu1 O1 1.982(5) . ? Cu1 N2 1.991(5) 1_645 ? Cu1 O4 1.994(5) . ? Cu1 N1 1.996(5) . ? Cu1 O1M 2.259(5) . ? Cu2 N3 2.007(5) . ? Cu2 N4 2.018(5) 1_656 ? Cu2 N5 2.038(6) . ? Cu2 O7 2.117(4) . ? Cu2 O10 2.196(5) . ? N2 Cu1 1.991(5) 1_465 ? N4 Cu2 2.018(5) 1_454 ? N11 O3 1.228(7) . ? N11 O2 1.233(6) . ? N11 O1 1.296(6) . ? N12 O6 1.224(9) . ? N12 O5 1.238(9) . ? N12 O4 1.281(7) . ? N13 O8 1.219(8) . ? N13 O9 1.225(7) . ? N13 O7 1.280(7) . ? N14 O12 1.216(7) . ? N14 O11 1.251(7) . ? N14 O10 1.257(7) . ? C1S O1S 1.363(12) . ? O2S C2S 1.374(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.8(6) . . ? C3 C2 C1 119.3(6) . . ? C2 C3 C4 117.7(6) . . ? C2 C3 C6 120.8(6) . . ? C4 C3 C6 121.5(6) . . ? C3 C4 C5 119.8(6) . . ? N1 C5 C4 121.8(6) . . ? C7 C6 C3 177.4(8) . . ? C6 C7 C8 179.0(8) . . ? C13 C8 C9 119.3(7) . . ? C13 C8 C7 120.6(6) . . ? C9 C8 C7 120.0(7) . . ? C10 C9 C8 120.5(7) . . ? C9 C10 C11 120.1(6) . . ? C10 C11 C12 119.4(6) . . ? C10 C11 C14 121.9(6) . . ? C12 C11 C14 118.6(6) . . ? C13 C12 C11 119.9(7) . . ? C8 C13 C12 120.6(7) . . ? C15 C14 C11 176.8(7) . . ? C14 C15 C18 177.5(8) . . ? N2 C16 C17 124.2(6) . . ? C16 C17 C18 118.4(6) . . ? C19 C18 C17 117.3(6) . . ? C19 C18 C15 121.5(6) . . ? C17 C18 C15 121.1(6) . . ? C20 C19 C18 120.1(6) . . ? N2 C20 C19 123.8(7) . . ? N3 C31 C32 122.8(6) . . ? C31 C32 C33 120.9(6) . . ? C32 C33 C34 116.8(6) . . ? C32 C33 C36 120.8(6) . . ? C34 C33 C36 122.4(6) . . ? C33 C34 C35 119.4(6) . . ? N3 C35 C34 123.3(6) . . ? C37 C36 C33 175.4(7) . . ? C36 C37 C38 176.2(8) . . ? C43 C38 C39 120.2(6) . . ? C43 C38 C37 118.7(6) . . ? C39 C38 C37 121.0(6) . . ? C40 C39 C38 119.6(6) . . ? C39 C40 C41 120.2(7) . . ? C42 C41 C40 119.8(6) . . ? C42 C41 C44 118.9(6) . . ? C40 C41 C44 121.3(6) . . ? C41 C42 C43 120.8(6) . . ? C42 C43 C38 119.4(6) . . ? C45 C44 C41 175.3(8) . . ? C44 C45 C48 178.9(9) . . ? N4 C46 C47 124.0(8) . . ? C48 C47 C46 119.7(7) . . ? C49 C48 C47 117.3(6) . . ? C49 C48 C45 121.7(7) . . ? C47 C48 C45 121.0(6) . . ? C48 C49 C50 119.0(7) . . ? N4 C50 C49 124.4(7) . . ? N5 C51 C52 123.1(7) . . ? C51 C52 C53 119.1(7) . . ? C54 C53 C52 117.1(7) . . ? C54 C53 C56 122.8(7) . . ? C52 C53 C56 120.0(7) . . ? C53 C54 C55 120.6(7) . . ? N5 C55 C54 121.4(7) . . ? C57 C56 C53 171.5(9) . . ? C56 C57 C58 178.6(9) . . ? C59 C58 C60 118.4(7) . 2_786 ? C59 C58 C57 122.1(7) . . ? C60 C58 C57 119.6(7) 2_786 . ? C60 C59 C58 121.4(7) . . ? C59 C60 C58 120.2(7) . 2_786 ? O1 Cu1 N2 91.8(2) . 1_645 ? O1 Cu1 O4 167.22(19) . . ? N2 Cu1 O4 88.5(2) 1_645 . ? O1 Cu1 N1 89.4(2) . . ? N2 Cu1 N1 167.8(2) 1_645 . ? O4 Cu1 N1 93.0(2) . . ? O1 Cu1 O1M 80.18(18) . . ? N2 Cu1 O1M 95.27(19) 1_645 . ? O4 Cu1 O1M 87.1(2) . . ? N1 Cu1 O1M 96.90(19) . . ? N3 Cu2 N4 178.5(2) . 1_656 ? N3 Cu2 N5 87.0(2) . . ? N4 Cu2 N5 93.7(2) 1_656 . ? N3 Cu2 O7 91.76(18) . . ? N4 Cu2 O7 88.67(19) 1_656 . ? N5 Cu2 O7 136.1(2) . . ? N3 Cu2 O10 87.52(19) . . ? N4 Cu2 O10 91.1(2) 1_656 . ? N5 Cu2 O10 143.2(2) . . ? O7 Cu2 O10 80.50(19) . . ? C5 N1 C1 118.5(6) . . ? C5 N1 Cu1 120.8(4) . . ? C1 N1 Cu1 120.7(4) . . ? C20 N2 C16 116.1(6) . . ? C20 N2 Cu1 120.7(4) . 1_465 ? C16 N2 Cu1 122.9(5) . 1_465 ? C35 N3 C31 116.8(5) . . ? C35 N3 Cu2 124.7(4) . . ? C31 N3 Cu2 118.1(4) . . ? C50 N4 C46 115.6(6) . . ? C50 N4 Cu2 119.9(4) . 1_454 ? C46 N4 Cu2 124.4(5) . 1_454 ? C51 N5 C55 118.4(6) . . ? C51 N5 Cu2 121.0(5) . . ? C55 N5 Cu2 120.5(5) . . ? O3 N11 O2 124.0(6) . . ? O3 N11 O1 117.6(5) . . ? O2 N11 O1 118.4(6) . . ? O6 N12 O5 122.2(8) . . ? O6 N12 O4 118.4(9) . . ? O5 N12 O4 119.4(8) . . ? O8 N13 O9 122.7(7) . . ? O8 N13 O7 117.7(7) . . ? O9 N13 O7 119.5(7) . . ? O12 N14 O11 121.8(7) . . ? O12 N14 O10 120.7(7) . . ? O11 N14 O10 117.5(6) . . ? N11 O1 Cu1 114.5(4) . . ? N12 O4 Cu1 112.9(5) . . ? N13 O7 Cu2 113.2(4) . . ? N14 O10 Cu2 104.5(4) . . ? C1M O1M Cu1 134.8(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1M H1M O7 0.899(11) 1.93(4) 2.750(7) 152(8) . O1M H1M O9 0.899(11) 2.63(5) 3.433(8) 150(7) . O1S H1S O6 0.85 2.40 3.254(18) 179.6 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.495 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.067 #===END