# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Ivan Bernal' 'Frank R. Fronczek' 'Manas K. Saha' _publ_contact_author_name 'Prof Ivan Bernal' _publ_contact_author_address ; Department of Chemistry University of Houston Houston UNITED STATES OF AMERICA ; _publ_contact_author_email IBERNAL@UH.EDU _publ_requested_journal 'Chemical Communications' _publ_section_title ; Novel ambient light induced trimerization of a simple copper(II) monomeric Schiff base complex ; data_Compound1 _database_code_CSD 219122 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_sum 'C48 H70 Cu2 N10 O10' _chemical_formula_weight 1074.22 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.587(3) _cell_length_b 25.273(6) _cell_length_c 39.355(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 10530(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4528 _exptl_special_details ? #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.872 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.2885 _diffrn_reflns_av_unetI/netI 0.1103 _diffrn_reflns_number 6787 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 21.97 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 6418 _reflns_number_gt 3184 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _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 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1151P)^2^] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 6418 _refine_ls_number_parameters 639 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1688 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1993 _refine_ls_wR_factor_gt 0.1369 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 0.532 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.098 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9383(8) 0.6295(4) 0.1859(3) 0.046(2) Uani 1 1 d . . . C2 C 1.0435(8) 0.6028(4) 0.1718(2) 0.054(3) Uani 1 1 d . . . H1 H 1.0712 0.6115 0.15 0.065 Uiso 1 1 calc R . . C3 C 1.1048(10) 0.5644(4) 0.1899(3) 0.074(3) Uani 1 1 d . . . H2 H 1.1722 0.5466 0.1799 0.089 Uiso 1 1 calc R . . C4 C 1.0687(12) 0.5510(4) 0.2232(3) 0.075(3) Uani 1 1 d . . . H3 H 1.1124 0.5255 0.2355 0.09 Uiso 1 1 calc R . . C5 C 0.9681(10) 0.5765(4) 0.2368(3) 0.060(3) Uani 1 1 d . . . H4 H 0.9424 0.5677 0.2586 0.072 Uiso 1 1 calc R . . C6 C 0.9008(8) 0.6159(3) 0.2191(2) 0.041(2) Uani 1 1 d . . . C7 C 0.8004(9) 0.6428(4) 0.2360(2) 0.048(2) Uani 1 1 d . . . H5 H 0.7905 0.6355 0.259 0.058 Uiso 1 1 calc R . . C8 C 0.6366(8) 0.7035(3) 0.2464(2) 0.050(2) Uani 1 1 d . . . H6 H 0.6339 0.6848 0.268 0.06 Uiso 1 1 calc R . . H7 H 0.552 0.7038 0.237 0.06 Uiso 1 1 calc R . . C9 C 0.6807(9) 0.7595(4) 0.2521(3) 0.058(3) Uani 1 1 d . . . H8 H 0.7693 0.759 0.2584 0.07 Uiso 1 1 calc R . . H9 H 0.6339 0.7746 0.271 0.07 Uiso 1 1 calc R . . C10 C 0.6637(9) 0.7943(4) 0.2211(3) 0.058(3) Uani 1 1 d . . . H10 H 0.5762 0.7918 0.2139 0.07 Uiso 1 1 calc R . . H11 H 0.6787 0.8307 0.2279 0.07 Uiso 1 1 calc R . . C11 C 0.7121(11) 0.8190(4) 0.1650(3) 0.079(3) Uani 1 1 d . . . H12 H 0.6248 0.8147 0.1591 0.119 Uiso 1 1 calc R . . H13 H 0.7639 0.8121 0.1455 0.119 Uiso 1 1 calc R . . H14 H 0.7262 0.8546 0.1727 0.119 Uiso 1 1 calc R . . C12 C 0.8785(9) 0.7895(4) 0.1994(3) 0.066(3) Uani 1 1 d . . . H15 H 0.9276 0.782 0.1795 0.098 Uiso 1 1 calc R . . H16 H 0.9022 0.7656 0.2173 0.098 Uiso 1 1 calc R . . H17 H 0.8937 0.8252 0.2065 0.098 Uiso 1 1 calc R . . C13 C 0.4487(8) 0.7069(3) 0.1536(2) 0.035(2) Uani 1 1 d . . . C14 C 0.3197(9) 0.7042(4) 0.1618(3) 0.059(3) Uani 1 1 d . . . H18 H 0.2991 0.6942 0.1838 0.07 Uiso 1 1 calc R . . C15 C 0.2258(10) 0.7144(4) 0.1411(3) 0.067(3) Uani 1 1 d . . . H19 H 0.1424 0.7131 0.1485 0.081 Uiso 1 1 calc R . . C16 C 0.2565(10) 0.7277(4) 0.1074(3) 0.066(3) Uani 1 1 d . . . H20 H 0.1928 0.7339 0.0917 0.079 Uiso 1 1 calc R . . C17 C 0.3803(10) 0.7313(4) 0.0978(2) 0.054(3) Uani 1 1 d . . . H21 H 0.4005 0.741 0.0757 0.065 Uiso 1 1 calc R . . C18 C 0.4765(9) 0.7205(3) 0.1210(2) 0.045(2) Uani 1 1 d . . . C19 C 0.6058(10) 0.7209(4) 0.1084(2) 0.050(3) Uani 1 1 d . . . H22 H 0.6164 0.7312 0.0859 0.06 Uiso 1 1 calc R . . C20 C 0.8217(8) 0.7077(4) 0.1033(2) 0.049(3) Uani 1 1 d . . . H23 H 0.8943 0.7167 0.1172 0.059 Uiso 1 1 calc R . . H24 H 0.8149 0.7338 0.0853 0.059 Uiso 1 1 calc R . . C21 C 0.8401(8) 0.6532(4) 0.0879(2) 0.051(3) Uani 1 1 d . . . H25 H 0.8463 0.6273 0.106 0.061 Uiso 1 1 calc R . . H26 H 0.7671 0.6444 0.0741 0.061 Uiso 1 1 calc R . . C22 C 0.9555(9) 0.6507(4) 0.0666(3) 0.072(3) Uani 1 1 d . . . H27 H 0.9538 0.6799 0.0506 0.087 Uiso 1 1 calc R . . H28 H 1.0287 0.6555 0.0811 0.087 Uiso 1 1 calc R . . C23 C 0.9864(14) 0.5539(5) 0.0702(3) 0.120(5) Uani 1 1 d . . . H30 H 1.0617 0.5578 0.0835 0.18 Uiso 1 1 calc R . . H31 H 0.993 0.5227 0.0564 0.18 Uiso 1 1 calc R . . H32 H 0.9147 0.5508 0.085 0.18 Uiso 1 1 calc R . . C24 C 1.0699(13) 0.6080(7) 0.0206(4) 0.158(7) Uani 1 1 d . . . H33 H 1.0461 0.6363 0.0056 0.236 Uiso 1 1 calc R . . H34 H 1.0777 0.5758 0.0079 0.236 Uiso 1 1 calc R . . H35 H 1.1494 0.6163 0.0311 0.236 Uiso 1 1 calc R . . C25 C 0.6951(10) 0.9133(4) 0.1059(3) 0.057(3) Uani 1 1 d . . . C26 C 0.6328(10) 0.8837(5) 0.0816(3) 0.078(3) Uani 1 1 d . . . H36 H 0.6808 0.8634 0.0667 0.094 Uiso 1 1 calc R . . C27 C 0.5032(12) 0.8829(6) 0.0782(3) 0.092(4) Uani 1 1 d . . . H37 H 0.4649 0.8622 0.0616 0.11 Uiso 1 1 calc R . . C28 C 0.4325(12) 0.9130(6) 0.0995(4) 0.099(4) Uani 1 1 d . . . H38 H 0.3451 0.9137 0.0971 0.118 Uiso 1 1 calc R . . C29 C 0.4870(10) 0.9418(5) 0.1242(3) 0.083(4) Uani 1 1 d . . . H39 H 0.4367 0.9612 0.139 0.1 Uiso 1 1 calc R . . C30 C 0.6197(9) 0.9431(4) 0.1278(3) 0.052(3) Uani 1 1 d . . . C31 C 0.6746(10) 0.9761(4) 0.1542(3) 0.068(3) Uani 1 1 d . . . H40 H 0.6199 0.9984 0.1659 0.082 Uiso 1 1 calc R . . C32 C 0.8269(9) 1.0189(4) 0.1864(3) 0.060(3) Uani 1 1 d . . . H41 H 0.884 1.0044 0.2033 0.072 Uiso 1 1 calc R . . H42 H 0.7522 1.0316 0.1981 0.072 Uiso 1 1 calc R . . C33 C 0.8897(10) 1.0643(4) 0.1689(3) 0.067(3) Uani 1 1 d . . . H43 H 0.8991 1.093 0.1851 0.081 Uiso 1 1 calc R . . H44 H 0.8347 1.0767 0.1509 0.081 Uiso 1 1 calc R . . C34 C 1.0180(10) 1.0521(4) 0.1538(3) 0.067(3) Uani 1 1 d . . . H45 H 1.0557 1.0851 0.1463 0.08 Uiso 1 1 calc R . . H46 H 1.0714 1.0379 0.1717 0.08 Uiso 1 1 calc R . . C35 C 0.9491(12) 1.0347(4) 0.0958(3) 0.091(4) Uani 1 1 d . . . H47 H 0.9866 1.0673 0.0882 0.136 Uiso 1 1 calc R . . H48 H 0.8629 1.041 0.1022 0.136 Uiso 1 1 calc R . . H49 H 0.9517 1.0093 0.0777 0.136 Uiso 1 1 calc R . . C36 C 1.1497(10) 1.0043(5) 0.1146(3) 0.084(4) Uani 1 1 d . . . H50 H 1.1878 1.0365 0.1068 0.126 Uiso 1 1 calc R . . H51 H 1.1507 0.9786 0.0966 0.126 Uiso 1 1 calc R . . H52 H 1.1964 0.9909 0.1337 0.126 Uiso 1 1 calc R . . C37 C 1.1191(10) 0.9185(3) 0.1978(2) 0.050(3) Uani 1 1 d . . . C38 C 1.1697(10) 0.9350(4) 0.2291(2) 0.056(3) Uani 1 1 d . . . H53 H 1.1212 0.9566 0.2431 0.067 Uiso 1 1 calc R . . C39 C 1.2866(11) 0.9205(4) 0.2395(3) 0.064(3) Uani 1 1 d . . . H54 H 1.3184 0.933 0.26 0.077 Uiso 1 1 calc R . . C40 C 1.3590(10) 0.8870(4) 0.2194(3) 0.070(3) Uani 1 1 d . . . H55 H 1.4393 0.8771 0.2265 0.084 Uiso 1 1 calc R . . C41 C 1.3138(9) 0.8685(4) 0.1894(3) 0.061(3) Uani 1 1 d . . . H56 H 1.3622 0.8454 0.1764 0.073 Uiso 1 1 calc R . . C42 C 1.1931(8) 0.8843(4) 0.1779(2) 0.044(2) Uani 1 1 d . . . C43 C 1.1492(9) 0.8626(3) 0.1468(3) 0.052(2) Uani 1 1 d . . . H57 H 1.2001 0.8366 0.1372 0.062 Uiso 1 1 calc R . . C44 C 1.0222(9) 0.8436(4) 0.0996(3) 0.061(3) Uani 1 1 d . . . H58 H 0.934 0.8333 0.0995 0.073 Uiso 1 1 calc R . . H59 H 1.0728 0.8116 0.1 0.073 Uiso 1 1 calc R . . C45 C 1.0506(9) 0.8740(4) 0.0676(2) 0.066(3) Uani 1 1 d . . . H60 H 1.0094 0.9083 0.0683 0.08 Uiso 1 1 calc R . . H61 H 1.1409 0.8796 0.0655 0.08 Uiso 1 1 calc R . . C46 C 1.0036(11) 0.8430(4) 0.0379(3) 0.075(3) Uani 1 1 d . . . H62 H 0.9195 0.8298 0.0428 0.09 Uiso 1 1 calc R . . H63 H 1.0585 0.8129 0.0341 0.09 Uiso 1 1 calc R . . C47 C 0.9016(15) 0.9181(6) 0.0073(4) 0.140(6) Uani 1 1 d . . . H65 H 0.9133 0.9397 0.0271 0.21 Uiso 1 1 calc R . . H66 H 0.8196 0.9019 0.0081 0.21 Uiso 1 1 calc R . . H67 H 0.9082 0.9396 -0.0128 0.21 Uiso 1 1 calc R . . C48 C 0.9809(12) 0.8446(5) -0.0246(3) 0.101(4) Uani 1 1 d . . . H70 H 0.9847 0.8672 -0.0442 0.151 Uiso 1 1 calc R . . H68 H 0.8998 0.8276 -0.0237 0.151 Uiso 1 1 calc R . . H69 H 1.0459 0.8182 -0.0262 0.151 Uiso 1 1 calc R . . N1 N 0.7227(7) 0.6757(3) 0.22300(17) 0.0404(18) Uani 1 1 d . . . N2 N 0.7442(7) 0.7827(3) 0.19163(19) 0.0474(19) Uani 1 1 d . . . N3 N 0.7057(7) 0.7088(3) 0.12445(19) 0.0460(19) Uani 1 1 d . . . N4 N 0.9703(10) 0.6015(4) 0.0477(3) 0.076(3) Uani 1 1 d . . . N5 N 0.7910(8) 0.9774(3) 0.16288(18) 0.0458(19) Uani 1 1 d . . . N6 N 1.0191(7) 1.0146(3) 0.1249(2) 0.056(2) Uani 1 1 d . . . N7 N 1.0480(7) 0.8742(3) 0.13003(18) 0.0463(19) Uani 1 1 d . . . N8 N 0.9998(10) 0.8765(4) 0.0064(3) 0.078(3) Uani 1 1 d . . . N9 N 0.2514(11) 0.9584(5) 1.0035(3) 0.091(3) Uani 1 1 d . . . N10 N 0.237(2) 0.7499(12) 0.9986(7) 0.200(12) Uani 1 1 d . . . O1 O 0.8826(6) 0.6657(3) 0.16731(16) 0.0553(17) Uani 1 1 d . . . O2 O 0.5318(5) 0.6963(2) 0.17781(15) 0.0531(16) Uani 1 1 d . . . O3 O 0.8186(6) 0.9125(3) 0.10740(16) 0.067(2) Uani 1 1 d . . . O4 O 1.0064(6) 0.9343(2) 0.18832(16) 0.0571(17) Uani 1 1 d . . . O5 O 0.2355(8) 0.9198(4) 0.9855(2) 0.104(3) Uani 1 1 d . . . O6 O 0.3500(12) 0.9826(4) 1.0004(3) 0.160(5) Uani 1 1 d . . . O7 O 0.1744(11) 0.9728(4) 1.0247(3) 0.130(4) Uani 1 1 d . . . O8 O 0.279(3) 0.7917(12) 0.9937(10) 0.42(2) Uani 1 1 d . . . O9 O 0.229(3) 0.7318(13) 0.9728(5) 0.35(2) Uani 1 1 d . . . O10 O 0.2040(13) 0.7322(6) 1.0230(3) 0.184(6) Uani 1 1 d . . . Cu1 Cu 0.71430(10) 0.69408(4) 0.17385(3) 0.0401(3) Uani 1 1 d . . . Cu2 Cu 0.92385(10) 0.92973(4) 0.14517(3) 0.0452(4) Uani 1 1 d . . . H29 H 0.902(8) 0.592(4) 0.036(2) 0.06(3) Uiso 1 1 d . . . H64 H 1.081(10) 0.890(4) -0.005(2) 0.09(4) 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 C1 0.032(5) 0.039(6) 0.067(7) -0.012(5) 0.001(5) 0.005(5) C2 0.052(6) 0.061(6) 0.050(6) -0.005(6) -0.013(5) 0.008(6) C3 0.058(7) 0.072(8) 0.091(9) -0.020(7) -0.012(7) 0.011(6) C4 0.075(8) 0.055(7) 0.095(10) 0.001(7) -0.032(8) 0.020(7) C5 0.074(8) 0.047(6) 0.058(7) 0.007(5) -0.021(6) -0.005(6) C6 0.045(6) 0.039(5) 0.038(6) -0.011(5) -0.004(5) -0.006(5) C7 0.054(6) 0.044(6) 0.047(6) 0.009(5) -0.002(5) -0.014(5) C8 0.040(5) 0.058(6) 0.051(6) 0.004(5) 0.007(5) -0.006(5) C9 0.048(6) 0.067(7) 0.059(7) -0.020(6) 0.021(5) -0.005(5) C10 0.054(6) 0.041(6) 0.080(8) -0.003(5) 0.006(6) -0.006(5) C11 0.100(9) 0.040(6) 0.096(9) 0.009(6) -0.012(7) -0.016(6) C12 0.050(7) 0.069(7) 0.077(8) -0.014(6) 0.013(6) -0.019(5) C13 0.034(6) 0.044(6) 0.029(5) 0.002(4) -0.005(4) 0.001(4) C14 0.050(7) 0.069(8) 0.057(7) 0.012(5) -0.002(5) -0.001(5) C15 0.055(7) 0.076(8) 0.071(8) -0.003(6) -0.004(7) 0.007(6) C16 0.048(7) 0.069(7) 0.081(9) -0.023(6) -0.030(6) 0.028(6) C17 0.061(7) 0.059(7) 0.044(6) -0.006(5) -0.013(5) 0.018(5) C18 0.052(6) 0.044(6) 0.038(6) 0.001(5) 0.000(5) 0.008(5) C19 0.078(8) 0.044(6) 0.026(5) -0.003(4) -0.010(5) -0.005(5) C20 0.044(6) 0.067(7) 0.037(5) 0.002(5) 0.010(5) -0.004(5) C21 0.047(6) 0.062(7) 0.043(6) -0.014(5) 0.009(5) -0.006(5) C22 0.059(7) 0.086(9) 0.072(8) -0.011(7) 0.016(6) -0.016(6) C23 0.186(16) 0.093(10) 0.081(10) -0.012(8) -0.019(10) 0.063(11) C24 0.129(12) 0.194(17) 0.150(14) -0.074(13) 0.092(12) -0.034(12) C25 0.048(7) 0.065(7) 0.057(7) 0.008(6) -0.010(6) -0.004(6) C26 0.048(7) 0.114(10) 0.073(8) 0.005(8) -0.007(6) -0.005(7) C27 0.067(9) 0.125(12) 0.084(10) 0.004(9) -0.011(8) -0.023(9) C28 0.051(8) 0.134(13) 0.111(11) -0.012(10) -0.012(9) -0.016(9) C29 0.038(7) 0.124(11) 0.087(9) 0.019(8) 0.014(7) 0.018(7) C30 0.044(6) 0.065(7) 0.047(6) 0.019(6) 0.008(6) 0.011(5) C31 0.049(8) 0.066(8) 0.090(9) 0.012(7) 0.022(7) 0.018(6) C32 0.063(7) 0.048(7) 0.071(7) -0.003(6) 0.011(6) 0.031(5) C33 0.075(8) 0.056(7) 0.071(7) -0.022(6) -0.002(6) 0.016(6) C34 0.078(8) 0.044(6) 0.079(8) -0.001(6) -0.004(6) -0.010(6) C35 0.127(11) 0.073(8) 0.073(8) 0.022(7) 0.000(8) 0.005(8) C36 0.079(9) 0.085(9) 0.088(9) -0.011(7) 0.021(7) -0.014(7) C37 0.060(7) 0.037(6) 0.054(7) 0.017(5) 0.008(6) -0.004(5) C38 0.067(7) 0.045(6) 0.056(7) -0.001(5) -0.013(6) 0.003(5) C39 0.073(8) 0.048(6) 0.070(7) 0.010(6) -0.012(7) -0.007(6) C40 0.055(7) 0.061(7) 0.093(9) 0.015(7) -0.021(7) 0.001(6) C41 0.052(7) 0.062(7) 0.068(7) 0.009(6) -0.012(6) 0.009(5) C42 0.044(6) 0.051(6) 0.038(6) -0.003(5) -0.004(5) 0.004(5) C43 0.047(6) 0.041(6) 0.067(7) 0.002(5) 0.008(6) 0.011(5) C44 0.062(7) 0.048(6) 0.072(8) -0.009(6) 0.003(6) 0.016(5) C45 0.055(7) 0.086(8) 0.058(7) -0.009(6) 0.004(6) 0.001(6) C46 0.103(9) 0.074(8) 0.048(7) -0.016(6) 0.012(6) -0.015(7) C47 0.149(14) 0.126(13) 0.144(14) -0.035(11) -0.071(11) 0.046(12) C48 0.135(12) 0.125(11) 0.042(7) -0.012(7) -0.010(7) -0.029(10) N1 0.040(4) 0.037(4) 0.044(4) 0.008(4) 0.000(4) -0.008(4) N2 0.055(5) 0.036(4) 0.051(5) 0.012(4) 0.002(4) -0.002(4) N3 0.043(5) 0.042(5) 0.053(5) 0.006(4) -0.008(4) -0.007(4) N4 0.065(7) 0.091(8) 0.073(7) -0.030(6) 0.015(6) 0.002(6) N5 0.047(5) 0.043(5) 0.047(5) -0.004(4) 0.006(4) 0.007(4) N6 0.057(5) 0.047(5) 0.064(6) 0.005(5) 0.003(5) -0.001(4) N7 0.047(5) 0.050(5) 0.042(5) -0.019(4) 0.001(4) 0.008(4) N8 0.064(6) 0.083(7) 0.086(8) -0.007(6) -0.003(6) -0.016(6) N9 0.081(9) 0.079(8) 0.112(10) -0.003(7) 0.017(7) -0.028(7) N10 0.161(16) 0.28(3) 0.154(19) 0.15(2) 0.056(16) 0.130(18) O1 0.048(4) 0.056(4) 0.061(4) 0.004(4) 0.009(3) 0.014(3) O2 0.038(4) 0.063(4) 0.058(4) 0.007(4) 0.006(3) 0.000(3) O3 0.034(4) 0.099(6) 0.068(5) -0.015(4) -0.003(3) 0.009(4) O4 0.044(4) 0.060(4) 0.067(4) -0.010(4) -0.003(4) 0.020(3) O5 0.103(7) 0.102(7) 0.107(7) -0.050(6) 0.027(5) -0.044(6) O6 0.158(10) 0.148(10) 0.174(11) -0.065(8) 0.057(8) -0.084(9) O7 0.153(9) 0.103(7) 0.135(9) -0.028(6) 0.070(8) -0.006(7) O8 0.51(5) 0.29(3) 0.45(4) 0.09(3) 0.32(4) 0.00(3) O9 0.56(5) 0.37(3) 0.106(13) 0.097(18) 0.02(2) 0.20(3) O10 0.222(15) 0.248(15) 0.083(8) 0.068(9) 0.003(9) 0.015(12) Cu1 0.0397(6) 0.0404(6) 0.0403(6) 0.0035(6) 0.0020(5) 0.0009(5) Cu2 0.0395(6) 0.0461(7) 0.0500(7) -0.0040(6) 0.0021(6) 0.0084(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.311(10) . ? C1 C6 1.409(12) . ? C1 C2 1.415(12) . ? C2 C3 1.370(14) . ? C3 C4 1.407(15) . ? C4 C5 1.354(14) . ? C5 C6 1.408(12) . ? C6 C7 1.425(12) . ? C7 N1 1.277(10) . ? C8 N1 1.474(10) . ? C8 C9 1.507(12) . ? C9 C10 1.516(13) . ? C10 N2 1.469(11) . ? C11 N2 1.433(11) . ? C12 N2 1.464(11) . ? C13 O2 1.323(9) . ? C13 C18 1.360(11) . ? C13 C14 1.405(12) . ? C14 C15 1.310(13) . ? C15 C16 1.407(14) . ? C16 C17 1.366(13) . ? C17 C18 1.395(12) . ? C18 C19 1.457(13) . ? C19 N3 1.269(11) . ? C20 N3 1.483(10) . ? C20 C21 1.517(12) . ? C21 C22 1.483(12) . ? C22 N4 1.458(13) . ? C23 N4 1.503(15) . ? C24 N4 1.508(14) . ? C25 O3 1.309(11) . ? C25 C26 1.383(13) . ? C25 C30 1.394(13) . ? C26 C27 1.379(14) . ? C27 C28 1.359(17) . ? C28 C29 1.342(16) . ? C29 C30 1.413(13) . ? C30 C31 1.453(14) . ? C31 N5 1.279(12) . ? C32 N5 1.450(11) . ? C32 C33 1.494(13) . ? C33 C34 1.514(13) . ? C34 N6 1.483(12) . ? C35 N6 1.456(12) . ? C36 N6 1.464(12) . ? C37 O4 1.313(11) . ? C37 C38 1.403(12) . ? C37 C42 1.407(12) . ? C38 C39 1.354(13) . ? C39 C40 1.391(14) . ? C40 C41 1.356(13) . ? C41 C42 1.413(11) . ? C42 C43 1.417(12) . ? C43 N7 1.292(11) . ? C44 N7 1.450(11) . ? C44 C45 1.506(13) . ? C45 C46 1.491(13) . ? C46 N8 1.500(13) . ? C47 N8 1.479(15) . ? C48 N8 1.479(13) . ? N1 Cu1 1.991(7) . ? N2 Cu1 2.368(7) . ? N3 Cu1 1.981(7) . ? N5 Cu2 1.978(7) . ? N7 Cu2 2.014(7) . ? N9 O6 1.216(12) . ? N9 O5 1.219(12) . ? N9 O7 1.220(12) . ? N10 O10 1.115(18) . ? N10 O9 1.12(4) . ? N10 O8 1.16(4) . ? O1 Cu1 1.939(6) . ? O2 Cu1 1.939(6) . ? O3 Cu2 1.909(6) . ? O4 Cu2 1.913(6) . ? O8 O9 1.81(4) . ? 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 C1 C6 124.1(8) . . ? O1 C1 C2 117.8(9) . . ? C6 C1 C2 118.1(9) . . ? C3 C2 C1 120.4(10) . . ? C2 C3 C4 121.8(10) . . ? C5 C4 C3 117.8(10) . . ? C4 C5 C6 122.7(10) . . ? C5 C6 C1 119.2(9) . . ? C5 C6 C7 119.0(9) . . ? C1 C6 C7 121.8(8) . . ? N1 C7 C6 127.3(9) . . ? N1 C8 C9 110.4(7) . . ? C8 C9 C10 112.9(8) . . ? N2 C10 C9 116.8(8) . . ? O2 C13 C18 125.9(8) . . ? O2 C13 C14 118.1(8) . . ? C18 C13 C14 116.0(8) . . ? C15 C14 C13 125.9(10) . . ? C14 C15 C16 117.2(10) . . ? C17 C16 C15 119.9(9) . . ? C16 C17 C18 120.4(9) . . ? C13 C18 C17 120.6(9) . . ? C13 C18 C19 121.8(8) . . ? C17 C18 C19 117.5(9) . . ? N3 C19 C18 127.7(8) . . ? N3 C20 C21 110.3(7) . . ? C22 C21 C20 111.8(8) . . ? N4 C22 C21 114.5(8) . . ? O3 C25 C26 119.9(10) . . ? O3 C25 C30 123.6(9) . . ? C26 C25 C30 116.5(10) . . ? C27 C26 C25 123.3(12) . . ? C28 C27 C26 118.7(13) . . ? C29 C28 C27 120.9(12) . . ? C28 C29 C30 120.8(12) . . ? C25 C30 C29 119.7(11) . . ? C25 C30 C31 121.4(9) . . ? C29 C30 C31 118.9(10) . . ? N5 C31 C30 126.3(10) . . ? N5 C32 C33 112.3(8) . . ? C32 C33 C34 115.1(8) . . ? N6 C34 C33 116.0(8) . . ? O4 C37 C38 120.4(9) . . ? O4 C37 C42 122.3(9) . . ? C38 C37 C42 117.4(9) . . ? C39 C38 C37 122.2(10) . . ? C38 C39 C40 119.7(10) . . ? C41 C40 C39 120.7(10) . . ? C40 C41 C42 120.1(10) . . ? C37 C42 C41 119.8(9) . . ? C37 C42 C43 122.4(8) . . ? C41 C42 C43 117.7(9) . . ? N7 C43 C42 128.8(8) . . ? N7 C44 C45 112.5(8) . . ? C46 C45 C44 108.7(9) . . ? C45 C46 N8 111.1(9) . . ? C7 N1 C8 117.3(8) . . ? C7 N1 Cu1 124.7(6) . . ? C8 N1 Cu1 118.0(6) . . ? C11 N2 C12 107.9(8) . . ? C11 N2 C10 108.2(8) . . ? C12 N2 C10 112.1(7) . . ? C11 N2 Cu1 111.0(6) . . ? C12 N2 Cu1 107.5(5) . . ? C10 N2 Cu1 110.2(5) . . ? C19 N3 C20 114.5(8) . . ? C19 N3 Cu1 124.9(7) . . ? C20 N3 Cu1 120.6(6) . . ? C22 N4 C23 113.3(9) . . ? C22 N4 C24 110.0(10) . . ? C23 N4 C24 115.1(11) . . ? C31 N5 C32 116.3(8) . . ? C31 N5 Cu2 125.1(7) . . ? C32 N5 Cu2 118.6(6) . . ? C35 N6 C36 109.0(9) . . ? C35 N6 C34 112.1(8) . . ? C36 N6 C34 109.4(8) . . ? C43 N7 C44 117.3(8) . . ? C43 N7 Cu2 123.2(6) . . ? C44 N7 Cu2 119.5(6) . . ? C48 N8 C47 108.1(10) . . ? C48 N8 C46 112.3(9) . . ? C47 N8 C46 113.6(11) . . ? O6 N9 O5 117.6(12) . . ? O6 N9 O7 119.5(13) . . ? O5 N9 O7 122.9(11) . . ? O10 N10 O9 126(5) . . ? O10 N10 O8 129(5) . . ? O9 N10 O8 105(3) . . ? C1 O1 Cu1 126.7(6) . . ? C13 O2 Cu1 127.6(5) . . ? C25 O3 Cu2 127.9(6) . . ? C37 O4 Cu2 130.5(6) . . ? N10 O8 O9 37(2) . . ? N10 O9 O8 38.6(18) . . ? O1 Cu1 O2 159.6(3) . . ? O1 Cu1 N3 88.9(3) . . ? O2 Cu1 N3 91.6(3) . . ? O1 Cu1 N1 90.1(3) . . ? O2 Cu1 N1 88.5(3) . . ? N3 Cu1 N1 177.3(3) . . ? O1 Cu1 N2 105.5(3) . . ? O2 Cu1 N2 94.7(3) . . ? N3 Cu1 N2 96.8(3) . . ? N1 Cu1 N2 85.8(3) . . ? O3 Cu2 O4 166.4(3) . . ? O3 Cu2 N5 89.9(3) . . ? O4 Cu2 N5 88.6(3) . . ? O3 Cu2 N7 89.5(3) . . ? O4 Cu2 N7 90.4(3) . . ? N5 Cu2 N7 173.1(3) . . ? # END OF CIF data_Compound2 _database_code_CSD 219123 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_moiety 'C52 H86 Cl8 Cu2 N8 O9' _chemical_formula_sum 'C52 H86 Cl8 Cu2 N8 O9' _chemical_formula_weight 1377.97 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.206(6) _cell_length_b 15.113(6) _cell_length_c 16.999(8) _cell_angle_alpha 107.37(2) _cell_angle_beta 92.56(2) _cell_angle_gamma 99.28(2) _cell_volume 3180(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_measurement_reflns_used 10691 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.062 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7978 _exptl_absorpt_correction_T_max 0.9654 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device 'KappaCCD (with Oxford Cryostream)' _diffrn_measurement_method ' \w scans with \k offsets' _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0814 _diffrn_reflns_av_unetI/netI 0.1355 _diffrn_reflns_number 20881 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 11060 _reflns_number_gt 6005 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _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 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0848P)^2^] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0000(4) _refine_ls_number_reflns 11060 _refine_ls_number_parameters 1000 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1411 _refine_ls_R_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.1785 _refine_ls_wR_factor_gt 0.1477 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 2.308 _refine_ls_shift/su_mean 0.006 _refine_diff_density_max 1.558 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.098 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7298(5) 0.3733(5) 0.2188(4) 0.0261(15) Uani 1 1 d . . . C2 C 0.8317(5) 0.3945(6) 0.2598(5) 0.0344(18) Uani 1 1 d . . . C3 C 0.8869(5) 0.3237(6) 0.2565(5) 0.0343(18) Uani 1 1 d . . . C4 C 0.8476(5) 0.2307(6) 0.2129(5) 0.0365(18) Uani 1 1 d . . . C5 C 0.7497(5) 0.2076(5) 0.1709(4) 0.0360(18) Uani 1 1 d . . . C6 C 0.6896(5) 0.2778(5) 0.1737(4) 0.0285(16) Uani 1 1 d . . . C7 C 0.5879(5) 0.2471(5) 0.1301(4) 0.0277(16) Uani 1 1 d . . . C8 C 0.4215(5) 0.2522(6) 0.0767(4) 0.0300(16) Uani 1 1 d . . . C9 C 0.3361(5) 0.2274(6) 0.1272(4) 0.0314(17) Uani 1 1 d . . . C10 C 0.2353(5) 0.1993(6) 0.0716(4) 0.0328(17) Uani 1 1 d . . . C11 C 0.1365(6) 0.1985(6) 0.1928(5) 0.039(2) Uani 1 1 d . . . C12 C 0.1601(7) 0.0478(6) 0.0939(6) 0.044(2) Uani 1 1 d . . . C13 C 0.0486(6) 0.1377(6) 0.0516(5) 0.0396(19) Uani 1 1 d . . . C14 C 0.3361(5) 0.4751(5) 0.1787(4) 0.0260(15) Uani 1 1 d . . . C15 C 0.2361(5) 0.4543(5) 0.1386(5) 0.0329(17) Uani 1 1 d . . . C16 C 0.1512(5) 0.4677(5) 0.1815(4) 0.0344(17) Uani 1 1 d . . . C17 C 0.1618(5) 0.5042(5) 0.2670(4) 0.0337(17) Uani 1 1 d . . . C18 C 0.2592(5) 0.5304(5) 0.3087(4) 0.0292(16) Uani 1 1 d . . . C19 C 0.3467(4) 0.5169(5) 0.2662(4) 0.0249(15) Uani 1 1 d . . . C20 C 0.4466(5) 0.5556(5) 0.3141(4) 0.0223(14) Uani 1 1 d . . . C21 C 0.6249(5) 0.5932(5) 0.3484(4) 0.0284(16) Uani 1 1 d . . . C22 C 0.6963(5) 0.6639(5) 0.3193(4) 0.0262(15) Uani 1 1 d . . . C23 C 0.7738(5) 0.7184(5) 0.3918(4) 0.0275(16) Uani 1 1 d . . . C24 C 0.9233(6) 0.8381(6) 0.4603(5) 0.038(2) Uani 1 1 d . . . C25 C 0.8034(7) 0.8714(7) 0.3643(6) 0.044(2) Uani 1 1 d . . . C26 C 0.9141(6) 0.7629(5) 0.3081(4) 0.0342(17) Uani 1 1 d . . . C27 C 0.7048(5) 0.5056(6) 0.0639(4) 0.0332(18) Uani 1 1 d . . . C28 C 0.7859(6) 0.4553(7) 0.0576(5) 0.0380(19) Uani 1 1 d . . . C29 C 0.8867(5) 0.4989(8) 0.0654(5) 0.048(2) Uani 1 1 d . . . C30 C 0.9130(6) 0.5958(7) 0.0839(5) 0.048(2) Uani 1 1 d . . . C31 C 0.8357(6) 0.6462(7) 0.0927(4) 0.042(2) Uani 1 1 d . . . C32 C 0.7304(5) 0.6040(6) 0.0823(4) 0.0346(17) Uani 1 1 d . . . C33 C 0.6543(6) 0.6640(6) 0.0938(4) 0.0370(18) Uani 1 1 d . . . C34 C 0.4912(6) 0.7046(6) 0.0842(5) 0.0391(18) Uani 1 1 d . . . C35 C 0.4196(7) 0.7032(7) 0.1512(6) 0.050(2) Uani 1 1 d . . . C36 C 0.3468(6) 0.7708(6) 0.1452(5) 0.055(2) Uani 1 1 d . . . H48 H 0.3861 0.8241 0.1326 0.066 Uiso 1 1 calc R . . H49 H 0.2948 0.7386 0.0991 0.066 Uiso 1 1 calc R . . C37 C 0.3733(7) 0.8753(7) 0.2883(6) 0.070(3) Uani 1 1 d . . . H50 H 0.4089 0.9235 0.2681 0.106 Uiso 1 1 calc R . . H51 H 0.4219 0.8413 0.304 0.106 Uiso 1 1 calc R . . H52 H 0.3391 0.9039 0.3355 0.106 Uiso 1 1 calc R . . C38 C 0.2397(9) 0.7343(8) 0.2519(9) 0.077(4) Uani 1 1 d . . . C39 C 0.2247(6) 0.8703(6) 0.2037(5) 0.0398(19) Uani 1 1 d . . . C40 C 0.2769(5) 0.4556(5) 0.4823(4) 0.0246(15) Uani 1 1 d . . . C41 C 0.1815(5) 0.4782(5) 0.5113(4) 0.0284(16) Uani 1 1 d . . . C42 C 0.0908(5) 0.4157(6) 0.4877(5) 0.0344(18) Uani 1 1 d . . . C43 C 0.0881(5) 0.3257(6) 0.4321(5) 0.0333(18) Uani 1 1 d . . . C44 C 0.1765(5) 0.3022(6) 0.4030(5) 0.0312(18) Uani 1 1 d . . . C45 C 0.2719(4) 0.3643(5) 0.4264(4) 0.0234(15) Uani 1 1 d . . . C46 C 0.3626(5) 0.3344(6) 0.3919(4) 0.0259(17) Uani 1 1 d . . . C47 C 0.5331(5) 0.3273(5) 0.3631(4) 0.0263(15) Uani 1 1 d . . . C48 C 0.5710(5) 0.2664(5) 0.4110(5) 0.0260(15) Uani 1 1 d . . . C49 C 0.6514(5) 0.2150(6) 0.3664(5) 0.0261(15) Uani 1 1 d . . . C50 C 0.7780(7) 0.1107(7) 0.3636(7) 0.038(2) Uani 1 1 d . . . C51 C 0.6048(6) 0.0646(6) 0.3996(6) 0.042(2) Uani 1 1 d . . . C52 C 0.7213(6) 0.1932(6) 0.4980(4) 0.0369(18) Uani 1 1 d . . . N1 N 0.5198(4) 0.2992(4) 0.1279(3) 0.0250(12) Uani 1 1 d . . . N2 N 0.1465(4) 0.1476(4) 0.1038(3) 0.0304(13) Uani 1 1 d . . . N3 N 0.5344(4) 0.5432(4) 0.2886(3) 0.0296(13) Uani 1 1 d . . . N4 N 0.8543(4) 0.7962(4) 0.3808(3) 0.0299(13) Uani 1 1 d . . . N5 N 0.5561(4) 0.6326(4) 0.0705(3) 0.0322(14) Uani 1 1 d . . . N6 N 0.2938(4) 0.8076(4) 0.2202(4) 0.0381(15) Uani 1 1 d . . . N7 N 0.4569(4) 0.3776(4) 0.4090(3) 0.0253(12) Uani 1 1 d . . . N8 N 0.6892(4) 0.1465(4) 0.4060(3) 0.0288(13) Uani 1 1 d . . . O1 O 0.6811(3) 0.4430(3) 0.2244(3) 0.0289(10) Uani 1 1 d . . . O2 O 0.4151(3) 0.4561(3) 0.1366(3) 0.0306(11) Uani 1 1 d . . . O3 O 0.6086(3) 0.4601(4) 0.0530(3) 0.0386(12) Uani 1 1 d . . . O4 O 0.3611(3) 0.5184(3) 0.5078(3) 0.0275(10) Uani 1 1 d . . . OW1 O 0.6904(5) 0.8973(5) 0.1953(5) 0.093(2) Uani 1 1 d . . . OW2 O 0.3384(4) 0.1026(4) 0.2618(3) 0.0439(13) Uani 1 1 d . . . OW3 O 0.6330(7) 0.9979(7) 0.9970(7) 0.184(5) Uani 1 1 d . . . OW4 O 0.3181(4) 0.1204(4) 0.4245(3) 0.0483(13) Uani 1 1 d . . . OW5 O 0.0022(4) 0.0622(4) 0.3390(3) 0.0554(15) Uani 1 1 d . . . Cl1 Cl 0.01375(14) 0.24734(15) 0.05728(12) 0.0461(5) Uani 1 1 d . . . Cl2 Cl 0.97542(13) 0.66950(14) 0.31530(11) 0.0421(5) Uani 1 1 d . . . Cl3 Cl 0.1226(2) 0.8101(2) 0.1301(2) 0.1106(12) Uani 1 1 d . . . Cl4 Cl 0.81915(13) 0.29308(14) 0.51642(11) 0.0413(5) Uani 1 1 d . . . Cl5 Cl 0.90506(15) 0.97775(16) 0.15161(12) 0.0533(5) Uani 1 1 d . . . Cl6 Cl 0.15351(12) 0.94238(13) 0.40652(11) 0.0368(4) Uani 1 1 d . . . Cl7 Cl 0.51878(18) 0.01446(18) 0.16949(15) 0.0682(7) Uani 1 1 d . . . Cl8 Cl 0.47140(13) 0.18618(14) 0.58056(11) 0.0408(5) Uani 1 1 d . . . Cu1 Cu 0.54298(6) 0.43832(6) 0.18473(5) 0.0274(2) Uani 1 1 d . . . Cu2 Cu 0.5 0.5 0 0.0341(3) Uani 1 2 d S . . Cu3 Cu 0.5 0.5 0.5 0.0243(3) Uani 1 2 d S . . H1 H 0.859(6) 0.454(5) 0.289(5) 0.05(2) Uiso 1 1 d . . . H2 H 0.953(5) 0.340(4) 0.281(4) 0.031(18) Uiso 1 1 d . . . H3 H 0.882(4) 0.186(4) 0.209(3) 0.010(14) Uiso 1 1 d . . . H4 H 0.702(5) 0.124(5) 0.136(4) 0.06(2) Uiso 1 1 d . . . H5 H 0.572(4) 0.182(4) 0.096(3) 0.000(13) Uiso 1 1 d . . . H6 H 0.443(5) 0.198(6) 0.039(5) 0.05(2) Uiso 1 1 d . . . H7 H 0.403(4) 0.301(4) 0.051(4) 0.030(17) Uiso 1 1 d . . . H8 H 0.329(4) 0.287(5) 0.181(4) 0.032(17) Uiso 1 1 d . . . H9 H 0.346(6) 0.194(6) 0.151(5) 0.05(3) Uiso 1 1 d . . . H10 H 0.211(5) 0.259(5) 0.068(4) 0.039(19) Uiso 1 1 d . . . H11 H 0.240(5) 0.159(5) 0.012(5) 0.05(2) Uiso 1 1 d . . . H12 H 0.131(4) 0.272(5) 0.199(4) 0.027(17) Uiso 1 1 d . . . H13 H 0.179(4) 0.200(4) 0.220(3) 0.000(15) Uiso 1 1 d . . . H14 H 0.065(5) 0.159(5) 0.199(4) 0.040(19) Uiso 1 1 d . . . H15 H 0.209(6) 0.053(5) 0.126(5) 0.05(2) Uiso 1 1 d . . . H16 H 0.105(5) 0.016(5) 0.107(4) 0.04(2) Uiso 1 1 d . . . H17 H 0.185(4) -0.013(4) 0.019(3) 0.020(15) Uiso 1 1 d . . . H18 H 0.001(4) 0.114(4) 0.075(3) 0.007(15) Uiso 1 1 d . . . H19 H 0.064(4) 0.105(4) -0.010(4) 0.024(16) Uiso 1 1 d . . . H20 H 0.232(5) 0.431(5) 0.083(4) 0.04(2) Uiso 1 1 d . . . H21 H 0.084(5) 0.452(5) 0.151(4) 0.035(18) Uiso 1 1 d . . . H22 H 0.104(5) 0.515(5) 0.297(4) 0.040(19) Uiso 1 1 d . . . H23 H 0.273(5) 0.568(5) 0.370(4) 0.039(19) Uiso 1 1 d . . . H24 H 0.443(4) 0.597(4) 0.373(4) 0.017(15) Uiso 1 1 d . . . H25 H 0.656(4) 0.537(4) 0.355(3) 0.015(14) Uiso 1 1 d . . . H26 H 0.602(4) 0.624(4) 0.395(3) 0.008(14) Uiso 1 1 d . . . H27 H 0.729(4) 0.638(4) 0.270(4) 0.016(15) Uiso 1 1 d . . . H28 H 0.662(5) 0.707(5) 0.300(4) 0.031(17) Uiso 1 1 d . . . H29 H 0.740(4) 0.750(4) 0.434(4) 0.020(16) Uiso 1 1 d . . . H30 H 0.816(4) 0.682(4) 0.409(3) 0.023(16) Uiso 1 1 d . . . H31 H 0.960(4) 0.875(4) 0.455(3) 0.000(16) Uiso 1 1 d . . . H32 H 0.881(6) 0.846(6) 0.507(5) 0.07(3) Uiso 1 1 d . . . H33 H 0.963(5) 0.780(5) 0.466(4) 0.037(18) Uiso 1 1 d . . . H34 H 0.771(5) 0.895(5) 0.412(4) 0.04(2) Uiso 1 1 d . . . H35 H 0.863(5) 0.925(5) 0.368(4) 0.030(17) Uiso 1 1 d . . . H36 H 0.764(4) 0.853(4) 0.317(4) 0.018(18) Uiso 1 1 d . . . H37 H 0.962(5) 0.816(5) 0.303(4) 0.04(2) Uiso 1 1 d . . . H38 H 0.860(6) 0.730(5) 0.241(5) 0.06(2) Uiso 1 1 d . . . H39 H 0.771(4) 0.398(4) 0.042(4) 0.009(18) Uiso 1 1 d . . . H40 H 0.931(5) 0.466(5) 0.066(4) 0.04(2) Uiso 1 1 d . . . H41 H 0.995(7) 0.635(6) 0.092(5) 0.08(3) Uiso 1 1 d . . . H42 H 0.847(4) 0.716(4) 0.105(3) 0.010(15) Uiso 1 1 d . . . H43 H 0.677(5) 0.732(5) 0.118(4) 0.04(2) Uiso 1 1 d . . . H44 H 0.540(4) 0.766(4) 0.103(3) 0.000(13) Uiso 1 1 d . . . H45 H 0.445(5) 0.694(5) 0.027(5) 0.05(2) Uiso 1 1 d . . . H46 H 0.455(5) 0.723(5) 0.209(5) 0.05(2) Uiso 1 1 d . . . H47 H 0.384(4) 0.638(4) 0.134(3) 0.004(14) Uiso 1 1 d . . . H53 H 0.194(5) 0.772(5) 0.298(4) 0.05(2) Uiso 1 1 d . . . H54 H 0.183(8) 0.688(8) 0.204(7) 0.11(4) Uiso 1 1 d . . . H55 H 0.278(4) 0.709(5) 0.272(4) 0.016(17) Uiso 1 1 d . . . H56 H 0.196(5) 0.892(4) 0.252(4) 0.024(17) Uiso 1 1 d . . . H57 H 0.268(6) 0.908(6) 0.180(5) 0.07(3) Uiso 1 1 d . . . H58 H 0.192(4) 0.542(4) 0.550(3) 0.002(13) Uiso 1 1 d . . . H59 H 0.036(6) 0.441(6) 0.518(5) 0.07(3) Uiso 1 1 d . . . H60 H 0.040(4) 0.286(4) 0.412(4) 0.010(16) Uiso 1 1 d . . . H61 H 0.179(4) 0.254(4) 0.377(3) 0.000(16) Uiso 1 1 d . . . H62 H 0.355(4) 0.295(4) 0.358(3) 0.000(17) Uiso 1 1 d . . . H63 H 0.503(5) 0.287(5) 0.311(4) 0.04(2) Uiso 1 1 d . . . H64 H 0.589(4) 0.371(4) 0.355(3) 0.015(15) Uiso 1 1 d . . . H65 H 0.515(5) 0.232(5) 0.416(4) 0.04(2) Uiso 1 1 d . . . H66 H 0.590(5) 0.303(5) 0.466(4) 0.04(2) Uiso 1 1 d . . . H67 H 0.628(4) 0.179(4) 0.320(4) 0.010(17) Uiso 1 1 d . . . H68 H 0.709(4) 0.254(4) 0.363(3) 0.000(13) Uiso 1 1 d . . . H69 H 0.759(7) 0.071(7) 0.312(6) 0.08(4) Uiso 1 1 d . . . H70 H 0.829(4) 0.158(4) 0.368(3) 0.000(14) Uiso 1 1 d . . . H71 H 0.801(5) 0.084(5) 0.387(4) 0.02(2) Uiso 1 1 d . . . H72 H 0.581(5) 0.031(5) 0.348(4) 0.024(19) Uiso 1 1 d . . . H73 H 0.550(6) 0.077(5) 0.430(4) 0.04(2) Uiso 1 1 d . . . H74 H 0.628(6) 0.021(7) 0.431(5) 0.08(3) Uiso 1 1 d . . . H75 H 0.665(6) 0.216(5) 0.530(5) 0.05(2) Uiso 1 1 d . . . H76 H 0.741(4) 0.145(4) 0.514(3) 0.014(15) 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 C1 0.025(3) 0.030(4) 0.026(4) 0.014(3) 0.004(3) 0.004(3) C2 0.025(4) 0.044(5) 0.035(4) 0.015(4) 0.001(3) 0.006(4) C3 0.020(4) 0.049(5) 0.044(4) 0.026(4) 0.010(3) 0.012(4) C4 0.034(4) 0.034(5) 0.048(5) 0.016(4) 0.020(4) 0.017(4) C5 0.024(4) 0.044(5) 0.048(4) 0.021(4) 0.017(3) 0.013(3) C6 0.027(4) 0.034(4) 0.031(4) 0.016(3) 0.008(3) 0.011(3) C7 0.028(4) 0.033(5) 0.024(4) 0.010(4) 0.005(3) 0.008(3) C8 0.026(4) 0.033(5) 0.028(4) 0.008(4) 0.001(3) 0.001(3) C9 0.028(4) 0.039(5) 0.030(4) 0.017(4) -0.004(3) 0.003(3) C10 0.024(4) 0.044(5) 0.030(4) 0.016(4) -0.002(3) -0.003(3) C11 0.025(4) 0.056(6) 0.032(4) 0.016(4) -0.011(4) -0.008(4) C12 0.030(4) 0.041(5) 0.063(6) 0.024(5) -0.002(4) -0.003(4) C13 0.027(4) 0.057(6) 0.038(5) 0.020(4) 0.008(4) 0.004(4) C14 0.023(3) 0.027(4) 0.026(4) 0.006(3) 0.003(3) 0.001(3) C15 0.033(4) 0.036(5) 0.030(4) 0.007(4) -0.001(3) 0.013(3) C16 0.023(4) 0.033(4) 0.044(5) 0.009(4) -0.007(3) 0.006(3) C17 0.029(4) 0.043(5) 0.033(4) 0.013(4) 0.009(3) 0.014(4) C18 0.034(4) 0.031(4) 0.021(4) 0.008(3) 0.001(3) 0.004(3) C19 0.021(3) 0.028(4) 0.030(4) 0.015(3) 0.005(3) 0.007(3) C20 0.024(4) 0.023(4) 0.020(3) 0.008(3) -0.003(3) 0.006(3) C21 0.028(4) 0.035(5) 0.021(4) 0.007(4) 0.002(3) 0.004(3) C22 0.029(4) 0.025(4) 0.029(4) 0.011(3) 0.004(3) 0.010(3) C23 0.023(3) 0.032(4) 0.031(4) 0.012(4) 0.007(3) 0.012(3) C24 0.036(5) 0.034(5) 0.032(4) 0.001(4) 0.009(4) -0.015(4) C25 0.040(5) 0.047(6) 0.053(6) 0.020(5) 0.020(5) 0.011(4) C26 0.038(4) 0.034(5) 0.035(4) 0.012(4) 0.015(3) 0.012(4) C27 0.019(3) 0.064(6) 0.026(4) 0.025(4) 0.002(3) 0.012(4) C28 0.036(5) 0.052(6) 0.030(4) 0.017(4) 0.004(3) 0.011(4) C29 0.020(4) 0.099(8) 0.038(5) 0.035(5) 0.006(3) 0.017(5) C30 0.039(5) 0.072(7) 0.036(5) 0.024(5) -0.001(4) 0.003(5) C31 0.042(5) 0.057(6) 0.020(4) 0.009(4) -0.002(3) -0.008(4) C32 0.031(4) 0.053(5) 0.017(4) 0.010(4) 0.001(3) 0.004(4) C33 0.042(5) 0.052(6) 0.020(4) 0.016(4) 0.007(3) 0.007(4) C34 0.045(5) 0.043(5) 0.036(4) 0.019(4) 0.007(4) 0.014(4) C35 0.060(6) 0.055(7) 0.054(6) 0.030(5) 0.028(5) 0.029(5) C36 0.067(5) 0.077(7) 0.037(4) 0.024(5) 0.014(4) 0.044(5) C37 0.061(6) 0.094(8) 0.062(6) 0.024(6) 0.002(5) 0.031(6) C38 0.069(7) 0.071(8) 0.135(11) 0.070(9) 0.063(8) 0.048(7) C39 0.039(4) 0.045(5) 0.038(5) 0.013(4) 0.004(4) 0.016(4) C40 0.023(3) 0.032(4) 0.023(3) 0.013(3) -0.001(3) 0.009(3) C41 0.032(4) 0.023(4) 0.032(4) 0.011(4) 0.003(3) 0.004(3) C42 0.022(4) 0.043(5) 0.043(4) 0.022(4) 0.002(3) 0.005(4) C43 0.020(4) 0.041(5) 0.036(4) 0.013(4) -0.012(3) -0.001(4) C44 0.035(4) 0.029(5) 0.029(4) 0.006(4) -0.003(3) 0.011(4) C45 0.022(3) 0.026(4) 0.023(3) 0.010(3) 0.000(3) 0.003(3) C46 0.035(5) 0.027(5) 0.012(4) 0.001(4) -0.003(3) 0.006(4) C47 0.028(4) 0.030(4) 0.024(4) 0.010(4) 0.003(3) 0.012(3) C48 0.022(4) 0.026(4) 0.032(4) 0.012(4) 0.011(3) 0.003(3) C49 0.023(4) 0.026(4) 0.032(4) 0.011(4) 0.002(3) 0.005(3) C50 0.033(5) 0.031(5) 0.057(6) 0.015(5) 0.014(4) 0.013(4) C51 0.035(5) 0.037(5) 0.053(6) 0.013(5) 0.003(4) 0.002(4) C52 0.034(4) 0.052(5) 0.034(4) 0.022(4) 0.012(3) 0.015(4) N1 0.027(3) 0.033(3) 0.019(3) 0.014(3) 0.007(2) 0.006(3) N2 0.029(3) 0.036(4) 0.025(3) 0.013(3) -0.001(2) -0.002(3) N3 0.024(3) 0.039(4) 0.028(3) 0.015(3) 0.000(2) 0.005(3) N4 0.028(3) 0.024(3) 0.037(3) 0.009(3) 0.004(3) 0.001(3) N5 0.034(3) 0.044(4) 0.024(3) 0.016(3) 0.007(3) 0.012(3) N6 0.033(3) 0.049(4) 0.041(4) 0.023(3) 0.012(3) 0.014(3) N7 0.025(3) 0.027(3) 0.024(3) 0.006(3) 0.006(2) 0.007(3) N8 0.022(3) 0.035(4) 0.035(3) 0.016(3) 0.005(2) 0.009(3) O1 0.023(2) 0.032(3) 0.032(3) 0.009(2) -0.0010(19) 0.005(2) O2 0.026(2) 0.040(3) 0.026(2) 0.007(2) 0.001(2) 0.010(2) O3 0.026(3) 0.050(3) 0.046(3) 0.022(3) 0.002(2) 0.011(2) O4 0.024(2) 0.031(3) 0.030(2) 0.012(2) 0.005(2) 0.006(2) OW1 0.084(5) 0.080(5) 0.100(5) 0.019(4) -0.020(4) -0.003(4) OW2 0.048(3) 0.046(3) 0.042(3) 0.022(3) -0.004(2) 0.007(3) OW3 0.129(7) 0.124(8) 0.208(11) -0.074(8) 0.106(8) -0.021(6) OW4 0.057(3) 0.044(3) 0.043(3) 0.018(3) 0.003(3) 0.001(3) OW5 0.053(3) 0.064(4) 0.043(3) 0.002(3) -0.005(3) 0.026(3) Cl1 0.0390(10) 0.0570(14) 0.0459(11) 0.0224(10) -0.0014(9) 0.0083(9) Cl2 0.0370(10) 0.0442(12) 0.0458(11) 0.0104(10) 0.0083(8) 0.0155(9) Cl3 0.0857(19) 0.071(2) 0.138(3) -0.0219(18) -0.0655(19) 0.0316(16) Cl4 0.0357(10) 0.0459(12) 0.0376(10) 0.0075(9) -0.0013(8) 0.0055(9) Cl5 0.0487(11) 0.0699(16) 0.0396(11) 0.0111(11) 0.0102(9) 0.0152(11) Cl6 0.0328(9) 0.0381(11) 0.0432(10) 0.0160(9) 0.0104(8) 0.0085(8) Cl7 0.0619(14) 0.0687(17) 0.0741(16) 0.0211(14) 0.0188(12) 0.0111(12) Cl8 0.0381(10) 0.0501(13) 0.0386(10) 0.0162(9) 0.0093(8) 0.0141(9) Cu1 0.0228(4) 0.0317(5) 0.0277(5) 0.0090(4) 0.0000(3) 0.0062(4) Cu2 0.0227(6) 0.0450(8) 0.0408(7) 0.0212(7) 0.0036(5) 0.0088(6) Cu3 0.0219(6) 0.0269(7) 0.0251(6) 0.0091(5) 0.0027(5) 0.0052(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.303(7) . ? C1 C6 1.417(9) . ? C1 C2 1.430(9) . ? C2 C3 1.378(10) . ? C3 C4 1.378(10) . ? C4 C5 1.389(10) . ? C5 C6 1.414(9) . ? C6 C7 1.440(9) . ? C7 N1 1.294(8) . ? C8 N1 1.477(8) . ? C8 C9 1.514(9) . ? C9 C10 1.519(9) . ? C10 N2 1.518(8) . ? C11 N2 1.501(9) . ? C12 N2 1.508(10) . ? C13 N2 1.496(8) . ? C13 Cl1 1.767(8) . ? C14 O2 1.313(7) . ? C14 C15 1.401(9) . ? C14 C19 1.423(9) . ? C15 C16 1.375(9) . ? C16 C17 1.383(10) . ? C17 C18 1.380(9) . ? C18 C19 1.400(9) . ? C19 C20 1.455(8) . ? C20 N3 1.278(8) . ? C21 N3 1.475(8) . ? C21 C22 1.520(9) . ? C22 C23 1.502(9) . ? C23 N4 1.514(8) . ? C24 N4 1.501(9) . ? C25 N4 1.498(9) . ? C26 N4 1.500(8) . ? C26 Cl2 1.768(7) . ? C27 O3 1.321(8) . ? C27 C28 1.400(10) . ? C27 C32 1.406(10) . ? C28 C29 1.368(11) . ? C29 C30 1.385(12) . ? C30 C31 1.358(11) . ? C31 C32 1.412(10) . ? C32 C33 1.440(10) . ? C33 N5 1.307(9) . ? C34 N5 1.463(9) . ? C34 C35 1.515(10) . ? C35 C36 1.533(10) . ? C36 N6 1.486(9) . ? C37 N6 1.525(11) . ? C38 N6 1.470(11) . ? C39 N6 1.492(9) . ? C39 Cl3 1.727(8) . ? C40 O4 1.302(7) . ? C40 C45 1.413(9) . ? C40 C41 1.428(8) . ? C41 C42 1.361(9) . ? C42 C43 1.400(11) . ? C43 C44 1.346(10) . ? C44 C45 1.407(10) . ? C45 C46 1.436(9) . ? C46 N7 1.285(9) . ? C47 N7 1.471(8) . ? C47 C48 1.524(9) . ? C48 C49 1.514(9) . ? C49 N8 1.525(8) . ? C50 N8 1.494(9) . ? C51 N8 1.500(9) . ? C52 N8 1.519(9) . ? C52 Cl4 1.761(8) . ? N1 Cu1 2.000(6) . ? N3 Cu1 2.012(6) . ? N5 Cu2 2.002(6) . ? N7 Cu3 2.003(5) . ? O1 Cu1 1.899(4) . ? O2 Cu1 1.935(4) . ? O3 Cu2 1.928(4) . ? O4 Cu3 1.904(4) . ? Cu2 O3 1.928(4) 2_665 ? Cu2 N5 2.002(6) 2_665 ? Cu3 O4 1.904(4) 2_666 ? Cu3 N7 2.003(5) 2_666 ? 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 C1 C6 124.7(5) . . ? O1 C1 C2 117.8(6) . . ? C6 C1 C2 117.5(6) . . ? C3 C2 C1 120.5(8) . . ? C2 C3 C4 122.0(7) . . ? C3 C4 C5 119.1(7) . . ? C4 C5 C6 120.8(7) . . ? C5 C6 C1 120.0(6) . . ? C5 C6 C7 117.1(7) . . ? C1 C6 C7 122.9(6) . . ? N1 C7 C6 126.6(7) . . ? N1 C8 C9 112.8(5) . . ? C8 C9 C10 107.6(5) . . ? N2 C10 C9 114.5(5) . . ? N2 C13 Cl1 112.8(5) . . ? O2 C14 C15 120.9(6) . . ? O2 C14 C19 122.4(5) . . ? C15 C14 C19 116.7(6) . . ? C16 C15 C14 122.2(7) . . ? C15 C16 C17 120.7(6) . . ? C18 C17 C16 119.1(6) . . ? C17 C18 C19 121.0(6) . . ? C18 C19 C14 120.2(6) . . ? C18 C19 C20 117.1(6) . . ? C14 C19 C20 122.4(5) . . ? N3 C20 C19 126.4(6) . . ? N3 C21 C22 113.1(5) . . ? C23 C22 C21 106.1(5) . . ? C22 C23 N4 117.6(5) . . ? N4 C26 Cl2 111.7(4) . . ? O3 C27 C28 119.7(7) . . ? O3 C27 C32 122.7(6) . . ? C28 C27 C32 117.6(7) . . ? C29 C28 C27 121.9(9) . . ? C28 C29 C30 121.1(9) . . ? C31 C30 C29 118.0(8) . . ? C30 C31 C32 123.0(9) . . ? C27 C32 C31 118.4(7) . . ? C27 C32 C33 122.9(7) . . ? C31 C32 C33 118.6(8) . . ? N5 C33 C32 123.5(8) . . ? N5 C34 C35 114.0(6) . . ? C34 C35 C36 105.5(6) . . ? N6 C36 C35 115.9(6) . . ? N6 C39 Cl3 112.9(6) . . ? O4 C40 C45 124.5(5) . . ? O4 C40 C41 119.5(6) . . ? C45 C40 C41 116.0(6) . . ? C42 C41 C40 122.5(7) . . ? C41 C42 C43 120.2(7) . . ? C44 C43 C42 118.9(7) . . ? C43 C44 C45 122.7(8) . . ? C44 C45 C40 119.6(6) . . ? C44 C45 C46 119.4(7) . . ? C40 C45 C46 120.9(6) . . ? N7 C46 C45 129.0(7) . . ? N7 C47 C48 109.0(5) . . ? C49 C48 C47 110.5(5) . . ? C48 C49 N8 114.9(5) . . ? N8 C52 Cl4 111.6(5) . . ? C7 N1 C8 116.8(6) . . ? C7 N1 Cu1 124.0(5) . . ? C8 N1 Cu1 119.1(4) . . ? C13 N2 C11 110.2(6) . . ? C13 N2 C12 104.8(6) . . ? C11 N2 C12 110.4(6) . . ? C13 N2 C10 109.5(5) . . ? C11 N2 C10 111.1(6) . . ? C12 N2 C10 110.7(6) . . ? C20 N3 C21 116.0(6) . . ? C20 N3 Cu1 119.9(5) . . ? C21 N3 Cu1 122.5(4) . . ? C25 N4 C26 105.7(5) . . ? C25 N4 C24 108.7(7) . . ? C26 N4 C24 111.8(5) . . ? C25 N4 C23 110.0(5) . . ? C26 N4 C23 113.0(5) . . ? C24 N4 C23 107.5(5) . . ? C33 N5 C34 115.6(7) . . ? C33 N5 Cu2 122.9(5) . . ? C34 N5 Cu2 120.4(5) . . ? C38 N6 C36 114.3(7) . . ? C38 N6 C39 112.4(7) . . ? C36 N6 C39 109.1(5) . . ? C38 N6 C37 108.9(8) . . ? C36 N6 C37 108.6(6) . . ? C39 N6 C37 102.8(6) . . ? C46 N7 C47 115.9(6) . . ? C46 N7 Cu3 122.4(5) . . ? C47 N7 Cu3 121.5(4) . . ? C50 N8 C51 109.2(6) . . ? C50 N8 C52 109.9(6) . . ? C51 N8 C52 105.9(6) . . ? C50 N8 C49 109.6(6) . . ? C51 N8 C49 110.9(5) . . ? C52 N8 C49 111.3(6) . . ? C1 O1 Cu1 128.5(4) . . ? C14 O2 Cu1 123.6(4) . . ? C27 O3 Cu2 121.3(4) . . ? C40 O4 Cu3 128.2(4) . . ? O1 Cu1 O2 167.71(19) . . ? O1 Cu1 N1 93.08(19) . . ? O2 Cu1 N1 95.0(2) . . ? O1 Cu1 N3 87.99(19) . . ? O2 Cu1 N3 90.24(19) . . ? N1 Cu1 N3 147.1(2) . . ? O3 Cu2 O3 180.0(3) 2_665 . ? O3 Cu2 N5 88.3(2) 2_665 2_665 ? O3 Cu2 N5 91.7(2) . 2_665 ? O3 Cu2 N5 91.7(2) 2_665 . ? O3 Cu2 N5 88.3(2) . . ? N5 Cu2 N5 180.0(4) 2_665 . ? O4 Cu3 O4 180.0(3) . 2_666 ? O4 Cu3 N7 88.22(19) . 2_666 ? O4 Cu3 N7 91.78(19) 2_666 2_666 ? O4 Cu3 N7 91.78(19) . . ? O4 Cu3 N7 88.22(19) 2_666 . ? N7 Cu3 N7 180.0(2) 2_666 . ? # END OF CIF