Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Chen, Xiao-Ming' 'Ling, Yong-Hua' 'Liu, Gao-Feng' 'Ye, Bao-Hui' _publ_contact_author_name 'Prof Xiao-Ming Chen' _publ_contact_author_address ; School of Chemistry and Chemical Engineering Sun Yat-Sen University 135 Xingang Rd. W. Guangzhou 510275 CHINA ; _publ_contact_author_phone '86 20 84113986' _publ_contact_author_fax '86 20 84112245' _publ_contact_author_email cescxm@zsu.edu.cn _publ_requested_joiurnal 'Chem. Commun.' _publ_requested_coeditor_name ? _publ_section_title ; Interlocking of Molecular Rhombi into 2D Polyrotaxane Network via Molecular Recognition. Crystal Structure of [Cu2(bpa)2(phen)2(H2O)]2(H2O (bpa2- = Biphenyl-4,4(-dicarboxylate, phen = 1,10-Phenanthroline ; _publ_contact_letter ; Dear Sir/Madam: Please consider this CIF as supplmentary data for a manuscript submitted to Chem. Commun. Xiao-Ming Chen ; #============================================================ data_cu1 _database_code_CSD 184400 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H72 Cu4 N8 O20' _chemical_formula_weight 2007.86 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.358(5) _cell_length_b 15.008(3) _cell_length_c 25.479(5) _cell_angle_alpha 90.00(2) _cell_angle_beta 90.00(2) _cell_angle_gamma 90.00(2) _cell_volume 8932(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 30 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4112 _exptl_absorpt_coefficient_mu 1.020 _exptl_absorpt_correction_type 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.6296 _exptl_absorpt_correction_T_max 0.8299 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_decay_% none _diffrn_reflns_number 50590 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.13 _reflns_number_total 9721 _reflns_number_gt 6562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+13.1702P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00000(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9721 _refine_ls_number_parameters 614 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1413 _refine_ls_wR_factor_gt 0.1180 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.072 _refine_ls_shift/su_mean 0.001 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 Cu1 Cu 0.034372(18) 0.04192(3) 0.126227(17) 0.05566(14) Uani 1 d . . . Cu2 Cu 0.356147(18) -0.57232(3) 0.491741(19) 0.06172(15) Uani 1 d . . . O1 O 0.03003(17) -1.1112(2) 0.77005(14) 0.1068(12) Uani 1 d . . . O2 O 0.02825(12) -1.0030(2) 0.82896(10) 0.0697(7) Uani 1 d . . . O3 O 0.31582(13) -0.7073(2) 0.50920(11) 0.0764(8) Uani 1 d . . . O4 O 0.30772(11) -0.58855(19) 0.55847(11) 0.0669(7) Uani 1 d . . . O5 O 0.08421(13) -0.0413(2) 0.16197(11) 0.0771(8) Uani 1 d . . . O6 O 0.13846(15) 0.0595(2) 0.20120(15) 0.0990(12) Uani 1 d . . . O7 O 0.28947(14) -0.5431(2) 0.43768(12) 0.0821(9) Uani 1 d . . . O8 O 0.32563(15) -0.4302(3) 0.47823(15) 0.1024(12) Uani 1 d . . . O1W O 0.05519(13) 0.17370(18) 0.16595(12) 0.0763(8) Uani 1 d . . . H1WA H 0.0280 0.1555 0.1926 0.050 Uiso 1 d R . . H1WB H 0.0857 0.1481 0.1779 0.050 Uiso 1 d R . . O2W O 0.1198(4) 0.1307(5) 0.3047(3) 0.327(6) Uani 1 d . . . H2WA H 0.1294 0.1317 0.3182 0.050 Uiso 1 d R . . H2WB H 0.0715 0.1427 0.2902 0.050 Uiso 1 d R . . N1 N 0.41163(12) -0.5875(2) 0.43137(13) 0.0593(8) Uani 1 d . . . N2 N 0.42895(14) -0.5925(2) 0.53318(13) 0.0619(8) Uani 1 d . . . N3 N -0.01958(12) 0.0966(2) 0.07398(12) 0.0540(7) Uani 1 d . . . N4 N 0.08958(12) 0.0558(2) 0.06559(12) 0.0572(7) Uani 1 d . . . C1 C 0.04472(17) -1.0379(3) 0.78653(15) 0.0622(9) Uani 1 d . . . C2 C 0.08620(15) -0.9830(2) 0.75501(13) 0.0539(8) Uani 1 d . . . C3 C 0.09430(17) -0.8939(3) 0.76443(14) 0.0617(9) Uani 1 d . . . H3A H 0.0744 -0.8667 0.7930 0.080 Uiso 1 d R . . C4 C 0.13070(16) -0.8435(3) 0.73376(14) 0.0611(9) Uani 1 d . . . H4A H 0.1354 -0.7813 0.7408 0.080 Uiso 1 d R . . C5 C 0.16090(14) -0.8814(2) 0.69237(12) 0.0489(8) Uani 1 d . . . C6 C 0.15350(17) -0.9719(3) 0.68411(14) 0.0612(9) Uani 1 d . . . H6A H 0.1748 -1.0008 0.6570 0.080 Uiso 1 d R . . C7 C 0.11653(18) -1.0216(3) 0.71429(15) 0.0641(10) Uani 1 d . . . H7A H 0.1109 -1.0835 0.7069 0.080 Uiso 1 d R . . C8 C 0.19803(14) -0.8271(2) 0.65722(12) 0.0493(8) Uani 1 d . . . C9 C 0.21488(18) -0.8591(3) 0.60851(14) 0.0663(10) Uani 1 d . . . H9A H 0.2038 -0.9179 0.5982 0.080 Uiso 1 d R . . C10 C 0.24698(18) -0.8082(3) 0.57485(14) 0.0677(10) Uani 1 d . . . H10A H 0.2584 -0.8324 0.5417 0.080 Uiso 1 d R . . C11 C 0.26360(14) -0.7232(2) 0.58797(13) 0.0521(8) Uani 1 d . . . C12 C 0.24636(18) -0.6901(3) 0.63612(15) 0.0648(10) Uani 1 d . . . H12A H 0.2575 -0.6311 0.6459 0.080 Uiso 1 d R . . C13 C 0.21461(17) -0.7414(3) 0.67014(14) 0.0634(10) Uani 1 d . . . H13A H 0.2034 -0.7173 0.7033 0.080 Uiso 1 d R . . C14 C 0.29786(15) -0.6704(3) 0.54907(15) 0.0598(9) Uani 1 d . . . C15 C 0.12240(18) -0.0178(3) 0.19379(16) 0.0673(10) Uani 1 d . . . C16 C 0.14949(16) -0.0912(3) 0.22527(15) 0.0610(9) Uani 1 d . . . C17 C 0.12395(18) -0.1733(3) 0.22999(16) 0.0699(11) Uani 1 d . . . H17A H 0.0910 -0.1865 0.2092 0.080 Uiso 1 d R . . C18 C 0.14539(17) -0.2366(3) 0.26478(15) 0.0681(10) Uani 1 d . . . H18A H 0.1269 -0.2931 0.2686 0.080 Uiso 1 d R . . C19 C 0.19390(16) -0.2183(2) 0.29443(13) 0.0563(9) Uani 1 d . . . C20 C 0.22100(16) -0.1373(3) 0.28662(14) 0.0611(9) Uani 1 d . . . H20A H 0.2558 -0.1256 0.3052 0.080 Uiso 1 d R . . C21 C 0.19894(17) -0.0739(3) 0.25349(15) 0.0641(10) Uani 1 d . . . H21A H 0.2176 -0.0174 0.2501 0.080 Uiso 1 d R . . C22 C 0.21639(16) -0.2823(2) 0.33355(14) 0.0560(9) Uani 1 d . . . C23 C 0.21266(19) -0.3737(3) 0.32641(16) 0.0699(11) Uani 1 d . . . H23A H 0.1934 -0.3967 0.2962 0.080 Uiso 1 d R . . C24 C 0.23613(19) -0.4312(3) 0.36287(17) 0.0714(11) Uani 1 d . . . H24A H 0.2325 -0.4941 0.3578 0.080 Uiso 1 d R . . C25 C 0.26388(15) -0.4001(3) 0.40657(14) 0.0572(9) Uani 1 d . . . C26 C 0.26568(17) -0.3097(3) 0.41479(15) 0.0632(10) Uani 1 d . . . H26A H 0.2840 -0.2870 0.4456 0.080 Uiso 1 d R . . C27 C 0.24219(17) -0.2517(3) 0.37931(14) 0.0633(10) Uani 1 d . . . H27A H 0.2430 -0.1890 0.3862 0.080 Uiso 1 d R . . C28 C 0.29505(19) -0.4615(3) 0.44406(18) 0.0724(12) Uani 1 d . . . C29 C 0.40244(19) -0.5811(3) 0.38056(17) 0.0768(12) Uani 1 d . . . H29A H 0.3653 -0.5629 0.3691 0.080 Uiso 1 d R . . C30 C 0.4446(2) -0.6003(4) 0.3436(2) 0.0954(15) Uani 1 d . . . H30A H 0.4364 -0.5918 0.3072 0.080 Uiso 1 d R . . C31 C 0.4962(2) -0.6296(4) 0.3589(2) 0.0907(15) Uani 1 d . . . H31A H 0.5244 -0.6450 0.3333 0.080 Uiso 1 d R . . C32 C 0.50789(16) -0.6371(3) 0.4121(2) 0.0706(11) Uani 1 d . . . C33 C 0.46433(14) -0.6137(2) 0.44728(16) 0.0557(9) Uani 1 d . . . C34 C 0.5612(2) -0.6656(3) 0.4329(3) 0.0903(15) Uani 1 d . . . H34A H 0.5907 -0.6850 0.4094 0.080 Uiso 1 d R . . C35 C 0.57078(17) -0.6648(3) 0.4842(3) 0.0876(15) Uani 1 d . . . H35A H 0.6075 -0.6818 0.4973 0.080 Uiso 1 d R . . C36 C 0.52788(17) -0.6383(3) 0.5217(2) 0.0707(11) Uani 1 d . . . C37 C 0.47385(14) -0.6148(2) 0.50206(16) 0.0564(9) Uani 1 d . . . C38 C 0.5344(2) -0.6340(3) 0.5753(2) 0.0901(15) Uani 1 d . . . H38A H 0.5706 -0.6479 0.5907 0.080 Uiso 1 d R . . C39 C 0.4905(3) -0.6102(3) 0.6066(2) 0.0949(16) Uani 1 d . . . H39A H 0.4954 -0.6066 0.6438 0.080 Uiso 1 d R . . C40 C 0.4368(2) -0.5904(3) 0.58419(19) 0.0820(13) Uani 1 d . . . H40A H 0.4050 -0.5757 0.6061 0.080 Uiso 1 d R . . C41 C -0.07402(16) 0.1195(3) 0.07984(18) 0.0696(11) Uani 1 d . . . H41A H -0.0910 0.1122 0.1137 0.080 Uiso 1 d R . . C42 C -0.10635(18) 0.1539(3) 0.0393(2) 0.0792(13) Uani 1 d . . . H42A H -0.1452 0.1711 0.0450 0.080 Uiso 1 d R . . C43 C -0.0831(2) 0.1617(3) -0.00890(19) 0.0774(12) Uani 1 d . . . H43A H -0.1054 0.1838 -0.0375 0.080 Uiso 1 d R . . C44 C -0.02570(18) 0.1386(2) -0.01730(15) 0.0629(10) Uani 1 d . . . C45 C 0.00446(15) 0.1076(2) 0.02608(13) 0.0505(8) Uani 1 d . . . C46 C 0.0042(2) 0.1449(3) -0.06631(16) 0.0774(13) Uani 1 d . . . H46A H -0.0162 0.1625 -0.0971 0.080 Uiso 1 d R . . C47 C 0.0596(2) 0.1256(3) -0.07019(16) 0.0809(13) Uani 1 d . . . H47A H 0.0788 0.1314 -0.1032 0.080 Uiso 1 d R . . C48 C 0.09188(19) 0.0966(3) -0.02607(15) 0.0653(10) Uani 1 d . . . C49 C 0.06365(15) 0.0859(2) 0.02171(13) 0.0519(8) Uani 1 d . . . C50 C 0.1509(2) 0.0763(3) -0.02619(19) 0.0822(14) Uani 1 d . . . H50A H 0.1723 0.0824 -0.0579 0.080 Uiso 1 d R . . C51 C 0.17674(18) 0.0473(4) 0.01850(19) 0.0857(14) Uani 1 d . . . H51A H 0.2167 0.0340 0.0182 0.080 Uiso 1 d R . . C52 C 0.14515(16) 0.0368(3) 0.06349(17) 0.0736(12) Uani 1 d . . . H52A H 0.1637 0.0164 0.0947 0.080 Uiso 1 d 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 0.0483(2) 0.0670(3) 0.0517(2) 0.0136(2) -0.00195(18) -0.0016(2) Cu2 0.0449(2) 0.0711(3) 0.0691(3) 0.0236(2) 0.0083(2) 0.0127(2) O1 0.136(3) 0.075(2) 0.110(3) -0.0132(19) 0.050(2) -0.033(2) O2 0.0760(18) 0.0801(19) 0.0530(15) 0.0079(13) 0.0117(13) -0.0133(15) O3 0.085(2) 0.0795(19) 0.0651(16) 0.0110(15) 0.0299(15) 0.0130(16) O4 0.0626(16) 0.0631(17) 0.0749(17) 0.0159(13) 0.0079(13) 0.0085(13) O5 0.0760(19) 0.084(2) 0.0715(18) 0.0160(15) -0.0189(15) 0.0041(16) O6 0.093(2) 0.080(2) 0.124(3) 0.040(2) -0.047(2) -0.0155(18) O7 0.087(2) 0.072(2) 0.087(2) 0.0243(16) 0.0194(17) 0.0264(16) O8 0.088(2) 0.120(3) 0.100(2) 0.037(2) -0.035(2) 0.010(2) O1W 0.0726(18) 0.0638(17) 0.092(2) 0.0115(15) -0.0092(15) -0.0081(14) O2W 0.449(16) 0.284(11) 0.248(9) 0.069(8) 0.017(10) 0.077(11) N1 0.0426(15) 0.0643(19) 0.071(2) 0.0067(16) 0.0030(14) -0.0019(14) N2 0.0631(19) 0.0538(18) 0.069(2) 0.0060(15) -0.0021(16) 0.0030(15) N3 0.0424(15) 0.0560(17) 0.0636(18) 0.0152(14) -0.0010(13) -0.0048(12) N4 0.0421(15) 0.073(2) 0.0562(17) 0.0047(15) -0.0035(13) -0.0084(14) C1 0.064(2) 0.066(3) 0.057(2) 0.0113(19) 0.0039(18) -0.0006(19) C2 0.057(2) 0.062(2) 0.0428(17) 0.0106(16) -0.0008(15) 0.0024(17) C3 0.069(2) 0.066(2) 0.050(2) 0.0016(17) 0.0134(17) 0.0010(19) C4 0.071(2) 0.059(2) 0.054(2) -0.0049(17) 0.0110(18) -0.0022(18) C5 0.0474(18) 0.058(2) 0.0409(16) 0.0038(15) -0.0014(14) 0.0057(15) C6 0.076(3) 0.056(2) 0.051(2) 0.0022(17) 0.0143(18) 0.0062(19) C7 0.080(3) 0.055(2) 0.057(2) 0.0047(17) 0.011(2) 0.0011(19) C8 0.0508(18) 0.056(2) 0.0415(16) 0.0020(14) 0.0016(14) 0.0045(15) C9 0.087(3) 0.059(2) 0.053(2) -0.0068(17) 0.016(2) -0.010(2) C10 0.085(3) 0.071(3) 0.0471(19) -0.0041(18) 0.0184(19) -0.002(2) C11 0.0503(19) 0.056(2) 0.0504(18) 0.0081(16) 0.0058(15) 0.0075(15) C12 0.076(3) 0.052(2) 0.066(2) -0.0039(17) 0.016(2) -0.0019(19) C13 0.077(3) 0.060(2) 0.054(2) -0.0051(17) 0.0179(19) -0.0017(19) C14 0.051(2) 0.062(2) 0.066(2) 0.0163(19) 0.0047(17) 0.0131(17) C15 0.061(2) 0.075(3) 0.066(2) 0.020(2) -0.0035(19) -0.004(2) C16 0.059(2) 0.068(2) 0.057(2) 0.0127(18) -0.0042(17) 0.0055(18) C17 0.068(2) 0.072(3) 0.070(2) 0.006(2) -0.024(2) 0.004(2) C18 0.074(3) 0.061(2) 0.069(2) 0.0044(19) -0.018(2) 0.002(2) C19 0.060(2) 0.057(2) 0.0512(19) -0.0014(16) -0.0099(16) 0.0126(17) C20 0.056(2) 0.067(2) 0.060(2) 0.0058(18) -0.0092(17) 0.0059(18) C21 0.059(2) 0.068(2) 0.066(2) 0.0134(19) -0.0056(18) 0.0017(18) C22 0.062(2) 0.053(2) 0.054(2) -0.0023(16) -0.0071(17) 0.0112(16) C23 0.086(3) 0.059(2) 0.065(2) -0.0089(19) -0.022(2) 0.011(2) C24 0.086(3) 0.048(2) 0.079(3) -0.0004(19) -0.009(2) 0.013(2) C25 0.054(2) 0.060(2) 0.058(2) 0.0098(17) 0.0007(16) 0.0138(17) C26 0.069(2) 0.065(2) 0.056(2) 0.0028(18) -0.0141(18) 0.0068(19) C27 0.075(2) 0.053(2) 0.062(2) -0.0011(17) -0.0171(19) 0.0106(19) C28 0.061(2) 0.077(3) 0.079(3) 0.024(2) 0.021(2) 0.020(2) C29 0.059(2) 0.099(3) 0.072(3) 0.002(2) 0.000(2) -0.010(2) C30 0.098(4) 0.118(4) 0.071(3) -0.009(3) 0.006(3) -0.008(3) C31 0.084(3) 0.096(4) 0.092(4) -0.011(3) 0.031(3) 0.000(3) C32 0.050(2) 0.058(2) 0.104(3) -0.001(2) 0.017(2) -0.0029(18) C33 0.0419(18) 0.0439(19) 0.081(3) 0.0052(17) 0.0032(17) -0.0055(14) C34 0.056(3) 0.079(3) 0.135(5) 0.006(3) 0.021(3) 0.004(2) C35 0.037(2) 0.072(3) 0.153(5) 0.011(3) -0.003(3) 0.0041(19) C36 0.058(2) 0.047(2) 0.108(3) 0.011(2) -0.021(2) -0.0055(17) C37 0.0440(18) 0.0389(18) 0.086(3) 0.0069(17) -0.0015(18) -0.0029(14) C38 0.079(3) 0.068(3) 0.123(4) 0.008(3) -0.038(3) -0.004(2) C39 0.125(5) 0.079(3) 0.081(3) 0.001(3) -0.034(3) -0.005(3) C40 0.097(3) 0.075(3) 0.074(3) -0.002(2) -0.005(3) 0.011(3) C41 0.048(2) 0.073(3) 0.087(3) 0.023(2) 0.002(2) 0.0026(18) C42 0.054(2) 0.076(3) 0.108(4) 0.020(3) -0.011(2) 0.011(2) C43 0.081(3) 0.060(3) 0.092(3) 0.015(2) -0.033(3) 0.006(2) C44 0.080(3) 0.0421(19) 0.066(2) 0.0082(17) -0.017(2) -0.0049(18) C45 0.057(2) 0.0423(18) 0.0526(19) 0.0054(14) -0.0068(16) -0.0079(15) C46 0.119(4) 0.057(2) 0.057(2) 0.0084(19) -0.020(3) -0.002(3) C47 0.120(4) 0.072(3) 0.051(2) 0.005(2) 0.010(2) -0.010(3) C48 0.077(3) 0.062(2) 0.057(2) -0.0018(18) 0.0089(19) -0.016(2) C49 0.0511(19) 0.051(2) 0.0540(19) 0.0010(15) -0.0018(15) -0.0123(15) C50 0.077(3) 0.097(3) 0.072(3) -0.014(2) 0.028(2) -0.029(3) C51 0.047(2) 0.122(4) 0.088(3) -0.019(3) 0.007(2) -0.019(2) C52 0.0404(19) 0.108(3) 0.073(3) -0.006(2) -0.0035(18) -0.006(2) _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 O5 1.935(3) . ? Cu1 O2 1.945(3) 5_546 ? Cu1 N3 2.009(3) . ? Cu1 N4 2.023(3) . ? Cu1 O1W 2.274(3) . ? Cu2 N1 2.024(3) . ? Cu2 N2 2.025(3) . ? Cu2 O4 2.057(3) . ? Cu2 O7 2.125(3) . ? Cu2 O8 2.275(4) . ? Cu2 O3 2.279(3) . ? Cu2 C14 2.481(4) . ? Cu2 C28 2.506(4) . ? O1 C1 1.226(5) . ? O2 C1 1.262(5) . ? O2 Cu1 1.945(3) 5_546 ? O3 C14 1.231(4) . ? O4 C14 1.273(5) . ? O5 C15 1.256(5) . ? O6 C15 1.233(5) . ? O7 C28 1.242(5) . ? O8 C28 1.220(6) . ? N1 C29 1.316(5) . ? N1 C33 1.355(4) . ? N2 C40 1.313(5) . ? N2 C37 1.356(5) . ? N3 C41 1.326(4) . ? N3 C45 1.354(4) . ? N4 C52 1.330(5) . ? N4 C49 1.349(4) . ? C1 C2 1.504(5) . ? C2 C3 1.372(5) . ? C2 C7 1.383(5) . ? C3 C4 1.380(5) . ? C4 C5 1.390(5) . ? C5 C6 1.385(5) . ? C5 C8 1.490(5) . ? C6 C7 1.376(5) . ? C8 C13 1.383(5) . ? C8 C9 1.388(5) . ? C9 C10 1.371(5) . ? C10 C11 1.375(5) . ? C11 C12 1.384(5) . ? C11 C14 1.500(5) . ? C12 C13 1.376(5) . ? C15 C16 1.502(5) . ? C16 C17 1.374(6) . ? C16 C21 1.385(5) . ? C17 C18 1.392(5) . ? C18 C19 1.389(5) . ? C19 C20 1.385(5) . ? C19 C22 1.480(5) . ? C20 C21 1.373(5) . ? C22 C23 1.387(5) . ? C22 C27 1.390(5) . ? C23 C24 1.381(5) . ? C24 C25 1.370(5) . ? C25 C26 1.373(5) . ? C25 C28 1.514(5) . ? C26 C27 1.370(5) . ? C29 C30 1.392(6) . ? C30 C31 1.340(7) . ? C31 C32 1.388(7) . ? C32 C33 1.400(5) . ? C32 C34 1.420(6) . ? C33 C37 1.414(5) . ? C34 C35 1.327(7) . ? C35 C36 1.441(7) . ? C36 C38 1.376(7) . ? C36 C37 1.403(5) . ? C38 C39 1.346(7) . ? C39 C40 1.412(7) . ? C41 C42 1.380(6) . ? C42 C43 1.347(6) . ? C43 C44 1.402(6) . ? C44 C45 1.391(5) . ? C44 C46 1.434(6) . ? C45 C49 1.425(5) . ? C46 C47 1.330(7) . ? C47 C48 1.421(6) . ? C48 C49 1.394(5) . ? C48 C50 1.411(6) . ? C50 C51 1.360(7) . ? C51 C52 1.372(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 O5 Cu1 O2 88.99(13) . 5_546 ? O5 Cu1 N3 162.41(13) . . ? O2 Cu1 N3 92.29(12) 5_546 . ? O5 Cu1 N4 92.43(13) . . ? O2 Cu1 N4 163.41(12) 5_546 . ? N3 Cu1 N4 81.47(12) . . ? O5 Cu1 O1W 102.90(12) . . ? O2 Cu1 O1W 99.25(12) 5_546 . ? N3 Cu1 O1W 94.22(12) . . ? N4 Cu1 O1W 96.54(12) . . ? N1 Cu2 N2 80.89(13) . . ? N1 Cu2 O4 165.26(12) . . ? N2 Cu2 O4 90.76(12) . . ? N1 Cu2 O7 90.00(12) . . ? N2 Cu2 O7 169.94(12) . . ? O4 Cu2 O7 99.04(11) . . ? N1 Cu2 O8 101.01(14) . . ? N2 Cu2 O8 118.86(13) . . ? O4 Cu2 O8 93.65(13) . . ? O7 Cu2 O8 58.57(13) . . ? N1 Cu2 O3 108.25(11) . . ? N2 Cu2 O3 96.44(12) . . ? O4 Cu2 O3 60.39(11) . . ? O7 Cu2 O3 90.42(12) . . ? O8 Cu2 O3 137.20(12) . . ? N1 Cu2 C14 137.06(13) . . ? N2 Cu2 C14 93.73(12) . . ? O4 Cu2 C14 30.82(12) . . ? O7 Cu2 C14 95.86(12) . . ? O8 Cu2 C14 118.26(13) . . ? O3 Cu2 C14 29.58(11) . . ? N1 Cu2 C28 94.06(13) . . ? N2 Cu2 C28 146.18(15) . . ? O4 Cu2 C28 99.56(12) . . ? O7 Cu2 C28 29.68(14) . . ? O8 Cu2 C28 29.06(14) . . ? O3 Cu2 C28 116.71(14) . . ? C14 Cu2 C28 111.52(13) . . ? C1 O2 Cu1 127.4(3) . 5_546 ? C14 O3 Cu2 84.4(2) . . ? C14 O4 Cu2 93.3(2) . . ? C15 O5 Cu1 123.3(3) . . ? C28 O7 Cu2 92.4(3) . . ? C28 O8 Cu2 86.0(3) . . ? C29 N1 C33 117.6(3) . . ? C29 N1 Cu2 129.4(3) . . ? C33 N1 Cu2 112.8(3) . . ? C40 N2 C37 118.5(4) . . ? C40 N2 Cu2 129.0(3) . . ? C37 N2 Cu2 112.4(3) . . ? C41 N3 C45 117.9(3) . . ? C41 N3 Cu1 129.3(3) . . ? C45 N3 Cu1 112.8(2) . . ? C52 N4 C49 118.5(3) . . ? C52 N4 Cu1 129.1(3) . . ? C49 N4 Cu1 112.4(2) . . ? O1 C1 O2 125.5(4) . . ? O1 C1 C2 119.3(4) . . ? O2 C1 C2 115.2(4) . . ? C3 C2 C7 117.9(3) . . ? C3 C2 C1 122.0(3) . . ? C7 C2 C1 120.1(4) . . ? C2 C3 C4 121.3(3) . . ? C3 C4 C5 121.2(4) . . ? C6 C5 C4 116.9(3) . . ? C6 C5 C8 121.2(3) . . ? C4 C5 C8 121.8(3) . . ? C7 C6 C5 121.6(3) . . ? C6 C7 C2 120.9(4) . . ? C13 C8 C9 117.1(3) . . ? C13 C8 C5 121.9(3) . . ? C9 C8 C5 120.9(3) . . ? C10 C9 C8 121.4(4) . . ? C9 C10 C11 121.3(3) . . ? C10 C11 C12 117.8(3) . . ? C10 C11 C14 118.7(3) . . ? C12 C11 C14 123.5(4) . . ? C13 C12 C11 121.0(4) . . ? C12 C13 C8 121.4(3) . . ? O3 C14 O4 121.9(4) . . ? O3 C14 C11 119.3(4) . . ? O4 C14 C11 118.8(3) . . ? O3 C14 Cu2 66.1(2) . . ? O4 C14 Cu2 55.85(19) . . ? C11 C14 Cu2 174.4(3) . . ? O6 C15 O5 125.4(4) . . ? O6 C15 C16 118.6(4) . . ? O5 C15 C16 116.0(4) . . ? C17 C16 C21 119.0(3) . . ? C17 C16 C15 121.4(4) . . ? C21 C16 C15 119.4(4) . . ? C16 C17 C18 120.8(4) . . ? C19 C18 C17 120.3(4) . . ? C20 C19 C18 117.9(3) . . ? C20 C19 C22 120.3(3) . . ? C18 C19 C22 121.8(4) . . ? C21 C20 C19 121.7(4) . . ? C20 C21 C16 120.2(4) . . ? C23 C22 C27 117.6(3) . . ? C23 C22 C19 122.1(3) . . ? C27 C22 C19 120.3(3) . . ? C24 C23 C22 120.3(4) . . ? C25 C24 C23 121.4(4) . . ? C24 C25 C26 118.4(3) . . ? C24 C25 C28 122.2(4) . . ? C26 C25 C28 119.4(4) . . ? C27 C26 C25 121.0(4) . . ? C26 C27 C22 121.2(4) . . ? O8 C28 O7 122.3(4) . . ? O8 C28 C25 119.8(4) . . ? O7 C28 C25 117.8(5) . . ? O8 C28 Cu2 64.9(3) . . ? O7 C28 Cu2 57.9(2) . . ? C25 C28 Cu2 169.7(3) . . ? N1 C29 C30 122.3(4) . . ? C31 C30 C29 120.5(5) . . ? C30 C31 C32 119.2(4) . . ? C31 C32 C33 117.5(4) . . ? C31 C32 C34 124.2(4) . . ? C33 C32 C34 118.3(5) . . ? N1 C33 C32 122.8(4) . . ? N1 C33 C37 116.2(3) . . ? C32 C33 C37 121.0(4) . . ? C35 C34 C32 120.8(5) . . ? C34 C35 C36 122.7(4) . . ? C38 C36 C37 116.3(4) . . ? C38 C36 C35 126.5(4) . . ? C37 C36 C35 117.3(4) . . ? N2 C37 C36 123.3(4) . . ? N2 C37 C33 116.9(3) . . ? C36 C37 C33 119.8(4) . . ? C39 C38 C36 121.0(5) . . ? C38 C39 C40 119.6(5) . . ? N2 C40 C39 121.3(5) . . ? N3 C41 C42 122.5(4) . . ? C43 C42 C41 119.7(4) . . ? C42 C43 C44 120.2(4) . . ? C45 C44 C43 116.5(4) . . ? C45 C44 C46 117.8(4) . . ? C43 C44 C46 125.7(4) . . ? N3 C45 C44 123.2(3) . . ? N3 C45 C49 116.4(3) . . ? C44 C45 C49 120.4(3) . . ? C47 C46 C44 121.6(4) . . ? C46 C47 C48 121.6(4) . . ? C49 C48 C50 116.0(4) . . ? C49 C48 C47 118.4(4) . . ? C50 C48 C47 125.6(4) . . ? N4 C49 C48 123.4(3) . . ? N4 C49 C45 116.6(3) . . ? C48 C49 C45 120.1(3) . . ? C51 C50 C48 120.1(4) . . ? C50 C51 C52 119.8(4) . . ? N4 C52 C51 122.2(4) . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 27.13 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 0.703 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.062 #End of Crystallographic Information File