Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'ProfD Nirmalendu Ray Chaudhuri' _publ_contact_author_address ; Department of Inorganic Chemistry Indian Association for the Cultivation of Science Raja S. C. Mallik Road Jadavpur Kolkata West Bengal 700 032 INDIA ; _publ_contact_author_email ICNRC@IACS.RES.IN _publ_section_title ; Polymeric networks of copper(II) using succinate and aromatic N-N donor ligands: synthesis, crystal structure, magnetic behaviour and the effect of weak interactions on their crystal packing ; loop_ _publ_author_name 'Nirmalendu Ray Chaudhuri' 'Debajyoti Ghoshal' 'Tian-Huey Lu' 'Tapas Kumar Maji' 'Golam Mostafa' 'Joan Ribas' ; S.Sain ; 'Ennio Zangrando' #===END data_complex4 _database_code_depnum_ccdc_archive 'CCDC 208793' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C160 H128 B8 Cu8 F32 N24 O24' _chemical_formula_weight 3973.66 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' F F 0.0171 0.0103 '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' B B 0.0013 0.0007 '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 12.5769(10) _cell_length_b 19.3034(15) _cell_length_c 19.3348(16) _cell_angle_alpha 60.187(2) _cell_angle_beta 86.864(2) _cell_angle_gamma 80.538(2) _cell_volume 4015.4(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Irregular _exptl_crystal_colour Blue _exptl_crystal_size_max .2 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 1.153 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min .8782 _exptl_absorpt_correction_T_max .9755 _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 '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_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42987 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_sigmaI/netI 0.2328 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 28.30 _reflns_number_total 19122 _reflns_number_gt 7039 _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, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1997)' _computing_publication_material 'Platon99 (Spek, 1999)' _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 w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+0.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19122 _refine_ls_number_parameters 1261 _refine_ls_number_restraints 135 _refine_ls_R_factor_all 0.2107 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 0.833 _refine_ls_restrained_S_all 0.852 _refine_ls_shift/su_max 0.001 _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 0.20783(5) 0.21585(4) 0.89500(4) 0.03943(19) Uani 1 1 d . . . Cu2 Cu 0.19407(5) 0.31491(4) 0.63457(4) 0.03671(18) Uani 1 1 d . . . Cu3 Cu -0.10306(5) 0.64583(4) 0.53016(4) 0.03654(18) Uani 1 1 d . . . Cu4 Cu -0.08323(5) 0.64633(4) 0.76282(4) 0.0420(2) Uani 1 1 d . . . O1 O 0.1979(3) 0.33421(19) 0.8481(2) 0.0402(10) Uani 1 1 d . . . O2 O 0.1927(3) 0.31766(19) 0.74399(18) 0.0409(9) Uani 1 1 d . . . O3 O -0.0565(3) 0.53642(19) 0.7765(2) 0.0450(10) Uani 1 1 d . . . O4 O -0.0423(3) 0.6100(2) 0.6475(2) 0.0415(9) Uani 1 1 d . . . O5 O 0.0265(3) 0.6136(2) 0.4864(2) 0.0448(10) Uani 1 1 d . . . O6 O -0.0371(3) 0.6794(2) 0.3597(2) 0.0459(10) Uani 1 1 d . . . O7 O 0.1929(3) 0.4301(2) 0.5628(2) 0.0439(10) Uani 1 1 d . . . O8 O 0.1539(3) 0.45522(19) 0.4393(2) 0.0439(10) Uani 1 1 d . . . C1S C 0.1831(4) 0.3625(3) 0.7745(4) 0.0371(14) Uani 1 1 d . . . C2S C 0.1441(4) 0.4517(3) 0.7243(3) 0.0417(14) Uani 1 1 d . . . H2S1 H 0.1796 0.4728 0.6736 0.050 Uiso 1 1 calc R . . H2S2 H 0.1615 0.4797 0.7512 0.050 Uiso 1 1 calc R . . C3S C 0.0204(4) 0.4660(3) 0.7102(4) 0.0574(18) Uani 1 1 d . . . H3S1 H 0.0048 0.4702 0.6596 0.069 Uiso 1 1 calc R . . H3S2 H -0.0099 0.4205 0.7521 0.069 Uiso 1 1 calc R . . C4S C -0.0305(4) 0.5429(3) 0.7099(4) 0.0352(14) Uani 1 1 d . . . C5S C 0.0348(4) 0.6403(3) 0.4119(3) 0.0358(13) Uani 1 1 d . . . C6S C 0.1474(4) 0.6237(3) 0.3857(3) 0.0396(14) Uani 1 1 d . . . H6S1 H 0.1798 0.6725 0.3639 0.048 Uiso 1 1 calc R . . H6S2 H 0.1422 0.6111 0.3435 0.048 Uiso 1 1 calc R . . C7S C 0.2214(4) 0.5543(3) 0.4529(3) 0.0403(14) Uani 1 1 d . . . H7S1 H 0.2932 0.5508 0.4327 0.048 Uiso 1 1 calc R . . H7S2 H 0.2261 0.5669 0.4953 0.048 Uiso 1 1 calc R . . C8S C 0.1855(4) 0.4729(3) 0.4877(4) 0.0353(13) Uani 1 1 d . . . N1 N 0.0455(3) 0.2277(2) 0.9058(3) 0.0388(11) Uani 1 1 d . . . N2 N 0.1946(4) 0.1883(2) 1.0202(3) 0.0392(11) Uani 1 1 d . . . N3 N 0.2240(3) 0.0982(2) 0.9223(2) 0.0384(11) Uani 1 1 d . . . N4 N 0.3653(3) 0.1993(2) 0.8747(2) 0.0394(11) Uani 1 1 d . . . N5 N 0.2167(3) 0.1926(2) 0.6893(2) 0.0369(11) Uani 1 1 d . . . N6 N 0.3559(3) 0.2950(3) 0.6269(2) 0.0396(11) Uani 1 1 d . . . N7 N -0.0714(4) 0.7602(3) 0.4844(2) 0.0416(12) Uani 1 1 d . . . N8 N -0.2510(3) 0.6991(3) 0.5383(2) 0.0394(11) Uani 1 1 d . . . N9 N -0.1089(3) 0.7696(2) 0.6889(2) 0.0360(11) Uani 1 1 d . . . N10 N -0.2431(3) 0.6633(3) 0.7501(3) 0.0430(12) Uani 1 1 d . . . N11 N -0.0950(4) 0.6325(2) 0.8831(3) 0.0416(12) Uani 1 1 d . . . N12 N 0.0721(3) 0.6358(2) 0.7890(3) 0.0395(11) Uani 1 1 d . . . C1 C -0.0286(5) 0.2505(3) 0.8492(4) 0.0511(16) Uani 1 1 d . . . H1 H -0.0057 0.2574 0.7999 0.061 Uiso 1 1 calc R . . C2 C -0.1377(5) 0.2644(3) 0.8596(4) 0.0602(18) Uani 1 1 d . . . H2 H -0.1867 0.2826 0.8175 0.072 Uiso 1 1 calc R . . C3 C -0.1719(5) 0.2512(3) 0.9312(4) 0.0544(17) Uani 1 1 d . . . H3 H -0.2455 0.2596 0.9389 0.065 Uiso 1 1 calc R . . C4 C -0.0990(5) 0.2251(3) 0.9948(4) 0.0440(14) Uani 1 1 d . . . C5 C 0.0094(4) 0.2154(3) 0.9789(3) 0.0374(13) Uani 1 1 d . . . C6 C -0.1299(5) 0.2081(3) 1.0730(4) 0.0596(18) Uani 1 1 d . . . H6 H -0.2027 0.2149 1.0836 0.071 Uiso 1 1 calc R . . C7 C -0.0568(6) 0.1829(4) 1.1310(4) 0.0656(19) Uani 1 1 d . . . H7 H -0.0790 0.1699 1.1822 0.079 Uiso 1 1 calc R . . C8 C 0.0554(5) 0.1755(3) 1.1156(4) 0.0502(16) Uani 1 1 d . . . C9 C 0.0902(4) 0.1918(3) 1.0399(3) 0.0386(14) Uani 1 1 d . . . C10 C 0.1374(6) 0.1514(3) 1.1734(4) 0.0642(19) Uani 1 1 d . . . H10 H 0.1191 0.1361 1.2257 0.077 Uiso 1 1 calc R . . C11 C 0.2432(5) 0.1500(3) 1.1537(4) 0.0599(18) Uani 1 1 d . . . H11 H 0.2972 0.1368 1.1912 0.072 Uiso 1 1 calc R . . C12 C 0.2675(5) 0.1693(3) 1.0755(4) 0.0531(17) Uani 1 1 d . . . H12 H 0.3396 0.1686 1.0618 0.064 Uiso 1 1 calc R . . C13 C 0.1535(5) 0.0476(3) 0.9487(3) 0.0544(17) Uani 1 1 d . . . H13 H 0.0822 0.0671 0.9529 0.065 Uiso 1 1 calc R . . C14 C 0.1811(5) -0.0337(3) 0.9706(4) 0.0624(18) Uani 1 1 d . . . H14 H 0.1288 -0.0673 0.9897 0.075 Uiso 1 1 calc R . . C15 C 0.2837(5) -0.0638(3) 0.9643(3) 0.0585(17) Uani 1 1 d . . . H15 H 0.3028 -0.1181 0.9792 0.070 Uiso 1 1 calc R . . C16 C 0.3609(4) -0.0115(3) 0.9347(3) 0.0411(14) Uani 1 1 d . . . C17 C 0.3290(4) 0.0692(3) 0.9161(3) 0.0364(13) Uani 1 1 d . . . C18 C 0.4718(5) -0.0362(4) 0.9257(3) 0.0557(17) Uani 1 1 d . . . H18 H 0.4957 -0.0899 0.9399 0.067 Uiso 1 1 calc R . . C19 C 0.5418(5) 0.0160(4) 0.8973(3) 0.0550(17) Uani 1 1 d . . . H19 H 0.6128 -0.0018 0.8904 0.066 Uiso 1 1 calc R . . C20 C 0.5107(4) 0.0977(4) 0.8774(3) 0.0458(15) Uani 1 1 d . . . C21 C 0.4032(4) 0.1233(3) 0.8889(3) 0.0386(14) Uani 1 1 d . . . C22 C 0.5787(5) 0.1565(4) 0.8487(3) 0.0586(18) Uani 1 1 d . . . H22 H 0.6505 0.1433 0.8394 0.070 Uiso 1 1 calc R . . C23 C 0.5404(5) 0.2317(4) 0.8347(4) 0.0619(18) Uani 1 1 d . . . H23 H 0.5857 0.2705 0.8158 0.074 Uiso 1 1 calc R . . C24 C 0.4314(5) 0.2518(3) 0.8486(4) 0.0598(18) Uani 1 1 d . . . H24 H 0.4061 0.3040 0.8388 0.072 Uiso 1 1 calc R . . C25 C 0.1460(4) 0.1417(3) 0.7229(3) 0.0440(15) Uani 1 1 d . . . H25 H 0.0741 0.1627 0.7235 0.053 Uiso 1 1 calc R . . C26 C 0.1753(5) 0.0578(3) 0.7574(3) 0.0518(16) Uani 1 1 d . . . H26 H 0.1238 0.0240 0.7810 0.062 Uiso 1 1 calc R . . C27 C 0.2792(5) 0.0266(3) 0.7561(3) 0.0539(17) Uani 1 1 d . . . H27 H 0.2990 -0.0291 0.7784 0.065 Uiso 1 1 calc R . . C28 C 0.3569(5) 0.0769(3) 0.7218(3) 0.0460(15) Uani 1 1 d . . . C29 C 0.3211(4) 0.1598(3) 0.6893(3) 0.0354(13) Uani 1 1 d . . . C30 C 0.4681(5) 0.0490(4) 0.7190(4) 0.0564(17) Uani 1 1 d . . . H30 H 0.4917 -0.0061 0.7402 0.068 Uiso 1 1 calc R . . C31 C 0.5389(5) 0.0997(4) 0.6871(4) 0.0631(19) Uani 1 1 d . . . H31 H 0.6108 0.0796 0.6854 0.076 Uiso 1 1 calc R . . C32 C 0.5064(4) 0.1856(4) 0.6547(3) 0.0494(16) Uani 1 1 d . . . C33 C 0.3964(4) 0.2139(3) 0.6563(3) 0.0382(14) Uani 1 1 d . . . C34 C 0.5736(5) 0.2439(4) 0.6224(4) 0.068(2) Uani 1 1 d . . . H34 H 0.6471 0.2280 0.6204 0.082 Uiso 1 1 calc R . . C35 C 0.5347(5) 0.3239(4) 0.5935(4) 0.074(2) Uani 1 1 d . . . H35 H 0.5806 0.3623 0.5715 0.089 Uiso 1 1 calc R . . C36 C 0.4240(5) 0.3470(4) 0.5976(3) 0.0580(17) Uani 1 1 d . . . H36 H 0.3976 0.4014 0.5788 0.070 Uiso 1 1 calc R . . C37 C 0.0190(5) 0.7894(4) 0.4587(4) 0.0615(18) Uani 1 1 d . . . H37 H 0.0820 0.7535 0.4656 0.074 Uiso 1 1 calc R . . C38 C 0.0247(7) 0.8712(5) 0.4217(4) 0.079(2) Uani 1 1 d . . . H38 H 0.0903 0.8895 0.4047 0.095 Uiso 1 1 calc R . . C39 C -0.0656(8) 0.9237(4) 0.4109(4) 0.086(3) Uani 1 1 d . . . H39 H -0.0629 0.9789 0.3838 0.104 Uiso 1 1 calc R . . C40 C -0.1633(7) 0.8968(4) 0.4398(4) 0.0626(19) Uani 1 1 d . . . C41 C -0.1625(5) 0.8132(3) 0.4765(3) 0.0427(15) Uani 1 1 d . . . C42 C -0.2627(8) 0.9479(4) 0.4327(4) 0.083(3) Uani 1 1 d . . . H42 H -0.2645 1.0035 0.4075 0.099 Uiso 1 1 calc R . . C43 C -0.3519(7) 0.9177(4) 0.4609(4) 0.080(3) Uani 1 1 d . . . H43 H -0.4154 0.9522 0.4566 0.097 Uiso 1 1 calc R . . C44 C -0.3530(5) 0.8323(4) 0.4985(3) 0.0514(17) Uani 1 1 d . . . C45 C -0.2580(4) 0.7803(3) 0.5057(3) 0.0403(14) Uani 1 1 d . . . C46 C -0.4433(6) 0.7972(5) 0.5276(4) 0.077(2) Uani 1 1 d . . . H46 H -0.5088 0.8295 0.5236 0.093 Uiso 1 1 calc R . . C47 C -0.4387(5) 0.7153(5) 0.5624(4) 0.073(2) Uani 1 1 d . . . H47 H -0.5003 0.6919 0.5826 0.088 Uiso 1 1 calc R . . C48 C -0.3398(5) 0.6672(4) 0.5674(3) 0.0567(17) Uani 1 1 d . . . H48 H -0.3364 0.6115 0.5917 0.068 Uiso 1 1 calc R . . C49 C -0.0408(5) 0.8213(4) 0.6518(3) 0.0482(15) Uani 1 1 d . . . H49 H 0.0322 0.8010 0.6549 0.058 Uiso 1 1 calc R . . C50 C -0.0727(5) 0.9041(4) 0.6087(3) 0.0556(17) Uani 1 1 d . . . H50 H -0.0225 0.9384 0.5819 0.067 Uiso 1 1 calc R . . C51 C -0.1781(5) 0.9345(3) 0.6061(3) 0.0559(17) Uani 1 1 d . . . H51 H -0.2000 0.9902 0.5804 0.067 Uiso 1 1 calc R . . C52 C -0.2551(5) 0.8825(3) 0.6421(3) 0.0436(14) Uani 1 1 d . . . C53 C -0.2171(4) 0.7999(3) 0.6816(3) 0.0347(13) Uani 1 1 d . . . C54 C -0.3702(5) 0.9076(4) 0.6418(4) 0.0593(18) Uani 1 1 d . . . H54 H -0.3981 0.9624 0.6174 0.071 Uiso 1 1 calc R . . C55 C -0.4364(5) 0.8533(4) 0.6760(4) 0.0607(18) Uani 1 1 d . . . H55 H -0.5099 0.8710 0.6754 0.073 Uiso 1 1 calc R . . C56 C -0.3978(5) 0.7687(4) 0.7134(3) 0.0468(15) Uani 1 1 d . . . C57 C -0.2867(4) 0.7421(4) 0.7171(3) 0.0411(14) Uani 1 1 d . . . C58 C -0.4636(5) 0.7097(4) 0.7460(4) 0.0622(18) Uani 1 1 d . . . H58 H -0.5378 0.7246 0.7460 0.075 Uiso 1 1 calc R . . C59 C -0.4204(5) 0.6300(4) 0.7781(4) 0.0644(18) Uani 1 1 d . . . H59 H -0.4647 0.5905 0.7987 0.077 Uiso 1 1 calc R . . C60 C -0.3076(5) 0.6084(4) 0.7797(3) 0.0533(16) Uani 1 1 d . . . H60 H -0.2779 0.5540 0.8022 0.064 Uiso 1 1 calc R . . C61 C -0.1783(5) 0.6316(3) 0.9285(4) 0.0525(16) Uani 1 1 d . . . H61 H -0.2474 0.6422 0.9071 0.063 Uiso 1 1 calc R . . C62 C -0.1675(6) 0.6156(3) 1.0059(4) 0.0625(19) Uani 1 1 d . . . H62 H -0.2283 0.6173 1.0350 0.075 Uiso 1 1 calc R . . C63 C -0.0674(6) 0.5974(3) 1.0390(3) 0.0571(18) Uani 1 1 d . . . H63 H -0.0595 0.5841 1.0919 0.069 Uiso 1 1 calc R . . C64 C 0.0234(5) 0.5985(3) 0.9945(3) 0.0435(15) Uani 1 1 d . . . C65 C 0.0058(5) 0.6165(3) 0.9154(4) 0.0428(15) Uani 1 1 d . . . C66 C 0.1320(6) 0.5817(3) 1.0219(4) 0.0614(18) Uani 1 1 d . . . H66 H 0.1457 0.5702 1.0736 0.074 Uiso 1 1 calc R . . C67 C 0.2149(5) 0.5819(3) 0.9760(4) 0.0639(19) Uani 1 1 d . . . H67 H 0.2847 0.5696 0.9968 0.077 Uiso 1 1 calc R . . C68 C 0.1997(5) 0.6004(3) 0.8961(4) 0.0461(15) Uani 1 1 d . . . C69 C 0.0934(4) 0.6182(3) 0.8650(3) 0.0383(14) Uani 1 1 d . . . C70 C 0.2839(5) 0.6016(4) 0.8455(4) 0.0663(19) Uani 1 1 d . . . H70 H 0.3551 0.5909 0.8631 0.080 Uiso 1 1 calc R . . C71 C 0.2611(5) 0.6185(4) 0.7706(4) 0.0622(18) Uani 1 1 d . . . H71 H 0.3169 0.6184 0.7370 0.075 Uiso 1 1 calc R . . C72 C 0.1551(5) 0.6358(3) 0.7436(4) 0.0504(16) Uani 1 1 d . . . H72 H 0.1416 0.6480 0.6917 0.060 Uiso 1 1 calc R . . B1 B 0.8652(7) 0.0692(5) 0.7987(5) 0.095(3) Uani 1 1 d D . . F11 F 0.9251(3) 0.0325(3) 0.7652(3) 0.1177(16) Uani 1 1 d D A . F12 F 0.7781(8) 0.0418(8) 0.8295(8) 0.111(7) Uani 0.60 1 d PD A 1 F13 F 0.8525(10) 0.1467(6) 0.7537(8) 0.168(6) Uani 0.60 1 d PD A 1 F14 F 0.9360(10) 0.0527(8) 0.8590(6) 0.172(6) Uani 0.60 1 d PD A 1 F12A F 0.7830(13) 0.1133(12) 0.7400(7) 0.184(8) Uani 0.40 1 d PD A 2 F13A F 0.9095(17) 0.1174(14) 0.8091(14) 0.205(16) Uani 0.40 1 d PD A 2 F14A F 0.8132(11) 0.0211(10) 0.8602(9) 0.072(5) Uani 0.40 1 d PD A 2 B2 B 0.7429(7) 0.1570(5) 0.4418(5) 0.077(3) Uani 1 1 d D . . F21 F 0.8322(3) 0.1102(2) 0.4406(2) 0.0834(12) Uani 1 1 d D B . F24 F 0.7246(10) 0.1509(9) 0.5156(7) 0.173(7) Uani 0.60 1 d PD B 3 F22 F 0.6596(4) 0.1054(4) 0.4473(5) 0.0660(17) Uani 0.60 1 d P B 3 F23 F 0.6891(7) 0.2211(5) 0.3805(4) 0.087(3) Uani 0.60 1 d PD B 3 F23A F 0.7688(8) 0.2256(5) 0.4259(6) 0.080(3) Uani 0.40 1 d PD B 4 F22A F 0.6759(8) 0.1677(8) 0.3826(6) 0.083(4) Uani 0.40 1 d PD B 4 F24A F 0.6959(8) 0.1191(7) 0.5107(6) 0.069(4) Uani 0.40 1 d PD B 4 B3 B 0.4686(17) 0.4942(8) 0.6690(9) 0.249(16) Uani 1 1 d D . . F31 F 0.5215(7) 0.5039(4) 0.6078(5) 0.212(3) Uani 1 1 d D C . F34 F 0.4233(11) 0.4329(7) 0.7077(7) 0.116(3) Uani 0.60 1 d PD C 5 F33 F 0.4822(10) 0.5396(8) 0.6961(7) 0.121(4) Uani 0.60 1 d PD C 5 F32 F 0.5854(10) 0.4290(8) 0.7056(7) 0.173(4) Uani 0.60 1 d P C 5 F33A F 0.4102(18) 0.5587(13) 0.6606(12) 0.211(12) Uani 0.40 1 d PD C 6 F34A F 0.468(2) 0.4304(11) 0.7319(10) 0.33(3) Uani 0.40 1 d PD C 6 F32A F 0.5782(19) 0.5143(16) 0.7037(10) 0.203(10) Uani 0.40 1 d PD C 6 B4 B 0.5419(6) 0.2345(4) 0.0957(4) 0.0482(19) Uani 1 1 d D . . F41 F 0.5678(3) 0.2348(2) 0.0278(2) 0.0989(13) Uani 1 1 d D D . F43 F 0.6166(8) 0.2529(6) 0.1279(6) 0.086(4) Uani 0.60 1 d PD D 7 F44 F 0.5120(5) 0.1620(4) 0.1505(3) 0.0554(16) Uani 0.60 1 d PD D 7 F42 F 0.4465(9) 0.2934(5) 0.0763(7) 0.076(3) Uani 0.60 1 d P D 7 F42A F 0.4464(11) 0.2465(8) 0.1079(9) 0.083(5) Uani 0.40 1 d PD D 8 F44A F 0.5968(10) 0.1659(6) 0.1537(7) 0.127(5) Uani 0.40 1 d PD D 8 F43A F 0.5922(11) 0.2949(7) 0.0910(8) 0.073(5) Uani 0.40 1 d PD D 8 O1W O 0.7605(7) 0.1525(4) 0.2750(5) 0.245(4) Uani 1 1 d . . . O2W O 0.2620(6) 0.6642(5) 0.5498(5) 0.220(3) Uani 1 1 d . . . O3W O 0.4826(8) 0.4500(5) 0.9649(7) 0.320(6) Uani 1 1 d . . . O4W O 0.6104(8) 0.4165(5) 0.8701(6) 0.257(4) Uani 1 1 d . . . 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 0.0377(4) 0.0368(4) 0.0414(5) -0.0197(4) 0.0015(3) 0.0013(3) Cu2 0.0374(4) 0.0366(4) 0.0362(4) -0.0191(4) 0.0003(3) -0.0023(3) Cu3 0.0371(4) 0.0364(4) 0.0382(4) -0.0212(4) 0.0043(3) -0.0030(3) Cu4 0.0364(4) 0.0428(4) 0.0518(5) -0.0279(4) 0.0057(3) -0.0051(3) O1 0.052(2) 0.039(2) 0.029(2) -0.019(2) -0.0008(19) 0.0047(18) O2 0.056(2) 0.035(2) 0.030(2) -0.0175(19) -0.0030(18) 0.0050(18) O3 0.058(3) 0.039(2) 0.037(3) -0.020(2) 0.003(2) -0.0006(19) O4 0.060(3) 0.031(2) 0.034(2) -0.017(2) -0.0020(19) 0.0004(19) O5 0.039(2) 0.056(3) 0.037(2) -0.024(2) -0.0016(18) 0.0048(18) O6 0.040(2) 0.043(2) 0.040(2) -0.012(2) -0.0088(19) 0.0068(19) O7 0.051(2) 0.034(2) 0.040(3) -0.013(2) -0.001(2) -0.0101(18) O8 0.061(3) 0.033(2) 0.044(3) -0.022(2) -0.003(2) -0.0104(18) C1S 0.029(3) 0.028(3) 0.059(4) -0.028(3) 0.004(3) 0.003(2) C2S 0.050(4) 0.035(3) 0.044(4) -0.024(3) 0.001(3) 0.000(3) C3S 0.073(5) 0.027(3) 0.084(5) -0.036(3) -0.028(4) 0.001(3) C4S 0.033(3) 0.029(3) 0.057(4) -0.031(3) -0.005(3) -0.001(3) C5S 0.040(4) 0.029(3) 0.038(4) -0.015(3) 0.005(3) -0.014(3) C6S 0.034(3) 0.042(3) 0.050(4) -0.028(3) 0.011(3) -0.010(3) C7S 0.025(3) 0.056(4) 0.047(4) -0.031(3) 0.001(3) -0.004(3) C8S 0.023(3) 0.028(3) 0.047(4) -0.014(3) 0.010(3) -0.002(2) N1 0.031(3) 0.037(3) 0.047(3) -0.021(3) 0.003(2) -0.002(2) N2 0.041(3) 0.036(3) 0.040(3) -0.021(2) 0.001(2) 0.002(2) N3 0.042(3) 0.036(3) 0.038(3) -0.019(2) 0.007(2) -0.005(2) N4 0.048(3) 0.027(3) 0.038(3) -0.012(2) -0.003(2) -0.003(2) N5 0.037(3) 0.043(3) 0.037(3) -0.025(2) 0.000(2) -0.003(2) N6 0.036(3) 0.043(3) 0.042(3) -0.021(3) 0.008(2) -0.013(2) N7 0.045(3) 0.050(3) 0.035(3) -0.022(3) 0.000(2) -0.015(3) N8 0.039(3) 0.049(3) 0.035(3) -0.025(3) 0.005(2) -0.006(2) N9 0.037(3) 0.040(3) 0.036(3) -0.023(2) 0.008(2) -0.008(2) N10 0.040(3) 0.044(3) 0.051(3) -0.027(3) 0.007(2) -0.013(2) N11 0.042(3) 0.040(3) 0.048(3) -0.026(3) 0.012(2) -0.005(2) N12 0.037(3) 0.041(3) 0.047(3) -0.027(3) 0.003(2) -0.005(2) C1 0.046(4) 0.055(4) 0.054(4) -0.029(4) -0.004(3) -0.004(3) C2 0.041(4) 0.058(4) 0.063(5) -0.016(4) -0.014(3) -0.005(3) C3 0.034(4) 0.056(4) 0.074(5) -0.030(4) 0.013(4) -0.019(3) C4 0.048(4) 0.033(3) 0.053(4) -0.021(3) 0.012(3) -0.015(3) C5 0.038(3) 0.029(3) 0.042(4) -0.017(3) 0.004(3) -0.002(3) C6 0.046(4) 0.058(4) 0.077(5) -0.034(4) 0.019(4) -0.014(3) C7 0.076(5) 0.064(5) 0.061(5) -0.031(4) 0.031(4) -0.032(4) C8 0.057(4) 0.045(4) 0.047(4) -0.022(3) 0.007(4) -0.010(3) C9 0.046(4) 0.026(3) 0.045(4) -0.020(3) -0.004(3) 0.000(3) C10 0.091(5) 0.062(4) 0.046(5) -0.030(4) 0.022(4) -0.020(4) C11 0.066(5) 0.072(5) 0.044(4) -0.032(4) -0.007(4) -0.004(4) C12 0.041(4) 0.057(4) 0.067(5) -0.039(4) -0.006(3) 0.007(3) C13 0.045(4) 0.045(4) 0.074(5) -0.030(4) 0.016(3) -0.010(3) C14 0.060(4) 0.042(4) 0.078(5) -0.024(4) 0.014(4) -0.015(3) C15 0.074(5) 0.037(4) 0.060(5) -0.022(3) 0.001(4) -0.002(4) C16 0.046(4) 0.035(3) 0.040(4) -0.019(3) -0.001(3) 0.001(3) C17 0.036(3) 0.044(4) 0.028(3) -0.019(3) -0.001(3) 0.003(3) C18 0.065(5) 0.042(4) 0.054(4) -0.023(4) -0.004(4) 0.006(3) C19 0.047(4) 0.052(4) 0.065(5) -0.035(4) 0.012(3) 0.012(3) C20 0.039(4) 0.055(4) 0.045(4) -0.025(3) 0.007(3) -0.009(3) C21 0.043(4) 0.036(3) 0.030(3) -0.013(3) -0.001(3) 0.003(3) C22 0.046(4) 0.057(4) 0.064(5) -0.029(4) 0.001(3) 0.010(3) C23 0.033(4) 0.058(4) 0.079(5) -0.021(4) 0.000(3) -0.013(3) C24 0.062(5) 0.039(4) 0.074(5) -0.024(4) -0.005(4) -0.007(3) C25 0.036(3) 0.060(4) 0.048(4) -0.034(4) 0.002(3) -0.015(3) C26 0.059(4) 0.037(4) 0.056(4) -0.019(3) -0.005(3) -0.012(3) C27 0.070(5) 0.031(4) 0.056(4) -0.019(3) 0.003(4) -0.007(3) C28 0.057(4) 0.034(3) 0.041(4) -0.018(3) -0.004(3) 0.006(3) C29 0.033(3) 0.047(4) 0.031(3) -0.024(3) 0.001(3) -0.004(3) C30 0.053(4) 0.055(4) 0.065(5) -0.035(4) 0.001(4) 0.002(4) C31 0.053(4) 0.053(4) 0.080(5) -0.037(4) 0.000(4) 0.015(4) C32 0.033(3) 0.075(5) 0.046(4) -0.034(4) 0.013(3) -0.015(3) C33 0.037(3) 0.047(4) 0.036(4) -0.027(3) 0.003(3) -0.003(3) C34 0.034(4) 0.086(5) 0.088(6) -0.047(5) -0.002(4) 0.001(4) C35 0.040(4) 0.090(6) 0.106(6) -0.054(5) 0.017(4) -0.032(4) C36 0.057(4) 0.061(4) 0.064(5) -0.035(4) -0.002(4) -0.016(4) C37 0.058(4) 0.074(5) 0.063(5) -0.041(4) -0.003(4) -0.011(4) C38 0.093(6) 0.086(6) 0.072(6) -0.036(5) 0.008(5) -0.068(5) C39 0.140(8) 0.061(5) 0.070(6) -0.036(5) -0.016(6) -0.030(6) C40 0.098(6) 0.041(4) 0.050(5) -0.021(4) -0.012(4) -0.016(4) C41 0.057(4) 0.040(4) 0.037(4) -0.025(3) -0.009(3) 0.000(3) C42 0.134(8) 0.051(5) 0.065(6) -0.036(5) -0.033(6) 0.017(6) C43 0.112(7) 0.055(6) 0.063(6) -0.034(5) -0.041(5) 0.047(5) C44 0.049(4) 0.066(5) 0.042(4) -0.034(4) -0.009(3) 0.012(4) C45 0.045(4) 0.041(4) 0.037(4) -0.023(3) -0.002(3) 0.003(3) C46 0.069(5) 0.094(6) 0.074(6) -0.056(5) -0.008(4) 0.028(5) C47 0.029(4) 0.133(7) 0.069(5) -0.060(5) 0.020(3) -0.012(4) C48 0.058(4) 0.074(5) 0.052(4) -0.040(4) 0.023(3) -0.021(4) C49 0.050(4) 0.052(4) 0.051(4) -0.031(4) 0.008(3) -0.013(3) C50 0.056(4) 0.047(4) 0.062(5) -0.023(4) 0.005(3) -0.018(3) C51 0.087(5) 0.027(3) 0.044(4) -0.011(3) -0.007(4) -0.007(4) C52 0.059(4) 0.043(4) 0.034(4) -0.023(3) 0.003(3) -0.009(3) C53 0.043(4) 0.043(4) 0.031(3) -0.027(3) 0.007(3) -0.012(3) C54 0.064(5) 0.049(4) 0.064(5) -0.034(4) -0.014(4) 0.019(4) C55 0.041(4) 0.070(5) 0.070(5) -0.037(4) 0.000(4) 0.001(4) C56 0.042(4) 0.065(4) 0.043(4) -0.033(4) 0.004(3) -0.014(3) C57 0.047(4) 0.054(4) 0.029(4) -0.026(3) 0.003(3) -0.005(3) C58 0.039(4) 0.081(5) 0.063(5) -0.037(4) 0.003(3) 0.002(4) C59 0.051(4) 0.087(5) 0.064(5) -0.039(4) 0.018(3) -0.035(4) C60 0.054(4) 0.050(4) 0.058(4) -0.026(4) 0.004(3) -0.018(3) C61 0.050(4) 0.057(4) 0.056(5) -0.034(4) 0.018(3) -0.010(3) C62 0.078(5) 0.059(4) 0.055(5) -0.033(4) 0.028(4) -0.013(4) C63 0.101(6) 0.039(4) 0.031(4) -0.017(3) 0.020(4) -0.019(4) C64 0.068(4) 0.024(3) 0.040(4) -0.017(3) 0.000(3) -0.009(3) C65 0.046(4) 0.027(3) 0.056(4) -0.021(3) 0.006(3) -0.008(3) C66 0.087(5) 0.047(4) 0.050(5) -0.023(4) -0.017(4) -0.004(4) C67 0.060(5) 0.057(4) 0.067(5) -0.025(4) -0.020(4) -0.003(4) C68 0.043(4) 0.043(4) 0.047(4) -0.016(3) -0.002(3) -0.013(3) C69 0.038(3) 0.029(3) 0.046(4) -0.016(3) 0.001(3) -0.005(3) C70 0.031(4) 0.081(5) 0.090(6) -0.046(5) 0.002(4) -0.005(3) C71 0.036(4) 0.083(5) 0.073(5) -0.042(4) 0.014(3) -0.013(3) C72 0.049(4) 0.056(4) 0.057(4) -0.036(4) 0.010(3) -0.013(3) B1 0.064(8) 0.095(9) 0.106(11) -0.041(9) 0.007(7) 0.004(7) F11 0.100(3) 0.131(4) 0.125(4) -0.067(3) 0.038(3) -0.029(3) F12 0.044(6) 0.112(10) 0.217(18) -0.110(12) 0.036(8) -0.024(6) F13 0.136(12) 0.128(8) 0.270(19) -0.116(10) -0.022(10) -0.031(8) F14 0.136(10) 0.243(16) 0.129(10) -0.078(10) 0.017(7) -0.061(10) F12A 0.163(16) 0.212(19) 0.072(10) -0.011(12) -0.011(10) 0.041(14) F13A 0.20(3) 0.31(4) 0.28(4) -0.24(3) 0.13(3) -0.20(3) F14A 0.051(10) 0.093(10) 0.080(9) -0.048(8) 0.044(9) -0.029(9) B2 0.074(7) 0.068(7) 0.057(7) -0.011(6) -0.005(6) 0.008(6) F21 0.047(2) 0.087(3) 0.100(3) -0.036(2) 0.009(2) -0.009(2) F24 0.143(11) 0.229(16) 0.178(13) -0.128(12) -0.027(9) -0.008(9) F22 0.038(3) 0.073(5) 0.113(6) -0.066(5) 0.011(4) -0.012(3) F23 0.092(6) 0.056(5) 0.079(6) -0.007(5) -0.002(4) -0.012(5) F23A 0.119(9) 0.029(5) 0.069(8) -0.003(5) -0.011(7) -0.019(5) F22A 0.081(8) 0.072(8) 0.058(8) 0.004(8) -0.007(6) -0.034(8) F24A 0.053(7) 0.067(7) 0.039(8) 0.001(6) -0.002(5) 0.019(6) B3 0.37(4) 0.154(18) 0.30(3) -0.18(2) 0.25(3) -0.12(3) F31 0.244(8) 0.184(7) 0.236(9) -0.125(7) 0.074(7) -0.054(6) F34 0.140(8) 0.106(9) 0.114(8) -0.058(7) 0.036(6) -0.046(6) F33 0.101(9) 0.133(10) 0.172(11) -0.107(9) 0.032(9) -0.029(8) F32 0.199(12) 0.166(10) 0.152(11) -0.077(9) 0.054(9) -0.051(10) F33A 0.17(2) 0.148(17) 0.27(3) -0.092(18) 0.086(18) 0.008(15) F34A 0.30(4) 0.12(2) 0.42(5) -0.01(2) 0.11(3) -0.11(2) F32A 0.28(3) 0.22(2) 0.190(18) -0.133(17) 0.090(19) -0.18(2) B4 0.038(5) 0.052(5) 0.074(6) -0.046(5) 0.010(4) -0.009(4) F41 0.115(3) 0.103(3) 0.092(3) -0.060(3) 0.026(3) -0.017(3) F43 0.066(5) 0.122(10) 0.104(9) -0.078(8) 0.017(5) -0.028(7) F44 0.057(4) 0.052(4) 0.058(4) -0.028(4) 0.010(3) -0.011(4) F42 0.063(5) 0.059(6) 0.106(8) -0.046(6) 0.007(5) 0.007(5) F42A 0.053(8) 0.122(15) 0.098(13) -0.073(12) 0.010(8) -0.013(11) F44A 0.113(11) 0.070(9) 0.176(14) -0.048(9) 0.016(10) 0.001(9) F43A 0.081(10) 0.061(9) 0.100(12) -0.050(9) 0.020(8) -0.042(8) O1W 0.223(9) 0.164(7) 0.280(10) -0.070(7) 0.055(7) -0.014(6) O2W 0.196(8) 0.252(9) 0.243(9) -0.145(8) 0.001(7) -0.037(7) O3W 0.211(9) 0.210(10) 0.374(15) -0.027(9) -0.031(9) 0.000(8) O4W 0.290(11) 0.169(7) 0.261(10) -0.061(7) -0.070(9) -0.035(7) _geom_special_details ; #--------------------------------------------------------------------- As usual all the BF4 moieties are having orientational disorder. In all three cases, B1,B2,B3 and the following three F atoms (F11,F21,F31) are not disordered. But, all other F atoms are found to be disordered. The two groups of F atoms around B1 (F12,F13,F14/F12A,F13A,F14A), around B2 (F22,F23,F24/ F22A,F23A,F24A) and around B3 (F32,F33,F34/ F32A,F33A,F34A) occupy two orientation with occupancy ratio 0.6/0.4. H-atoms on water oxygens could not be located from difference map. #---------------------------------------------------------------------- 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 1.979(3) . ? Cu1 N4 2.002(4) . ? Cu1 N1 2.028(4) . ? Cu1 N3 2.037(4) . ? Cu1 N2 2.208(4) . ? Cu2 O7 1.948(3) . ? Cu2 O6 1.959(3) 2_566 ? Cu2 N6 2.019(4) . ? Cu2 N5 2.026(4) . ? Cu2 O2 2.142(3) . ? Cu3 O8 1.946(3) 2_566 ? Cu3 O5 1.948(3) . ? Cu3 N8 2.011(4) . ? Cu3 N7 2.030(4) . ? Cu3 O4 2.160(3) . ? Cu4 O3 1.976(3) . ? Cu4 N10 1.992(4) . ? Cu4 N12 1.998(4) . ? Cu4 N9 2.055(4) . ? Cu4 N11 2.204(4) . ? O1 C1S 1.256(6) . ? O2 C1S 1.256(5) . ? O3 C4S 1.258(6) . ? O4 C4S 1.248(6) . ? O5 C5S 1.272(6) . ? O6 C5S 1.235(5) . ? O6 Cu2 1.959(3) 2_566 ? O7 C8S 1.264(6) . ? O8 C8S 1.246(6) . ? O8 Cu3 1.946(3) 2_566 ? C1S C2S 1.503(6) . ? C2S C3S 1.550(7) . ? C3S C4S 1.516(6) . ? C5S C6S 1.515(6) . ? C6S C7S 1.530(6) . ? C7S C8S 1.508(6) . ? N1 C1 1.324(6) . ? N1 C5 1.376(6) . ? N2 C12 1.314(6) . ? N2 C9 1.347(6) . ? N3 C13 1.319(6) . ? N3 C17 1.371(6) . ? N4 C24 1.302(6) . ? N4 C21 1.356(6) . ? N5 C25 1.329(6) . ? N5 C29 1.361(6) . ? N6 C36 1.314(6) . ? N6 C33 1.384(6) . ? N7 C37 1.314(7) . ? N7 C41 1.366(6) . ? N8 C48 1.325(6) . ? N8 C45 1.357(6) . ? N9 C49 1.321(6) . ? N9 C53 1.375(6) . ? N10 C60 1.318(6) . ? N10 C57 1.350(6) . ? N11 C61 1.327(6) . ? N11 C65 1.363(6) . ? N12 C72 1.326(6) . ? N12 C69 1.364(6) . ? C1 C2 1.378(7) . ? C2 C3 1.336(7) . ? C3 C4 1.402(7) . ? C4 C5 1.384(7) . ? C4 C6 1.424(7) . ? C5 C9 1.441(7) . ? C6 C7 1.328(7) . ? C7 C8 1.425(8) . ? C8 C9 1.396(7) . ? C8 C10 1.407(8) . ? C10 C11 1.363(8) . ? C11 C12 1.395(7) . ? C13 C14 1.391(7) . ? C14 C15 1.351(7) . ? C15 C16 1.406(7) . ? C16 C17 1.403(7) . ? C16 C18 1.428(7) . ? C17 C21 1.400(7) . ? C18 C19 1.335(7) . ? C19 C20 1.413(7) . ? C20 C22 1.403(7) . ? C20 C21 1.407(7) . ? C22 C23 1.345(7) . ? C23 C24 1.410(7) . ? C25 C26 1.400(7) . ? C26 C27 1.350(7) . ? C27 C28 1.393(7) . ? C28 C29 1.396(6) . ? C28 C30 1.422(7) . ? C29 C33 1.412(7) . ? C30 C31 1.326(7) . ? C31 C32 1.442(7) . ? C32 C34 1.389(8) . ? C32 C33 1.405(7) . ? C34 C35 1.363(8) . ? C35 C36 1.401(7) . ? C37 C38 1.387(8) . ? C38 C39 1.340(9) . ? C39 C40 1.392(9) . ? C40 C41 1.401(7) . ? C40 C42 1.426(9) . ? C41 C45 1.409(7) . ? C42 C43 1.315(9) . ? C43 C44 1.436(9) . ? C44 C46 1.367(8) . ? C44 C45 1.391(7) . ? C46 C47 1.368(8) . ? C47 C48 1.401(7) . ? C49 C50 1.384(7) . ? C50 C51 1.351(7) . ? C51 C52 1.408(7) . ? C52 C53 1.389(7) . ? C52 C54 1.448(7) . ? C53 C57 1.406(7) . ? C54 C55 1.330(7) . ? C55 C56 1.424(7) . ? C56 C58 1.385(8) . ? C56 C57 1.400(7) . ? C58 C59 1.364(7) . ? C59 C60 1.409(7) . ? C61 C62 1.378(7) . ? C62 C63 1.356(8) . ? C63 C64 1.389(7) . ? C64 C65 1.411(7) . ? C64 C66 1.419(7) . ? C65 C69 1.424(7) . ? C66 C67 1.331(8) . ? C67 C68 1.418(7) . ? C68 C70 1.396(7) . ? C68 C69 1.414(7) . ? C70 C71 1.354(8) . ? C71 C72 1.384(7) . ? B1 F13A 1.259(12) . ? B1 F12 1.281(11) . ? B1 F13 1.289(11) . ? B1 F14A 1.312(12) . ? B1 F11 1.310(8) . ? B1 F14 1.381(11) . ? B1 F12A 1.400(12) . ? B2 F23A 1.297(10) . ? B2 F23 1.323(8) . ? B2 F24A 1.322(11) . ? B2 F21 1.327(7) . ? B2 F22A 1.369(13) . ? B2 F24 1.381(11) . ? B2 F22 1.524(11) . ? B3 F34A 1.229(14) . ? B3 F34 1.256(12) . ? B3 F33 1.259(12) . ? B3 F31 1.270(10) . ? B3 F33A 1.276(12) . ? B3 F32 1.69(2) . ? B3 F32A 1.74(3) . ? B4 F42A 1.219(15) . ? B4 F41 1.332(7) . ? B4 F44A 1.340(10) . ? B4 F43 1.338(9) . ? B4 F44 1.371(8) . ? B4 F43A 1.378(11) . ? B4 F42 1.432(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 O1 Cu1 N4 93.86(16) . . ? O1 Cu1 N1 89.29(15) . . ? N4 Cu1 N1 172.77(18) . . ? O1 Cu1 N3 169.35(15) . . ? N4 Cu1 N3 81.79(17) . . ? N1 Cu1 N3 93.98(17) . . ? O1 Cu1 N2 96.06(14) . . ? N4 Cu1 N2 106.92(17) . . ? N1 Cu1 N2 79.17(17) . . ? N3 Cu1 N2 94.52(15) . . ? O7 Cu2 O6 96.11(14) . 2_566 ? O7 Cu2 N6 89.82(16) . . ? O6 Cu2 N6 171.78(16) 2_566 . ? O7 Cu2 N5 166.49(16) . . ? O6 Cu2 N5 91.72(16) 2_566 . ? N6 Cu2 N5 81.40(18) . . ? O7 Cu2 O2 97.18(14) . . ? O6 Cu2 O2 87.98(14) 2_566 . ? N6 Cu2 O2 96.95(15) . . ? N5 Cu2 O2 94.08(14) . . ? O8 Cu3 O5 91.00(15) 2_566 . ? O8 Cu3 N8 92.21(17) 2_566 . ? O5 Cu3 N8 161.69(15) . . ? O8 Cu3 N7 170.16(16) 2_566 . ? O5 Cu3 N7 92.54(17) . . ? N8 Cu3 N7 81.62(19) . . ? O8 Cu3 O4 95.89(14) 2_566 . ? O5 Cu3 O4 100.26(13) . . ? N8 Cu3 O4 97.33(14) . . ? N7 Cu3 O4 92.52(15) . . ? O3 Cu4 N10 96.54(17) . . ? O3 Cu4 N12 89.93(15) . . ? N10 Cu4 N12 170.22(17) . . ? O3 Cu4 N9 149.55(15) . . ? N10 Cu4 N9 81.39(18) . . ? N12 Cu4 N9 96.71(17) . . ? O3 Cu4 N11 107.08(15) . . ? N10 Cu4 N11 91.60(17) . . ? N12 Cu4 N11 79.46(17) . . ? N9 Cu4 N11 103.35(15) . . ? C1S O1 Cu1 104.8(3) . . ? C1S O2 Cu2 145.0(4) . . ? C4S O3 Cu4 107.6(3) . . ? C4S O4 Cu3 130.8(3) . . ? C5S O5 Cu3 121.4(3) . . ? C5S O6 Cu2 130.9(4) . 2_566 ? C8S O7 Cu2 132.1(3) . . ? C8S O8 Cu3 124.1(4) . 2_566 ? O2 C1S O1 121.7(5) . . ? O2 C1S C2S 120.2(5) . . ? O1 C1S C2S 117.9(5) . . ? C1S C2S C3S 109.1(4) . . ? C4S C3S C2S 110.1(4) . . ? O4 C4S O3 121.5(4) . . ? O4 C4S C3S 121.9(5) . . ? O3 C4S C3S 116.6(5) . . ? O6 C5S O5 127.3(5) . . ? O6 C5S C6S 117.7(5) . . ? O5 C5S C6S 114.9(5) . . ? C5S C6S C7S 113.8(4) . . ? C8S C7S C6S 114.5(4) . . ? O8 C8S O7 127.7(5) . . ? O8 C8S C7S 116.6(5) . . ? O7 C8S C7S 115.7(5) . . ? C1 N1 C5 117.1(5) . . ? C1 N1 Cu1 127.2(4) . . ? C5 N1 Cu1 115.5(4) . . ? C12 N2 C9 117.7(5) . . ? C12 N2 Cu1 132.2(4) . . ? C9 N2 Cu1 110.1(4) . . ? C13 N3 C17 118.3(5) . . ? C13 N3 Cu1 130.7(4) . . ? C17 N3 Cu1 110.8(4) . . ? C24 N4 C21 118.6(5) . . ? C24 N4 Cu1 128.4(4) . . ? C21 N4 Cu1 113.1(4) . . ? C25 N5 C29 117.1(5) . . ? C25 N5 Cu2 130.0(4) . . ? C29 N5 Cu2 112.9(4) . . ? C36 N6 C33 118.1(5) . . ? C36 N6 Cu2 129.5(4) . . ? C33 N6 Cu2 112.4(3) . . ? C37 N7 C41 117.8(5) . . ? C37 N7 Cu3 130.4(4) . . ? C41 N7 Cu3 111.7(4) . . ? C48 N8 C45 117.6(5) . . ? C48 N8 Cu3 129.8(4) . . ? C45 N8 Cu3 112.6(4) . . ? C49 N9 C53 118.0(5) . . ? C49 N9 Cu4 131.3(4) . . ? C53 N9 Cu4 110.6(3) . . ? C60 N10 C57 119.0(5) . . ? C60 N10 Cu4 128.1(4) . . ? C57 N10 Cu4 112.1(4) . . ? C61 N11 C65 117.6(5) . . ? C61 N11 Cu4 132.4(4) . . ? C65 N11 Cu4 109.8(4) . . ? C72 N12 C69 118.0(5) . . ? C72 N12 Cu4 126.7(4) . . ? C69 N12 Cu4 114.9(3) . . ? N1 C1 C2 123.5(6) . . ? C3 C2 C1 118.8(6) . . ? C2 C3 C4 121.3(6) . . ? C5 C4 C3 116.4(6) . . ? C5 C4 C6 119.3(6) . . ? C3 C4 C6 124.2(6) . . ? N1 C5 C4 122.7(5) . . ? N1 C5 C9 117.0(5) . . ? C4 C5 C9 120.3(5) . . ? C7 C6 C4 121.3(6) . . ? C6 C7 C8 120.5(6) . . ? C9 C8 C10 115.7(6) . . ? C9 C8 C7 120.5(6) . . ? C10 C8 C7 123.8(6) . . ? N2 C9 C8 124.0(5) . . ? N2 C9 C5 118.1(5) . . ? C8 C9 C5 117.9(5) . . ? C11 C10 C8 121.0(6) . . ? C10 C11 C12 117.7(6) . . ? N2 C12 C11 123.8(6) . . ? N3 C13 C14 123.0(5) . . ? C15 C14 C13 120.1(6) . . ? C14 C15 C16 118.8(5) . . ? C17 C16 C15 118.4(5) . . ? C17 C16 C18 117.5(5) . . ? C15 C16 C18 124.0(5) . . ? N3 C17 C21 117.6(5) . . ? N3 C17 C16 121.3(5) . . ? C21 C17 C16 121.0(5) . . ? C19 C18 C16 121.6(5) . . ? C18 C19 C20 121.6(5) . . ? C22 C20 C21 115.8(5) . . ? C22 C20 C19 125.7(5) . . ? C21 C20 C19 118.4(6) . . ? N4 C21 C17 116.6(5) . . ? N4 C21 C20 123.5(5) . . ? C17 C21 C20 119.8(5) . . ? C23 C22 C20 120.2(6) . . ? C22 C23 C24 120.0(6) . . ? N4 C24 C23 121.9(5) . . ? N5 C25 C26 122.6(5) . . ? C27 C26 C25 119.3(6) . . ? C26 C27 C28 120.6(5) . . ? C27 C28 C29 116.5(5) . . ? C27 C28 C30 124.2(5) . . ? C29 C28 C30 119.3(6) . . ? N5 C29 C28 123.9(5) . . ? N5 C29 C33 116.7(5) . . ? C28 C29 C33 119.4(5) . . ? C31 C30 C28 121.5(6) . . ? C30 C31 C32 121.2(6) . . ? C34 C32 C33 116.0(6) . . ? C34 C32 C31 126.3(6) . . ? C33 C32 C31 117.7(6) . . ? N6 C33 C32 122.8(5) . . ? N6 C33 C29 116.4(5) . . ? C32 C33 C29 120.9(5) . . ? C35 C34 C32 121.7(6) . . ? C34 C35 C36 118.6(6) . . ? N6 C36 C35 122.8(6) . . ? N7 C37 C38 123.0(6) . . ? C39 C38 C37 119.2(7) . . ? C38 C39 C40 120.9(7) . . ? C39 C40 C41 116.5(7) . . ? C39 C40 C42 124.9(7) . . ? C41 C40 C42 118.6(7) . . ? N7 C41 C40 122.5(6) . . ? N7 C41 C45 116.8(5) . . ? C40 C41 C45 120.7(6) . . ? C43 C42 C40 121.2(7) . . ? C42 C43 C44 121.1(7) . . ? C46 C44 C45 116.3(6) . . ? C46 C44 C43 124.0(7) . . ? C45 C44 C43 119.7(6) . . ? N8 C45 C44 124.3(6) . . ? N8 C45 C41 117.0(5) . . ? C44 C45 C41 118.7(6) . . ? C44 C46 C47 121.0(6) . . ? C46 C47 C48 119.1(6) . . ? N8 C48 C47 121.7(6) . . ? N9 C49 C50 123.2(5) . . ? C51 C50 C49 118.9(6) . . ? C50 C51 C52 120.5(5) . . ? C53 C52 C51 117.0(5) . . ? C53 C52 C54 117.4(5) . . ? C51 C52 C54 125.6(6) . . ? N9 C53 C52 122.1(5) . . ? N9 C53 C57 115.8(5) . . ? C52 C53 C57 122.1(5) . . ? C55 C54 C52 120.8(6) . . ? C54 C55 C56 121.8(6) . . ? C58 C56 C57 116.9(6) . . ? C58 C56 C55 124.2(6) . . ? C57 C56 C55 119.0(6) . . ? N10 C57 C56 123.0(6) . . ? N10 C57 C53 118.0(5) . . ? C56 C57 C53 118.9(5) . . ? C59 C58 C56 120.4(6) . . ? C58 C59 C60 119.1(6) . . ? N10 C60 C59 121.6(6) . . ? N11 C61 C62 123.3(6) . . ? C63 C62 C61 119.3(6) . . ? C62 C63 C64 120.5(6) . . ? C63 C64 C65 116.9(6) . . ? C63 C64 C66 125.8(6) . . ? C65 C64 C66 117.3(6) . . ? N11 C65 C64 122.4(5) . . ? N11 C65 C69 116.2(5) . . ? C64 C65 C69 121.4(5) . . ? C67 C66 C64 122.1(6) . . ? C66 C67 C68 121.9(6) . . ? C70 C68 C69 117.2(6) . . ? C70 C68 C67 124.0(6) . . ? C69 C68 C67 118.8(6) . . ? N12 C69 C68 122.3(5) . . ? N12 C69 C65 119.1(5) . . ? C68 C69 C65 118.6(5) . . ? C71 C70 C68 119.5(6) . . ? C70 C71 C72 120.4(6) . . ? N12 C72 C71 122.6(6) . . ? F12 B1 F13 114.0(9) . . ? F13A B1 F14A 114.6(11) . . ? F13 B1 F14A 132.8(12) . . ? F13A B1 F11 115.1(10) . . ? F12 B1 F11 116.5(10) . . ? F13 B1 F11 111.5(9) . . ? F14A B1 F11 113.7(10) . . ? F12 B1 F14 109.0(9) . . ? F13 B1 F14 104.7(9) . . ? F11 B1 F14 99.3(8) . . ? F13A B1 F12A 109.2(12) . . ? F13 B1 F12A 56.5(9) . . ? F14A B1 F12A 102.5(9) . . ? F11 B1 F12A 99.6(8) . . ? F23A B2 F24A 114.7(9) . . ? F23A B2 F21 107.7(8) . . ? F23 B2 F21 127.8(7) . . ? F24A B2 F21 109.6(7) . . ? F23A B2 F22A 110.1(8) . . ? F24A B2 F22A 108.3(9) . . ? F21 B2 F22A 106.1(8) . . ? F23 B2 F24 116.1(8) . . ? F21 B2 F24 113.3(8) . . ? F23 B2 F22 91.0(8) . . ? F21 B2 F22 99.6(6) . . ? F24 B2 F22 96.1(9) . . ? F34 B3 F33 122.4(11) . . ? F34 B3 F31 120.2(10) . . ? F33 B3 F31 116.0(12) . . ? F34A B3 F33A 119.7(13) . . ? F31 B3 F33A 113.9(12) . . ? F34 B3 F32 85.5(14) . . ? F33 B3 F32 97.4(18) . . ? F31 B3 F32 75.2(10) . . ? F34A B3 F32A 90.9(16) . . ? F31 B3 F32A 88.7(13) . . ? F33A B3 F32A 91.5(13) . . ? F42A B4 F41 117.5(9) . . ? F42A B4 F44A 114.4(9) . . ? F41 B4 F44A 105.8(7) . . ? F41 B4 F43 115.9(7) . . ? F41 B4 F44 110.3(5) . . ? F43 B4 F44 110.2(7) . . ? F42A B4 F43A 110.1(9) . . ? F41 B4 F43A 103.1(8) . . ? F44A B4 F43A 104.7(9) . . ? F41 B4 F42 105.1(7) . . ? F43 B4 F42 109.1(7) . . ? F44 B4 F42 105.7(7) . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.430 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.066 data_complex1 _database_code_depnum_ccdc_archive 'CCDC 208794' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Cu N3 O6' _chemical_formula_weight 357.79 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 7.0641(6) _cell_length_b 9.8410(8) _cell_length_c 10.4885(9) _cell_angle_alpha 72.079(2) _cell_angle_beta 73.176(2) _cell_angle_gamma 74.6290(10) _cell_volume 651.55(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Parallelopiped _exptl_crystal_colour Blue _exptl_crystal_size_max .20 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 364 _exptl_absorpt_coefficient_mu 1.713 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min .8230 _exptl_absorpt_correction_T_max .9375 _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 '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_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7029 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 28.27 _reflns_number_total 3116 _reflns_number_gt 2507 _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, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1997)' _computing_publication_material 'Platon99 (Spek, 1999)' _refine_special_details ; #--------------------------------------------------------------------- All non-H atoms were refined anisotropically. H-atoms were placed in calculated positions by appropriate HFIX command. #--------------------------------------------------------------------- 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 w=1/[\s^2^(Fo^2^)+(0.0769P)^2^+0.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3116 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1371 _refine_ls_wR_factor_gt 0.1295 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 Cu Cu 0.10427(7) 0.42673(4) 0.14656(4) 0.02288(17) Uani 1 1 d . . . O1 O 0.1953(4) 0.2350(3) 0.1123(3) 0.0292(6) Uani 1 1 d . . . O2 O 0.4257(4) 0.2709(3) -0.0882(3) 0.0361(7) Uani 1 1 d . . . O3W O 0.2224(4) 0.5169(3) -0.0461(3) 0.0285(6) Uani 1 1 d . . . O4 O 0.4054(5) 0.3711(3) 0.2497(3) 0.0407(7) Uani 1 1 d . . . O5 O 0.4395(5) 0.1411(3) 0.3524(3) 0.0449(8) Uani 1 1 d . . . O6 O 0.6602(4) 0.2181(3) 0.1696(3) 0.0415(8) Uani 1 1 d . . . N1 N 0.0017(4) 0.6098(3) 0.2110(3) 0.0234(6) Uani 1 1 d . . . N2 N -0.0634(4) 0.3462(3) 0.3314(3) 0.0236(6) Uani 1 1 d . . . N3 N 0.5009(5) 0.2408(3) 0.2587(3) 0.0281(7) Uani 1 1 d . . . C1 C 0.0352(6) 0.7454(4) 0.1388(4) 0.0312(9) Uani 1 1 d . . . H1 H 0.1229 0.7575 0.0526 0.037 Uiso 1 1 calc R . . C2 C -0.0585(6) 0.8655(4) 0.1909(4) 0.0337(9) Uani 1 1 d . . . H2 H -0.0356 0.9575 0.1392 0.040 Uiso 1 1 calc R . . C3 C -0.1847(6) 0.8490(4) 0.3184(4) 0.0324(9) Uani 1 1 d . . . H3 H -0.2498 0.9297 0.3535 0.039 Uiso 1 1 calc R . . C4 C -0.2149(5) 0.7113(4) 0.3950(4) 0.0283(8) Uani 1 1 d . . . H4 H -0.2956 0.6974 0.4837 0.034 Uiso 1 1 calc R . . C5 C -0.1223(5) 0.5940(4) 0.3368(3) 0.0197(7) Uani 1 1 d . . . C6 C -0.1554(5) 0.4428(4) 0.4075(4) 0.0215(7) Uani 1 1 d . . . C7 C -0.2716(5) 0.4044(4) 0.5383(4) 0.0261(8) Uani 1 1 d . . . H7 H -0.3309 0.4731 0.5896 0.031 Uiso 1 1 calc R . . C8 C -0.2989(6) 0.2613(4) 0.5927(4) 0.0306(9) Uani 1 1 d . . . H8 H -0.3764 0.2322 0.6809 0.037 Uiso 1 1 calc R . . C9 C -0.2078(6) 0.1633(4) 0.5121(4) 0.0322(9) Uani 1 1 d . . . H9 H -0.2263 0.0674 0.5451 0.039 Uiso 1 1 calc R . . C10 C -0.0902(6) 0.2077(4) 0.3834(4) 0.0277(8) Uani 1 1 d . . . H10 H -0.0274 0.1405 0.3309 0.033 Uiso 1 1 calc R . . C11 C 0.3448(5) 0.1909(4) 0.0195(4) 0.0249(8) Uani 1 1 d . . . C12 C 0.4181(6) 0.0290(4) 0.0528(4) 0.0315(9) Uani 1 1 d . . . H12A H 0.4642 0.0001 0.1376 0.038 Uiso 1 1 calc R . . H12B H 0.3044 -0.0170 0.0701 0.038 Uiso 1 1 calc R . . H1W H 0.2723 0.4527 -0.0926 0.038 Uiso 1 1 d . . . H2W H 0.2840 0.5878 -0.0872 0.038 Uiso 1 1 d . . . 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 Cu 0.0284(3) 0.0156(2) 0.0178(2) -0.00616(16) 0.00370(16) -0.00046(16) O1 0.0344(14) 0.0175(12) 0.0269(14) -0.0096(10) 0.0067(11) -0.0005(11) O2 0.0436(16) 0.0223(14) 0.0265(14) -0.0065(11) 0.0081(12) 0.0026(12) O3W 0.0371(15) 0.0195(13) 0.0194(12) -0.0044(10) 0.0061(11) -0.0041(11) O4 0.0415(17) 0.0270(15) 0.0491(19) -0.0132(13) -0.0073(14) 0.0016(13) O5 0.0529(19) 0.0346(17) 0.0351(17) -0.0027(14) 0.0053(14) -0.0126(15) O6 0.0369(16) 0.0388(17) 0.0383(17) -0.0145(14) 0.0107(13) -0.0053(13) N1 0.0255(15) 0.0203(15) 0.0212(15) -0.0078(12) -0.0013(12) -0.0005(12) N2 0.0234(15) 0.0208(15) 0.0223(15) -0.0055(12) -0.0008(12) -0.0018(12) N3 0.0281(16) 0.0271(17) 0.0277(17) -0.0114(14) -0.0025(13) -0.0019(13) C1 0.034(2) 0.028(2) 0.027(2) -0.0059(16) 0.0018(16) -0.0091(17) C2 0.042(2) 0.0158(17) 0.039(2) -0.0044(16) -0.0075(19) -0.0032(16) C3 0.032(2) 0.026(2) 0.039(2) -0.0196(17) -0.0047(17) 0.0032(16) C4 0.0243(18) 0.028(2) 0.029(2) -0.0146(16) 0.0013(15) 0.0017(15) C5 0.0168(16) 0.0201(17) 0.0203(17) -0.0066(14) -0.0037(13) 0.0008(13) C6 0.0199(16) 0.0209(17) 0.0229(17) -0.0069(14) -0.0044(14) -0.0017(13) C7 0.0224(17) 0.0277(19) 0.0245(18) -0.0093(15) -0.0008(14) -0.0004(14) C8 0.0266(19) 0.036(2) 0.0214(18) -0.0014(16) -0.0010(15) -0.0046(16) C9 0.035(2) 0.0231(19) 0.032(2) -0.0012(16) -0.0048(17) -0.0055(16) C10 0.033(2) 0.0217(18) 0.0273(19) -0.0080(15) -0.0058(16) -0.0027(15) C11 0.0258(18) 0.0233(18) 0.0264(19) -0.0151(15) -0.0036(15) 0.0018(15) C12 0.034(2) 0.0183(18) 0.034(2) -0.0083(16) 0.0029(17) -0.0013(15) _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 Cu O1 1.934(2) . ? Cu O3W 1.970(3) . ? Cu N1 2.001(3) . ? Cu N2 2.003(3) . ? O1 C11 1.294(4) . ? O2 C11 1.241(5) . ? O4 N3 1.269(4) . ? O5 N3 1.226(4) . ? O6 N3 1.256(4) . ? N1 C5 1.345(4) . ? N1 C1 1.361(5) . ? N2 C6 1.342(5) . ? N2 C10 1.345(5) . ? C1 C2 1.381(5) . ? C2 C3 1.365(6) . ? C3 C4 1.382(5) . ? C4 C5 1.391(5) . ? C5 C6 1.492(5) . ? C6 C7 1.376(5) . ? C7 C8 1.390(5) . ? C8 C9 1.385(6) . ? C9 C10 1.373(6) . ? C11 C12 1.501(5) . ? C12 C12 1.480(7) 2_655 ? 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 Cu O3W 90.97(11) . . ? O1 Cu N1 171.66(11) . . ? O3W Cu N1 97.19(11) . . ? O1 Cu N2 90.90(12) . . ? O3W Cu N2 169.54(12) . . ? N1 Cu N2 81.40(12) . . ? C11 O1 Cu 128.8(2) . . ? C5 N1 C1 118.5(3) . . ? C5 N1 Cu 114.3(2) . . ? C1 N1 Cu 127.0(3) . . ? C6 N2 C10 118.9(3) . . ? C6 N2 Cu 115.0(2) . . ? C10 N2 Cu 126.2(3) . . ? O5 N3 O6 121.4(3) . . ? O5 N3 O4 120.7(3) . . ? O6 N3 O4 117.9(3) . . ? N1 C1 C2 121.4(4) . . ? C3 C2 C1 119.9(4) . . ? C2 C3 C4 119.4(4) . . ? C3 C4 C5 118.7(3) . . ? N1 C5 C4 122.0(3) . . ? N1 C5 C6 115.2(3) . . ? C4 C5 C6 122.8(3) . . ? N2 C6 C7 122.4(3) . . ? N2 C6 C5 114.0(3) . . ? C7 C6 C5 123.6(3) . . ? C6 C7 C8 118.9(4) . . ? C9 C8 C7 118.3(4) . . ? C10 C9 C8 119.9(4) . . ? N2 C10 C9 121.6(4) . . ? O2 C11 O1 125.1(3) . . ? O2 C11 C12 121.0(3) . . ? O1 C11 C12 113.8(3) . . ? C12 C12 C11 116.4(4) 2_655 . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.423 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.127 #===END data_complex2 _database_code_depnum_ccdc_archive 'CCDC 208795' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 Cu N3 O6' _chemical_formula_weight 381.81 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' Cu Cu 0.3201 1.2651 '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' _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 6.9386(8) _cell_length_b 10.3463(14) _cell_length_c 10.8572(17) _cell_angle_alpha 69.734(11) _cell_angle_beta 81.354(11) _cell_angle_gamma 75.687(10) _cell_volume 706.68(17) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.915 _cell_measurement_theta_max 14.165 _exptl_crystal_description Prism _exptl_crystal_colour Blue _exptl_crystal_size_max .28 _exptl_crystal_size_mid .22 _exptl_crystal_size_min .12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 1.586 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min .928 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; North, A.C.T.; Phillips, D.C. and Mathews, F.S. (1968). Acta Crystallographica, A24, 351-9 ; _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 'Rigaku AFC7S diffractometer' _diffrn_measurement_method '\w-2\q scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.95% _diffrn_reflns_number 3240 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3240 _reflns_number_gt 2277 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC diffractometer control (MSC, 1992)' _computing_cell_refinement 'MSC/AFC diffractometer control (MSC, 1992)' _computing_data_reduction 'teXsan, (MSC, 1992)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1997)' _computing_publication_material 'Platon99 (Spek, 1999)' _refine_special_details ; #--------------------------------------------------------------------- All non-H atoms were refined anisotropically. H-atoms were placed in calculated positions by appropriate HFIX command. #--------------------------------------------------------------------- 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 w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+0.5185P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3240 _refine_ls_number_parameters 219 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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 Cu Cu 0.15033(6) 0.08981(4) 0.36424(3) 0.02759(12) Uani 1 1 d . . . N1 N 0.2745(4) -0.0801(2) 0.3101(2) 0.0270(5) Uani 1 1 d . . . N2 N 0.0796(4) 0.1709(2) 0.1762(2) 0.0279(5) Uani 1 1 d . . . O3W O 0.1911(3) -0.0021(2) 0.55507(19) 0.0307(5) Uani 1 1 d . . . H1W H 0.1759 0.0793 0.5821 0.073(14) Uiso 1 1 d . . . H2W H 0.3086 -0.0793 0.6021 0.101(18) Uiso 1 1 d . . . O1 O 0.0352(4) 0.2691(2) 0.3882(2) 0.0351(5) Uani 1 1 d . . . O2 O 0.1231(4) 0.2393(2) 0.5869(2) 0.0410(6) Uani 1 1 d . . . C1 C 0.3639(5) -0.2088(3) 0.3815(3) 0.0355(7) Uani 1 1 d . . . H1 H 0.3716 -0.2284 0.4711 0.043 Uiso 1 1 calc R . . C2 C 0.4464(5) -0.3151(3) 0.3256(4) 0.0412(8) Uani 1 1 d . . . H2 H 0.5054 -0.4043 0.3784 0.049 Uiso 1 1 calc R . . C3 C 0.4408(5) -0.2889(4) 0.1940(4) 0.0393(8) Uani 1 1 d . . . H3 H 0.4953 -0.3597 0.1568 0.047 Uiso 1 1 calc R . . C4 C 0.3516(5) -0.1535(3) 0.1153(3) 0.0305(6) Uani 1 1 d . . . C5 C 0.2672(4) -0.0542(3) 0.1794(3) 0.0255(6) Uani 1 1 d . . . C6 C 0.1656(4) 0.0833(3) 0.1063(3) 0.0258(6) Uani 1 1 d . . . C7 C 0.1580(5) 0.1208(4) -0.0300(3) 0.0326(7) Uani 1 1 d . . . C8 C 0.2541(5) 0.0198(4) -0.0939(3) 0.0393(8) Uani 1 1 d . . . H8 H 0.2537 0.0449 -0.1848 0.047 Uiso 1 1 calc R . . C9 C 0.3458(5) -0.1119(4) -0.0245(3) 0.0380(8) Uani 1 1 d . . . H9 H 0.4059 -0.1761 -0.0683 0.046 Uiso 1 1 calc R . . C10 C 0.0518(5) 0.2576(4) -0.0943(3) 0.0390(8) Uani 1 1 d . . . H10 H 0.0451 0.2891 -0.1852 0.047 Uiso 1 1 calc R . . C11 C -0.0408(6) 0.3434(4) -0.0225(3) 0.0420(8) Uani 1 1 d . . . H11 H -0.1156 0.4323 -0.0639 0.050 Uiso 1 1 calc R . . C12 C -0.0237(5) 0.2980(3) 0.1135(3) 0.0357(7) Uani 1 1 d . . . H12 H -0.0862 0.3581 0.1611 0.043 Uiso 1 1 calc R . . C13 C 0.0592(5) 0.3144(3) 0.4787(3) 0.0287(6) Uani 1 1 d . . . C14 C 0.0011(6) 0.4727(3) 0.4451(3) 0.0381(8) Uani 1 1 d . . . H14A H 0.0931 0.5141 0.3743 0.046 Uiso 1 1 calc R . . H14B H -0.1307 0.5045 0.4121 0.046 Uiso 1 1 calc R . . N3 N 0.4717(4) 0.2984(3) 0.2653(3) 0.0356(6) Uani 1 1 d . . . O4 O 0.4801(4) 0.1664(2) 0.3169(2) 0.0432(6) Uani 1 1 d . . . O6 O 0.5383(6) 0.3596(3) 0.3210(3) 0.0801(11) Uani 1 1 d . . . O5 O 0.3978(5) 0.3612(3) 0.1596(3) 0.0637(8) Uani 1 1 d . . . 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 Cu 0.0417(2) 0.01982(17) 0.02034(17) -0.00743(12) -0.00835(13) 0.00028(14) N1 0.0357(14) 0.0210(12) 0.0237(11) -0.0065(9) -0.0054(10) -0.0041(10) N2 0.0374(14) 0.0228(12) 0.0240(12) -0.0058(10) -0.0073(10) -0.0068(10) O3W 0.0454(13) 0.0221(10) 0.0230(10) -0.0064(8) -0.0101(9) -0.0011(9) O1 0.0528(15) 0.0232(10) 0.0296(11) -0.0125(9) -0.0141(10) 0.0037(10) O2 0.0703(17) 0.0239(11) 0.0286(11) -0.0090(9) -0.0191(11) 0.0006(11) C1 0.047(2) 0.0252(15) 0.0306(15) -0.0064(12) -0.0092(14) -0.0006(14) C2 0.044(2) 0.0226(15) 0.053(2) -0.0119(14) -0.0086(16) 0.0033(14) C3 0.0386(19) 0.0345(17) 0.052(2) -0.0257(16) 0.0020(15) -0.0064(14) C4 0.0294(16) 0.0328(16) 0.0363(16) -0.0194(13) 0.0013(12) -0.0097(13) C5 0.0260(15) 0.0281(14) 0.0253(13) -0.0105(11) -0.0017(11) -0.0079(12) C6 0.0286(15) 0.0289(15) 0.0226(13) -0.0081(11) -0.0020(11) -0.0107(12) C7 0.0342(17) 0.0416(17) 0.0258(14) -0.0087(13) -0.0025(12) -0.0175(14) C8 0.046(2) 0.059(2) 0.0233(14) -0.0193(15) 0.0053(13) -0.0243(17) C9 0.0362(18) 0.053(2) 0.0358(17) -0.0277(16) 0.0077(14) -0.0165(16) C10 0.051(2) 0.0425(19) 0.0228(14) 0.0018(13) -0.0115(14) -0.0205(16) C11 0.056(2) 0.0307(17) 0.0362(17) 0.0027(14) -0.0209(16) -0.0120(16) C12 0.0470(19) 0.0236(15) 0.0341(16) -0.0048(12) -0.0120(14) -0.0045(13) C13 0.0359(17) 0.0230(14) 0.0282(14) -0.0105(11) -0.0033(12) -0.0040(12) C14 0.060(2) 0.0204(14) 0.0333(16) -0.0104(12) -0.0137(15) 0.0005(14) N3 0.0395(16) 0.0305(14) 0.0326(14) -0.0081(11) -0.0057(12) -0.0012(12) O4 0.0451(14) 0.0250(11) 0.0532(15) -0.0068(10) -0.0132(11) 0.0012(10) O6 0.143(3) 0.0467(17) 0.0626(19) -0.0082(15) -0.048(2) -0.0312(19) O5 0.085(2) 0.0449(15) 0.0496(16) -0.0020(13) -0.0329(15) 0.0041(15) _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 Cu O1 1.920(2) . ? Cu O3W 1.989(2) . ? Cu N1 1.998(2) . ? Cu N2 2.006(2) . ? N1 C1 1.334(4) . ? N1 C5 1.357(3) . ? N2 C12 1.329(4) . ? N2 C6 1.351(4) . ? O1 C13 1.273(3) . ? O2 C13 1.239(3) . ? C1 C2 1.398(4) . ? C2 C3 1.363(5) . ? C3 C4 1.407(5) . ? C4 C5 1.399(4) . ? C4 C9 1.430(4) . ? C5 C6 1.428(4) . ? C6 C7 1.400(4) . ? C7 C10 1.410(5) . ? C7 C8 1.426(5) . ? C8 C9 1.354(5) . ? C10 C11 1.362(5) . ? C11 C12 1.400(4) . ? C13 C14 1.511(4) . ? C14 C14 1.482(6) 2_566 ? N3 O6 1.214(4) . ? N3 O5 1.224(3) . ? N3 O4 1.274(3) . ? 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 Cu O3W 91.90(8) . . ? O1 Cu N1 171.25(9) . . ? O3W Cu N1 96.51(9) . . ? O1 Cu N2 89.75(9) . . ? O3W Cu N2 172.76(10) . . ? N1 Cu N2 82.19(10) . . ? C1 N1 C5 117.7(3) . . ? C1 N1 Cu 130.0(2) . . ? C5 N1 Cu 112.27(19) . . ? C12 N2 C6 118.6(3) . . ? C12 N2 Cu 129.0(2) . . ? C6 N2 Cu 112.16(19) . . ? C13 O1 Cu 128.98(19) . . ? N1 C1 C2 122.0(3) . . ? C3 C2 C1 120.4(3) . . ? C2 C3 C4 119.2(3) . . ? C5 C4 C3 116.9(3) . . ? C5 C4 C9 119.0(3) . . ? C3 C4 C9 124.1(3) . . ? N1 C5 C4 123.7(3) . . ? N1 C5 C6 116.4(2) . . ? C4 C5 C6 119.8(3) . . ? N2 C6 C7 123.5(3) . . ? N2 C6 C5 116.4(2) . . ? C7 C6 C5 120.1(3) . . ? C6 C7 C10 116.5(3) . . ? C6 C7 C8 118.8(3) . . ? C10 C7 C8 124.6(3) . . ? C9 C8 C7 121.2(3) . . ? C8 C9 C4 120.9(3) . . ? C11 C10 C7 119.6(3) . . ? C10 C11 C12 120.1(3) . . ? N2 C12 C11 121.6(3) . . ? O2 C13 O1 125.1(3) . . ? O2 C13 C14 120.6(3) . . ? O1 C13 C14 114.3(2) . . ? C14 C14 C13 115.6(3) 2_566 . ? O6 N3 O5 121.1(3) . . ? O6 N3 O4 119.6(3) . . ? O5 N3 O4 119.3(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.373 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.075 #===END data_complex3 _database_code_depnum_ccdc_archive 'CCDC 208796' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(CU (N2 C10 H8)) (C4 H4 O4 2-) 2(Cl O4 1-) 1.5(O H2)' _chemical_formula_sum 'C24 H23 Cl2 Cu2 N4 O13.50' _chemical_formula_weight 781.44 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.947(4) _cell_length_b 12.566(3) _cell_length_c 14.539(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.46(2) _cell_angle_gamma 90.00 _cell_volume 2936.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelepiped _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1580 _exptl_absorpt_coefficient_mu 1.706 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.4085 _exptl_absorpt_correction_T_max 0.6826 _exptl_special_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _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 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11307 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 26.02 _reflns_number_total 5769 _reflns_number_gt 3901 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius xpress' _computing_cell_refinement 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_data_reduction 'Mosflm (Acta Cryst. D50, 760, 1994)' _computing_structure_solution 'Shelxs-97 (Sheldrick, 1990)' _computing_structure_refinement 'Shelxl-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.64.02 (Farrugia, 1999)' _refine_special_details ; #--------------------------------------------------------------------- All non-H atoms were refined anisotropically. During refinement both the perchlorate moieties (ClO4) were found to be disordered over two positions. The oxygen atoms around Cl1 take two orientation (O61,O62,O63,O64)/(O51,O52,O53,O54) with occupancy ratio 0.336/0.664. Similarly for Cl2 two disordered orientation of oxygens (O71,O72,O73,O74)/(O81,O82,O83,O84) are having occupancy ratio 0.224/0.776. The non-coordinated water oxygen (O2W) was located from difference map and its occupancy was kept fixed at 0.5 (random positional disorder) after a series of experiment. The H-atoms around coordinated water oxygen (O1W) were located from difference Fourier and kept fixed in subsequent refinements. All the H-atoms were placed in calculated positions. #--------------------------------------------------------------------- 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 w=1/[\s^2^(Fo^2^)+(0.0884P)^2^+1.6214P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5769 _refine_ls_number_parameters 459 _refine_ls_number_restraints 116 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1608 _refine_ls_wR_factor_gt 0.1465 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.014 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 0.09544(4) 0.95529(4) 0.51099(4) 0.0496(2) Uani 1 1 d . . . Cu2 Cu 0.18699(4) 0.96450(5) 0.36209(5) 0.0530(2) Uani 1 1 d . . . N1 N 0.1596(3) 1.0736(3) 0.5924(3) 0.0571(10) Uani 1 1 d . . . N2 N 0.1898(3) 0.8708(3) 0.5956(3) 0.0571(10) Uani 1 1 d . . . N3 N 0.2768(3) 1.0611(3) 0.4393(3) 0.0587(11) Uani 1 1 d . . . N4 N 0.2778(3) 0.8563(3) 0.4150(3) 0.0623(11) Uani 1 1 d . . . O1 O 0.0493(2) 0.8352(3) 0.4250(2) 0.0572(8) Uani 1 1 d . . . O2 O 0.0157(2) 1.0524(2) 0.4237(2) 0.0511(8) Uani 1 1 d . . . O3 O 0.1052(2) 0.8565(3) 0.3056(3) 0.0597(9) Uani 1 1 d . . . O4 O 0.1011(2) 1.0777(3) 0.3366(2) 0.0553(8) Uani 1 1 d . . . C1 C 0.1382(4) 1.1760(4) 0.5874(4) 0.0645(14) Uani 1 1 d . . . H1 H 0.0872 1.1967 0.5443 0.077 Uiso 1 1 calc R . . C2 C 0.1902(4) 1.2528(5) 0.6450(5) 0.0765(17) Uani 1 1 d . . . H2 H 0.1738 1.3238 0.6400 0.092 Uiso 1 1 calc R . . C3 C 0.2651(4) 1.2239(6) 0.7086(5) 0.0829(18) Uani 1 1 d . . . H3 H 0.3003 1.2743 0.7476 0.099 Uiso 1 1 calc R . . C4 C 0.2874(4) 1.1185(5) 0.7139(4) 0.0774(17) Uani 1 1 d . . . H4 H 0.3382 1.0967 0.7568 0.093 Uiso 1 1 calc R . . C5 C 0.2343(3) 1.0452(4) 0.6555(4) 0.0606(13) Uani 1 1 d . . . C6 C 0.2518(3) 0.9293(4) 0.6555(4) 0.0574(12) Uani 1 1 d . . . C7 C 0.3258(4) 0.8824(6) 0.7072(4) 0.0751(16) Uani 1 1 d . . . H7 H 0.3682 0.9235 0.7480 0.090 Uiso 1 1 calc R . . C8 C 0.3371(4) 0.7761(6) 0.6989(5) 0.0836(19) Uani 1 1 d . . . H8 H 0.3870 0.7438 0.7337 0.100 Uiso 1 1 calc R . . C9 C 0.2728(4) 0.7169(5) 0.6375(5) 0.0741(16) Uani 1 1 d . . . H9 H 0.2792 0.6442 0.6299 0.089 Uiso 1 1 calc R . . C10 C 0.2011(4) 0.7657(4) 0.5891(4) 0.0650(14) Uani 1 1 d . . . H10 H 0.1577 0.7251 0.5496 0.078 Uiso 1 1 calc R . . C11 C 0.2700(4) 1.1673(4) 0.4448(4) 0.0680(15) Uani 1 1 d . . . H11 H 0.2210 1.2001 0.4081 0.082 Uiso 1 1 calc R . . C12 C 0.3330(4) 1.2287(5) 0.5027(5) 0.0771(17) Uani 1 1 d . . . H12 H 0.3272 1.3020 0.5064 0.093 Uiso 1 1 calc R . . C13 C 0.4053(4) 1.1781(6) 0.5554(5) 0.087(2) Uani 1 1 d . . . H13 H 0.4487 1.2175 0.5964 0.104 Uiso 1 1 calc R . . C14 C 0.4142(4) 1.0696(5) 0.5480(5) 0.0757(16) Uani 1 1 d . . . H14 H 0.4634 1.0356 0.5825 0.091 Uiso 1 1 calc R . . C15 C 0.3487(3) 1.0131(5) 0.4885(4) 0.0623(13) Uani 1 1 d . . . C16 C 0.3492(3) 0.8968(5) 0.4748(4) 0.0638(14) Uani 1 1 d . . . C17 C 0.4167(4) 0.8320(6) 0.5189(5) 0.0790(17) Uani 1 1 d . . . H17 H 0.4658 0.8606 0.5600 0.095 Uiso 1 1 calc R . . C18 C 0.4095(4) 0.7217(6) 0.5003(5) 0.087(2) Uani 1 1 d . . . H18 H 0.4539 0.6765 0.5291 0.105 Uiso 1 1 calc R . . C19 C 0.3371(4) 0.6825(5) 0.4397(5) 0.0820(18) Uani 1 1 d . . . H19 H 0.3313 0.6100 0.4264 0.098 Uiso 1 1 calc R . . C20 C 0.2722(4) 0.7508(4) 0.3981(4) 0.0701(15) Uani 1 1 d . . . H20 H 0.2227 0.7232 0.3569 0.084 Uiso 1 1 calc R . . C21 C 0.0558(3) 0.8133(4) 0.3432(4) 0.0499(11) Uani 1 1 d . . . C22 C -0.0012(3) 0.7258(4) 0.2865(4) 0.0557(12) Uani 1 1 d . . . H22A H -0.0005 0.6672 0.3301 0.067 Uiso 1 1 calc R . . H22B H -0.0576 0.7531 0.2634 0.067 Uiso 1 1 calc R . . C23 C 0.0216(3) 0.6836(4) 0.2005(4) 0.0547(12) Uani 1 1 d . . . H23A H 0.0217 0.7423 0.1572 0.066 Uiso 1 1 calc R . . H23B H 0.0777 0.6552 0.2236 0.066 Uiso 1 1 calc R . . C24 C 0.0361(3) 1.0983(4) 0.3559(3) 0.0482(11) Uani 1 1 d . . . Cl2 Cl 0.14153(14) 0.46361(14) 0.38836(17) 0.0983(6) Uani 1 1 d D . . O61 O 0.0558(8) 0.4664(16) 0.3460(18) 0.164(7) Uani 0.336(15) 1 d PD . . O62 O 0.1830(13) 0.5147(17) 0.3352(15) 0.164(7) Uani 0.336(15) 1 d PD . . O63 O 0.1680(14) 0.3641(12) 0.4169(19) 0.164(7) Uani 0.336(15) 1 d PD . . O64 O 0.1557(14) 0.5238(17) 0.4774(13) 0.164(7) Uani 0.336(15) 1 d PD . . O51 O 0.0969(8) 0.4591(8) 0.2859(7) 0.167(7) Uani 0.664(15) 1 d PD . . O52 O 0.1126(11) 0.3829(9) 0.4322(9) 0.205(8) Uani 0.664(15) 1 d PD . . O53 O 0.1404(7) 0.5637(6) 0.4233(8) 0.146(5) Uani 0.664(15) 1 d PD . . O54 O 0.2268(7) 0.4357(12) 0.3957(11) 0.203(8) Uani 0.664(15) 1 d PD . . Cl1 Cl 0.42900(11) 0.46915(14) 0.70757(15) 0.0872(5) Uani 1 1 d D . . O71 O 0.4414(16) 0.3946(18) 0.7796(15) 0.127(8) Uani 0.224(12) 1 d PD . . O72 O 0.3442(10) 0.472(2) 0.6526(19) 0.127(8) Uani 0.224(12) 1 d PD . . O73 O 0.4705(13) 0.434(2) 0.6417(16) 0.127(8) Uani 0.224(12) 1 d PD . . O74 O 0.4571(16) 0.5683(13) 0.740(2) 0.127(8) Uani 0.224(12) 1 d PD . . O81 O 0.3606(5) 0.4671(8) 0.6237(6) 0.154(5) Uani 0.776(12) 1 d PD . . O82 O 0.3989(5) 0.4968(10) 0.7857(6) 0.179(5) Uani 0.776(12) 1 d PD . . O83 O 0.4867(5) 0.5480(6) 0.7041(7) 0.129(3) Uani 0.776(12) 1 d PD . . O84 O 0.4692(4) 0.3719(5) 0.7274(7) 0.129(4) Uani 0.776(12) 1 d PD . . O1W O 0.2086(3) 0.9988(4) 0.2258(3) 0.0851(13) Uani 1 1 d G . . H1W1 H 0.1603 0.9901 0.1729 0.128 Uiso 1 1 d G . . H1W2 H 0.2550 0.9857 0.2058 0.128 Uiso 1 1 d G . . O2W O 0.0728(6) 0.5607(10) 0.5856(7) 0.103(3) Uani 0.50 1 d PG . . H2W1 H 0.0693 0.5014 0.5456 0.154 Uiso 0.50 1 d PG . . H2W2 H 0.0205 0.5739 0.5921 0.154 Uiso 0.50 1 d PG . . 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 0.0502(4) 0.0442(3) 0.0531(4) -0.0012(3) 0.0142(3) 0.0012(3) Cu2 0.0476(4) 0.0464(4) 0.0669(4) -0.0003(3) 0.0207(3) -0.0004(3) N1 0.059(3) 0.054(2) 0.063(3) -0.005(2) 0.026(2) -0.002(2) N2 0.054(3) 0.056(2) 0.063(2) 0.003(2) 0.021(2) 0.002(2) N3 0.053(3) 0.057(2) 0.068(3) 0.003(2) 0.022(2) -0.001(2) N4 0.061(3) 0.056(3) 0.076(3) 0.002(2) 0.032(2) 0.006(2) O1 0.064(2) 0.0496(18) 0.059(2) -0.0077(16) 0.0206(17) -0.0032(16) O2 0.0524(19) 0.0501(18) 0.0526(19) 0.0057(15) 0.0191(16) 0.0015(15) O3 0.059(2) 0.0544(19) 0.070(2) -0.0030(17) 0.0256(18) -0.0060(17) O4 0.053(2) 0.0514(18) 0.065(2) 0.0028(16) 0.0245(17) 0.0038(16) C1 0.063(3) 0.053(3) 0.081(4) -0.010(3) 0.026(3) 0.000(3) C2 0.084(5) 0.059(3) 0.096(4) -0.017(3) 0.042(4) -0.013(3) C3 0.085(5) 0.084(5) 0.083(4) -0.023(4) 0.032(4) -0.021(4) C4 0.059(4) 0.091(5) 0.074(4) -0.013(3) 0.010(3) -0.016(3) C5 0.053(3) 0.071(3) 0.059(3) -0.003(3) 0.018(2) -0.004(3) C6 0.046(3) 0.068(3) 0.058(3) 0.004(3) 0.017(2) 0.001(3) C7 0.053(3) 0.092(5) 0.074(4) 0.008(3) 0.011(3) -0.001(3) C8 0.060(4) 0.094(5) 0.091(4) 0.030(4) 0.015(3) 0.013(3) C9 0.071(4) 0.066(3) 0.094(4) 0.023(3) 0.037(3) 0.013(3) C10 0.064(3) 0.054(3) 0.080(4) 0.013(3) 0.028(3) 0.006(3) C11 0.059(3) 0.063(3) 0.088(4) -0.002(3) 0.030(3) -0.002(3) C12 0.066(4) 0.068(4) 0.100(4) -0.017(3) 0.031(3) -0.017(3) C13 0.069(4) 0.102(5) 0.090(4) -0.027(4) 0.026(4) -0.026(4) C14 0.056(4) 0.089(4) 0.081(4) -0.010(3) 0.020(3) -0.004(3) C15 0.054(3) 0.068(3) 0.070(3) -0.001(3) 0.026(3) -0.001(3) C16 0.056(3) 0.072(3) 0.069(3) 0.004(3) 0.027(3) 0.010(3) C17 0.063(4) 0.092(5) 0.081(4) 0.007(4) 0.023(3) 0.013(3) C18 0.075(5) 0.090(5) 0.103(5) 0.017(4) 0.036(4) 0.027(4) C19 0.089(5) 0.067(4) 0.098(5) 0.009(3) 0.042(4) 0.023(4) C20 0.073(4) 0.054(3) 0.089(4) 0.001(3) 0.034(3) 0.006(3) C21 0.049(3) 0.040(2) 0.059(3) -0.002(2) 0.015(2) 0.006(2) C22 0.055(3) 0.052(3) 0.063(3) -0.013(2) 0.023(2) -0.008(2) C23 0.056(3) 0.049(3) 0.062(3) -0.009(2) 0.024(2) -0.010(2) C24 0.050(3) 0.045(2) 0.047(2) -0.002(2) 0.013(2) -0.001(2) Cl2 0.0994(14) 0.0719(11) 0.1179(16) 0.0048(10) 0.0264(12) 0.0069(10) O61 0.143(12) 0.131(10) 0.220(16) 0.049(10) 0.062(10) 0.000(8) O62 0.143(12) 0.131(10) 0.220(16) 0.049(10) 0.062(10) 0.000(8) O63 0.143(12) 0.131(10) 0.220(16) 0.049(10) 0.062(10) 0.000(8) O64 0.143(12) 0.131(10) 0.220(16) 0.049(10) 0.062(10) 0.000(8) O51 0.184(13) 0.131(8) 0.118(8) 0.004(6) -0.050(8) 0.000(8) O52 0.30(2) 0.137(10) 0.217(13) 0.036(9) 0.136(14) -0.063(12) O53 0.223(14) 0.064(5) 0.147(10) -0.006(5) 0.052(9) 0.014(6) O54 0.158(13) 0.201(15) 0.248(17) -0.017(12) 0.062(12) 0.050(11) Cl1 0.0663(10) 0.0732(10) 0.1048(13) -0.0072(9) 0.0023(9) 0.0069(8) O71 0.085(10) 0.136(15) 0.153(16) -0.036(11) 0.031(9) -0.003(9) O72 0.085(10) 0.136(15) 0.153(16) -0.036(11) 0.031(9) -0.003(9) O73 0.085(10) 0.136(15) 0.153(16) -0.036(11) 0.031(9) -0.003(9) O74 0.085(10) 0.136(15) 0.153(16) -0.036(11) 0.031(9) -0.003(9) O81 0.130(7) 0.121(7) 0.142(8) -0.047(6) -0.057(6) 0.049(6) O82 0.110(7) 0.289(14) 0.148(8) -0.073(9) 0.054(6) 0.005(8) O83 0.108(6) 0.126(7) 0.148(8) 0.028(5) 0.033(5) -0.018(5) O84 0.081(5) 0.086(5) 0.191(10) -0.007(5) 0.000(5) 0.030(4) O1W 0.097(3) 0.076(3) 0.100(3) 0.012(3) 0.057(3) 0.009(3) O2W 0.068(6) 0.175(10) 0.064(5) -0.034(7) 0.020(5) -0.019(6) _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 1.957(3) . ? Cu1 O2 1.960(3) . ? Cu1 N2 1.988(4) . ? Cu1 N1 1.995(4) . ? Cu1 O2 2.365(3) 3_576 ? Cu1 Cu2 3.0388(11) . ? Cu2 O3 1.928(3) . ? Cu2 O4 1.984(3) . ? Cu2 N3 1.992(5) . ? Cu2 N4 2.015(4) . ? Cu2 O1W 2.169(4) . ? N1 C1 1.333(6) . ? N1 C5 1.354(7) . ? N2 C10 1.342(7) . ? N2 C6 1.349(7) . ? N3 C11 1.344(7) . ? N3 C15 1.345(7) . ? N4 C20 1.346(7) . ? N4 C16 1.346(7) . ? O1 C21 1.259(6) . ? O2 C24 1.280(6) . ? O2 Cu1 2.365(3) 3_576 ? O3 C21 1.259(6) . ? O4 C24 1.248(6) . ? C1 C2 1.393(8) . ? C2 C3 1.362(9) . ? C3 C4 1.372(9) . ? C4 C5 1.376(8) . ? C5 C6 1.487(8) . ? C6 C7 1.374(8) . ? C7 C8 1.360(9) . ? C8 C9 1.386(9) . ? C9 C10 1.344(8) . ? C11 C12 1.370(8) . ? C12 C13 1.377(9) . ? C13 C14 1.380(9) . ? C14 C15 1.369(8) . ? C15 C16 1.475(8) . ? C16 C17 1.385(8) . ? C17 C18 1.409(10) . ? C18 C19 1.357(9) . ? C19 C20 1.375(8) . ? C21 C22 1.522(6) . ? C22 C23 1.517(7) . ? C23 C24 1.507(6) 2_545 ? C24 C23 1.507(6) 2 ? Cl2 O63 1.349(13) . ? Cl2 O53 1.359(7) . ? Cl2 O62 1.359(13) . ? Cl2 O52 1.369(8) . ? Cl2 O61 1.388(13) . ? Cl2 O51 1.442(8) . ? Cl2 O64 1.452(14) . ? Cl2 O54 1.457(10) . ? Cl1 O74 1.362(15) . ? Cl1 O71 1.371(15) . ? Cl1 O84 1.385(6) . ? Cl1 O81 1.392(7) . ? Cl1 O83 1.404(7) . ? Cl1 O72 1.406(14) . ? Cl1 O73 1.426(14) . ? Cl1 O82 1.428(7) . ? 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 O2 90.72(14) . . ? O1 Cu1 N2 93.67(16) . . ? O2 Cu1 N2 171.11(16) . . ? O1 Cu1 N1 170.38(16) . . ? O2 Cu1 N1 93.14(17) . . ? N2 Cu1 N1 81.38(18) . . ? O1 Cu1 O2 90.99(13) . 3_576 ? O2 Cu1 O2 79.15(13) . 3_576 ? N2 Cu1 O2 108.47(14) . 3_576 ? N1 Cu1 O2 98.39(15) . 3_576 ? O1 Cu1 Cu2 76.40(10) . . ? O2 Cu1 Cu2 85.29(10) . . ? N2 Cu1 Cu2 88.22(12) . . ? N1 Cu1 Cu2 95.12(12) . . ? O2 Cu1 Cu2 159.87(9) 3_576 . ? O3 Cu2 O4 92.27(15) . . ? O3 Cu2 N3 170.75(17) . . ? O4 Cu2 N3 92.99(16) . . ? O3 Cu2 N4 92.68(17) . . ? O4 Cu2 N4 168.94(16) . . ? N3 Cu2 N4 80.86(19) . . ? O3 Cu2 O1W 93.28(17) . . ? O4 Cu2 O1W 90.77(16) . . ? N3 Cu2 O1W 94.26(19) . . ? N4 Cu2 O1W 98.81(18) . . ? O3 Cu2 Cu1 79.43(11) . . ? O4 Cu2 Cu1 69.54(10) . . ? N3 Cu2 Cu1 95.31(13) . . ? N4 Cu2 Cu1 101.70(13) . . ? O1W Cu2 Cu1 158.49(13) . . ? C1 N1 C5 118.1(5) . . ? C1 N1 Cu1 126.8(4) . . ? C5 N1 Cu1 115.0(3) . . ? C10 N2 C6 118.8(5) . . ? C10 N2 Cu1 126.0(4) . . ? C6 N2 Cu1 114.7(3) . . ? C11 N3 C15 119.6(5) . . ? C11 N3 Cu2 125.1(4) . . ? C15 N3 Cu2 115.4(4) . . ? C20 N4 C16 119.2(5) . . ? C20 N4 Cu2 126.4(4) . . ? C16 N4 Cu2 114.4(4) . . ? C21 O1 Cu1 129.5(3) . . ? C24 O2 Cu1 118.7(3) . . ? C24 O2 Cu1 140.4(3) . 3_576 ? Cu1 O2 Cu1 100.85(13) . 3_576 ? C21 O3 Cu2 127.3(3) . . ? C24 O4 Cu2 139.0(3) . . ? N1 C1 C2 121.8(6) . . ? C3 C2 C1 119.9(6) . . ? C2 C3 C4 118.5(6) . . ? C3 C4 C5 119.7(6) . . ? N1 C5 C4 122.0(5) . . ? N1 C5 C6 113.6(5) . . ? C4 C5 C6 124.4(5) . . ? N2 C6 C7 120.6(5) . . ? N2 C6 C5 114.8(5) . . ? C7 C6 C5 124.5(5) . . ? C8 C7 C6 120.1(6) . . ? C7 C8 C9 118.7(6) . . ? C10 C9 C8 119.2(6) . . ? N2 C10 C9 122.6(6) . . ? N3 C11 C12 122.1(6) . . ? C11 C12 C13 117.7(6) . . ? C12 C13 C14 120.9(6) . . ? C15 C14 C13 118.3(6) . . ? N3 C15 C14 121.4(6) . . ? N3 C15 C16 114.5(5) . . ? C14 C15 C16 124.1(6) . . ? N4 C16 C17 121.2(6) . . ? N4 C16 C15 114.8(5) . . ? C17 C16 C15 124.0(6) . . ? C16 C17 C18 118.8(6) . . ? C19 C18 C17 119.1(6) . . ? C18 C19 C20 119.5(6) . . ? N4 C20 C19 122.3(6) . . ? O3 C21 O1 125.8(4) . . ? O3 C21 C22 118.2(4) . . ? O1 C21 C22 116.1(4) . . ? C23 C22 C21 114.5(4) . . ? C24 C23 C22 114.0(4) 2_545 . ? O4 C24 O2 123.5(4) . . ? O4 C24 C23 119.5(4) . 2 ? O2 C24 C23 116.9(4) . 2 ? O63 Cl2 O53 141.8(11) . . ? O63 Cl2 O62 115.6(10) . . ? O53 Cl2 O62 81.2(10) . . ? O63 Cl2 O52 45.8(9) . . ? O53 Cl2 O52 117.5(7) . . ? O62 Cl2 O52 160.2(10) . . ? O63 Cl2 O61 111.0(10) . . ? O53 Cl2 O61 90.3(11) . . ? O62 Cl2 O61 113.1(10) . . ? O52 Cl2 O61 75.3(10) . . ? O63 Cl2 O51 107.2(12) . . ? O53 Cl2 O51 111.0(6) . . ? O62 Cl2 O51 68.1(10) . . ? O52 Cl2 O51 107.7(7) . . ? O61 Cl2 O51 53.8(10) . . ? O63 Cl2 O64 105.3(10) . . ? O53 Cl2 O64 37.1(8) . . ? O62 Cl2 O64 107.0(9) . . ? O52 Cl2 O64 87.3(11) . . ? O61 Cl2 O64 103.7(10) . . ? O51 Cl2 O64 145.7(10) . . ? O63 Cl2 O54 61.9(9) . . ? O53 Cl2 O54 109.1(7) . . ? O62 Cl2 O54 58.5(9) . . ? O52 Cl2 O54 106.3(7) . . ? O61 Cl2 O54 155.9(12) . . ? O51 Cl2 O54 104.5(7) . . ? O64 Cl2 O54 100.3(11) . . ? O74 Cl1 O71 114.3(11) . . ? O74 Cl1 O84 129.8(12) . . ? O71 Cl1 O84 44.9(10) . . ? O74 Cl1 O81 114.9(13) . . ? O71 Cl1 O81 122.7(12) . . ? O84 Cl1 O81 112.6(5) . . ? O74 Cl1 O83 36.4(10) . . ? O71 Cl1 O83 124.7(11) . . ? O84 Cl1 O83 109.1(5) . . ? O81 Cl1 O83 112.2(6) . . ? O74 Cl1 O72 111.0(11) . . ? O71 Cl1 O72 109.3(11) . . ? O84 Cl1 O72 119.0(13) . . ? O81 Cl1 O72 23.7(13) . . ? O83 Cl1 O72 124.2(14) . . ? O74 Cl1 O73 108.6(11) . . ? O71 Cl1 O73 108.3(11) . . ? O84 Cl1 O73 63.4(10) . . ? O81 Cl1 O73 81.8(11) . . ? O83 Cl1 O73 72.3(10) . . ? O72 Cl1 O73 104.9(11) . . ? O74 Cl1 O82 71.3(11) . . ? O71 Cl1 O82 64.2(11) . . ? O84 Cl1 O82 109.0(6) . . ? O81 Cl1 O82 107.1(5) . . ? O83 Cl1 O82 106.6(6) . . ? O72 Cl1 O82 83.6(12) . . ? O73 Cl1 O82 170.5(11) . . ? 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 O1 Cu1 Cu2 O3 8.19(15) . . . . ? O2 Cu1 Cu2 O3 -83.69(14) . . . . ? N2 Cu1 Cu2 O3 102.40(17) . . . . ? N1 Cu1 Cu2 O3 -176.42(17) . . . . ? O2 Cu1 Cu2 O3 -44.3(3) 3_576 . . . ? O1 Cu1 Cu2 O4 104.66(15) . . . . ? O2 Cu1 Cu2 O4 12.78(14) . . . . ? N2 Cu1 Cu2 O4 -161.14(17) . . . . ? N1 Cu1 Cu2 O4 -79.96(17) . . . . ? O2 Cu1 Cu2 O4 52.1(3) 3_576 . . . ? O1 Cu1 Cu2 N3 -164.12(16) . . . . ? O2 Cu1 Cu2 N3 104.00(17) . . . . ? N2 Cu1 Cu2 N3 -69.91(18) . . . . ? N1 Cu1 Cu2 N3 11.26(18) . . . . ? O2 Cu1 Cu2 N3 143.3(3) 3_576 . . . ? O1 Cu1 Cu2 N4 -82.38(17) . . . . ? O2 Cu1 Cu2 N4 -174.26(16) . . . . ? N2 Cu1 Cu2 N4 11.83(18) . . . . ? N1 Cu1 Cu2 N4 93.01(19) . . . . ? O2 Cu1 Cu2 N4 -134.9(3) 3_576 . . . ? O1 Cu1 Cu2 O1W 79.8(4) . . . . ? O2 Cu1 Cu2 O1W -12.1(4) . . . . ? N2 Cu1 Cu2 O1W 174.0(4) . . . . ? N1 Cu1 Cu2 O1W -104.8(4) . . . . ? O2 Cu1 Cu2 O1W 27.3(4) 3_576 . . . ? O1 Cu1 N1 C1 122.4(9) . . . . ? O2 Cu1 N1 C1 8.9(5) . . . . ? N2 Cu1 N1 C1 -178.1(5) . . . . ? O2 Cu1 N1 C1 -70.6(5) 3_576 . . . ? Cu2 Cu1 N1 C1 94.5(4) . . . . ? O1 Cu1 N1 C5 -54.2(11) . . . . ? O2 Cu1 N1 C5 -167.7(4) . . . . ? N2 Cu1 N1 C5 5.3(4) . . . . ? O2 Cu1 N1 C5 112.8(4) 3_576 . . . ? Cu2 Cu1 N1 C5 -82.1(4) . . . . ? O1 Cu1 N2 C10 -5.9(4) . . . . ? O2 Cu1 N2 C10 -125.3(10) . . . . ? N1 Cu1 N2 C10 -177.6(5) . . . . ? O2 Cu1 N2 C10 86.4(4) 3_576 . . . ? Cu2 Cu1 N2 C10 -82.1(4) . . . . ? O1 Cu1 N2 C6 165.2(3) . . . . ? O2 Cu1 N2 C6 45.8(12) . . . . ? N1 Cu1 N2 C6 -6.5(3) . . . . ? O2 Cu1 N2 C6 -102.5(3) 3_576 . . . ? Cu2 Cu1 N2 C6 88.9(3) . . . . ? O3 Cu2 N3 C11 -135.7(9) . . . . ? O4 Cu2 N3 C11 -11.1(5) . . . . ? N4 Cu2 N3 C11 178.1(5) . . . . ? O1W Cu2 N3 C11 79.9(5) . . . . ? Cu1 Cu2 N3 C11 -80.8(5) . . . . ? O3 Cu2 N3 C15 44.5(12) . . . . ? O4 Cu2 N3 C15 169.1(4) . . . . ? N4 Cu2 N3 C15 -1.7(4) . . . . ? O1W Cu2 N3 C15 -99.9(4) . . . . ? Cu1 Cu2 N3 C15 99.4(4) . . . . ? O3 Cu2 N4 C20 6.6(5) . . . . ? O4 Cu2 N4 C20 123.1(8) . . . . ? N3 Cu2 N4 C20 179.9(5) . . . . ? O1W Cu2 N4 C20 -87.2(5) . . . . ? Cu1 Cu2 N4 C20 86.3(5) . . . . ? O3 Cu2 N4 C16 -171.6(4) . . . . ? O4 Cu2 N4 C16 -55.0(10) . . . . ? N3 Cu2 N4 C16 1.8(4) . . . . ? O1W Cu2 N4 C16 94.7(4) . . . . ? Cu1 Cu2 N4 C16 -91.8(4) . . . . ? O2 Cu1 O1 C21 72.3(4) . . . . ? N2 Cu1 O1 C21 -100.0(4) . . . . ? N1 Cu1 O1 C21 -41.3(11) . . . . ? O2 Cu1 O1 C21 151.5(4) 3_576 . . . ? Cu2 Cu1 O1 C21 -12.7(4) . . . . ? O1 Cu1 O2 C24 -90.0(3) . . . . ? N2 Cu1 O2 C24 29.6(11) . . . . ? N1 Cu1 O2 C24 81.2(3) . . . . ? O2 Cu1 O2 C24 179.2(4) 3_576 . . . ? Cu2 Cu1 O2 C24 -13.7(3) . . . . ? O1 Cu1 O2 Cu1 90.87(14) . . . 3_576 ? N2 Cu1 O2 Cu1 -149.5(10) . . . 3_576 ? N1 Cu1 O2 Cu1 -97.95(16) . . . 3_576 ? O2 Cu1 O2 Cu1 0.0 3_576 . . 3_576 ? Cu2 Cu1 O2 Cu1 167.16(11) . . . 3_576 ? O4 Cu2 O3 C21 -76.7(4) . . . . ? N3 Cu2 O3 C21 47.9(12) . . . . ? N4 Cu2 O3 C21 93.4(4) . . . . ? O1W Cu2 O3 C21 -167.6(4) . . . . ? Cu1 Cu2 O3 C21 -8.0(4) . . . . ? O3 Cu2 O4 C24 57.2(5) . . . . ? N3 Cu2 O4 C24 -115.2(5) . . . . ? N4 Cu2 O4 C24 -59.4(11) . . . . ? O1W Cu2 O4 C24 150.5(5) . . . . ? Cu1 Cu2 O4 C24 -20.7(5) . . . . ? C5 N1 C1 C2 -0.2(8) . . . . ? Cu1 N1 C1 C2 -176.7(4) . . . . ? N1 C1 C2 C3 -0.1(9) . . . . ? C1 C2 C3 C4 0.2(9) . . . . ? C2 C3 C4 C5 0.0(10) . . . . ? C1 N1 C5 C4 0.3(8) . . . . ? Cu1 N1 C5 C4 177.3(4) . . . . ? C1 N1 C5 C6 179.8(5) . . . . ? Cu1 N1 C5 C6 -3.2(6) . . . . ? C3 C4 C5 N1 -0.3(9) . . . . ? C3 C4 C5 C6 -179.7(6) . . . . ? C10 N2 C6 C7 1.4(8) . . . . ? Cu1 N2 C6 C7 -170.3(4) . . . . ? C10 N2 C6 C5 178.3(5) . . . . ? Cu1 N2 C6 C5 6.6(6) . . . . ? N1 C5 C6 N2 -2.2(7) . . . . ? C4 C5 C6 N2 177.3(5) . . . . ? N1 C5 C6 C7 174.6(5) . . . . ? C4 C5 C6 C7 -5.9(9) . . . . ? N2 C6 C7 C8 -0.4(9) . . . . ? C5 C6 C7 C8 -177.0(6) . . . . ? C6 C7 C8 C9 0.1(10) . . . . ? C7 C8 C9 C10 -0.8(9) . . . . ? C6 N2 C10 C9 -2.3(8) . . . . ? Cu1 N2 C10 C9 168.5(4) . . . . ? C8 C9 C10 N2 2.0(9) . . . . ? C15 N3 C11 C12 -3.1(8) . . . . ? Cu2 N3 C11 C12 177.1(4) . . . . ? N3 C11 C12 C13 0.8(9) . . . . ? C11 C12 C13 C14 1.4(10) . . . . ? C12 C13 C14 C15 -1.3(10) . . . . ? C11 N3 C15 C14 3.2(8) . . . . ? Cu2 N3 C15 C14 -176.9(4) . . . . ? C11 N3 C15 C16 -178.5(5) . . . . ? Cu2 N3 C15 C16 1.3(6) . . . . ? C13 C14 C15 N3 -1.1(9) . . . . ? C13 C14 C15 C16 -179.1(6) . . . . ? C20 N4 C16 C17 0.1(8) . . . . ? Cu2 N4 C16 C17 178.3(4) . . . . ? C20 N4 C16 C15 -179.8(5) . . . . ? Cu2 N4 C16 C15 -1.6(6) . . . . ? N3 C15 C16 N4 0.2(7) . . . . ? C14 C15 C16 N4 178.4(5) . . . . ? N3 C15 C16 C17 -179.7(5) . . . . ? C14 C15 C16 C17 -1.5(9) . . . . ? N4 C16 C17 C18 -0.1(9) . . . . ? C15 C16 C17 C18 179.8(6) . . . . ? C16 C17 C18 C19 0.2(10) . . . . ? C17 C18 C19 C20 -0.3(10) . . . . ? C16 N4 C20 C19 -0.2(8) . . . . ? Cu2 N4 C20 C19 -178.2(4) . . . . ? C18 C19 C20 N4 0.3(9) . . . . ? Cu2 O3 C21 O1 2.0(7) . . . . ? Cu2 O3 C21 C22 -177.4(3) . . . . ? Cu1 O1 C21 O3 12.0(7) . . . . ? Cu1 O1 C21 C22 -168.6(3) . . . . ? O3 C21 C22 C23 13.1(7) . . . . ? O1 C21 C22 C23 -166.3(4) . . . . ? C21 C22 C23 C24 -179.1(4) . . . 2_545 ? Cu2 O4 C24 O2 17.0(8) . . . . ? Cu2 O4 C24 C23 -164.9(4) . . . 2 ? Cu1 O2 C24 O4 6.5(6) . . . . ? Cu1 O2 C24 O4 -174.8(3) 3_576 . . . ? Cu1 O2 C24 C23 -171.7(3) . . . 2 ? Cu1 O2 C24 C23 7.1(7) 3_576 . . 2 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.600 _refine_diff_density_min -0.723 _refine_diff_density_rms 0.094