# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global #TrackingRef 'complex-1.CIF' _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Wu, Xintao' _publ_contact_author_email wxt@fjirsm.ac.cn _publ_section_title ; Syntheses, structural aspects, luminescence and magnetism of four coordination polymers based on a novel flexible polycarboxylate ; loop_ _publ_author_name 'Qilong Zhu' 'Xintao Wu' 'Tianlu Sheng' 'Ruibiao Fu' 'Shengmin Hu' ; Chaojun Shen ; 'Xiao Ma' # Attachment 'complex-4.CIF' data_complex-4 #TrackingRef 'complex-4.CIF' _database_code_depnum_ccdc_archive 'CCDC 769618' #TrackingRef '- complex 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H42 Ca5 N12 O32' _chemical_formula_weight 1283.16 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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 11.300(6) _cell_length_b 19.440(11) _cell_length_c 21.466(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4716(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3565 _cell_measurement_theta_min 2.0849 _cell_measurement_theta_max 27.4565 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.807 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2648 _exptl_absorpt_coefficient_mu 0.687 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6983 _exptl_absorpt_correction_T_max 1.0000 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35236 _diffrn_reflns_av_R_equivalents 0.0782 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.46 _reflns_number_total 5400 _reflns_number_gt 4396 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1152P)^2^+5.7981P] 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_extinction_coef ? _refine_ls_number_reflns 5400 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0982 _refine_ls_R_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.2263 _refine_ls_wR_factor_gt 0.2105 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 Ca1 Ca 0.02969(8) 0.01778(5) 0.17399(4) 0.0322(2) Uani 1 1 d . . . Ca2 Ca 0.28220(8) 0.14982(4) 0.17412(5) 0.0343(3) Uani 1 1 d . . . Ca3 Ca 0.0000 0.0000 0.0000 0.0315(3) Uani 1 2 d S . . C1 C -0.1085(4) 0.2949(2) -0.0043(2) 0.0304(9) Uani 1 1 d . . . C2 C -0.1186(4) 0.3170(2) 0.0986(2) 0.0278(8) Uani 1 1 d . . . C3 C -0.1509(3) 0.4013(2) 0.0293(2) 0.0272(8) Uani 1 1 d . . . C4 C -0.0663(4) 0.1783(2) -0.0389(2) 0.0388(11) Uani 1 1 d . . . H4A H -0.0852 0.1507 -0.0752 0.047 Uiso 1 1 calc R . . H4B H -0.1161 0.1625 -0.0050 0.047 Uiso 1 1 calc R . . C5 C 0.0613(4) 0.1654(2) -0.0216(2) 0.0370(10) Uani 1 1 d . . . C6 C -0.0957(5) 0.2745(3) -0.1148(2) 0.0449(12) Uani 1 1 d . . . H6A H -0.1643 0.3039 -0.1202 0.054 Uiso 1 1 calc R . . H6B H -0.1049 0.2356 -0.1428 0.054 Uiso 1 1 calc R . . C7 C 0.0123(6) 0.3142(3) -0.1347(3) 0.0554(15) Uani 1 1 d . . . C8 C -0.0853(4) 0.2213(2) 0.1687(2) 0.0298(9) Uani 1 1 d . . . H8A H -0.1318 0.1946 0.1394 0.036 Uiso 1 1 calc R . . H8B H -0.1126 0.2096 0.2102 0.036 Uiso 1 1 calc R . . C9 C 0.0419(4) 0.1990(2) 0.1630(2) 0.0300(9) Uani 1 1 d . . . C10 C -0.1429(4) 0.3381(2) 0.2102(2) 0.0315(9) Uani 1 1 d . . . H10A H -0.1737 0.3087 0.2430 0.038 Uiso 1 1 calc R . . H10B H -0.2073 0.3675 0.1967 0.038 Uiso 1 1 calc R . . C11 C -0.0489(4) 0.3834(2) 0.2387(2) 0.0373(10) Uani 1 1 d . . . C12 C -0.1552(4) 0.4974(2) -0.0448(2) 0.0332(9) Uani 1 1 d . . . H12A H -0.0956 0.4692 -0.0650 0.040 Uiso 1 1 calc R . . H12B H -0.1218 0.5431 -0.0400 0.040 Uiso 1 1 calc R . . C13 C -0.2608(4) 0.5029(2) -0.0887(2) 0.0281(9) Uani 1 1 d . . . C14 C -0.1925(4) 0.5158(2) 0.0699(2) 0.0329(9) Uani 1 1 d . . . H14A H -0.1880 0.5628 0.0549 0.039 Uiso 1 1 calc R . . H14B H -0.1277 0.5091 0.0989 0.039 Uiso 1 1 calc R . . C15 C -0.3082(4) 0.5071(2) 0.1051(2) 0.0357(10) Uani 1 1 d . . . N1 N -0.0969(3) 0.27070(18) 0.05380(18) 0.0313(8) Uani 1 1 d . . . N2 N -0.1327(3) 0.36060(18) -0.02012(18) 0.0324(8) Uani 1 1 d . . . N3 N -0.1488(3) 0.38303(18) 0.08986(17) 0.0298(8) Uani 1 1 d . . . N4 N -0.0961(3) 0.24919(19) -0.05228(18) 0.0331(8) Uani 1 1 d . . . N5 N -0.1753(3) 0.46946(18) 0.01697(17) 0.0312(8) Uani 1 1 d . . . N6 N -0.1103(3) 0.29427(18) 0.15793(17) 0.0291(8) Uani 1 1 d . . . O1 O 0.1356(3) 0.21433(18) -0.0253(2) 0.0533(10) Uani 1 1 d . . . O1W O 0.2970(7) 0.1817(3) 0.2926(4) 0.138(3) Uani 1 1 d . . . H1W1 H 0.3356 0.1474 0.3065 0.166 Uiso 1 1 d R . . H1W2 H 0.2755 0.2128 0.3181 0.166 Uiso 1 1 d R . . O2 O 0.0901(3) 0.10734(18) -0.00340(18) 0.0462(9) Uani 1 1 d . . . O2W O 0.1612(4) 0.0662(4) 0.2560(2) 0.106(2) Uani 1 1 d . . . H2W1 H 0.1030 0.0938 0.2546 0.127 Uiso 1 1 d R . . H2W2 H 0.2097 0.0813 0.2830 0.127 Uiso 1 1 d R . . O3 O 0.0044(5) 0.3510(3) -0.1808(3) 0.0918(19) Uani 1 1 d . . . O3W O -0.1091(4) 0.0466(3) 0.2550(2) 0.0728(13) Uani 1 1 d . . . H3W1 H -0.0698 0.0704 0.2811 0.087 Uiso 1 1 d R . . H3W2 H -0.1705 0.0694 0.2453 0.087 Uiso 1 1 d R . . O4 O 0.1098(4) 0.3093(2) -0.1033(2) 0.0628(12) Uani 1 1 d . . . H4C H 0.1109 0.2756 -0.0781 0.09(3) Uiso 1 1 d R . . O4W O 0.3127(4) 0.16639(19) 0.06373(18) 0.0503(9) Uani 1 1 d . . . H4W1 H 0.3558 0.1910 0.0401 0.060 Uiso 1 1 d R . . H4W2 H 0.2617 0.1463 0.0410 0.060 Uiso 1 1 d R . . O5 O 0.0616(3) 0.13594(16) 0.15768(18) 0.0421(8) Uani 1 1 d . . . O6 O 0.1250(3) 0.24174(17) 0.1670(2) 0.0516(10) Uani 1 1 d . . . O7 O -0.0776(4) 0.4096(2) 0.2897(2) 0.0702(14) Uani 1 1 d . . . O8 O 0.0446(3) 0.3941(2) 0.2109(2) 0.0552(10) Uani 1 1 d . . . O9 O -0.3605(3) 0.47702(16) -0.07480(15) 0.0336(7) Uani 1 1 d . . . O10 O -0.2446(3) 0.53334(15) -0.13920(16) 0.0379(7) Uani 1 1 d . . . O11 O -0.3883(3) 0.46859(16) 0.08455(15) 0.0353(7) Uani 1 1 d . . . O12 O -0.3219(4) 0.5407(2) 0.1542(2) 0.0645(12) 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 Ca1 0.0319(5) 0.0288(5) 0.0359(5) 0.0012(3) -0.0038(4) 0.0016(3) Ca2 0.0248(4) 0.0241(5) 0.0540(6) -0.0044(4) -0.0019(4) -0.0010(3) Ca3 0.0265(6) 0.0369(7) 0.0311(7) 0.0040(5) -0.0027(5) -0.0031(5) C1 0.0225(19) 0.029(2) 0.040(2) -0.0001(17) 0.0029(17) -0.0005(15) C2 0.0238(19) 0.0230(19) 0.036(2) 0.0023(15) -0.0010(17) 0.0006(15) C3 0.0217(19) 0.027(2) 0.033(2) 0.0029(15) 0.0017(16) 0.0042(15) C4 0.033(2) 0.029(2) 0.055(3) -0.0074(19) 0.004(2) -0.0030(18) C5 0.034(2) 0.033(2) 0.044(3) -0.0055(19) 0.004(2) -0.0052(18) C6 0.052(3) 0.045(3) 0.038(3) -0.007(2) -0.001(2) -0.002(2) C7 0.054(3) 0.048(3) 0.064(4) 0.011(3) 0.012(3) 0.006(2) C8 0.025(2) 0.029(2) 0.035(2) 0.0063(16) -0.0011(16) -0.0004(16) C9 0.027(2) 0.025(2) 0.038(2) 0.0020(16) 0.0012(17) -0.0003(16) C10 0.025(2) 0.035(2) 0.034(2) 0.0007(17) 0.0026(17) -0.0001(16) C11 0.033(2) 0.030(2) 0.049(3) -0.0078(19) 0.006(2) -0.0037(18) C12 0.025(2) 0.034(2) 0.041(3) 0.0080(18) -0.0004(18) 0.0000(17) C13 0.028(2) 0.0197(19) 0.037(2) -0.0004(15) 0.0052(17) 0.0025(15) C14 0.028(2) 0.025(2) 0.046(3) 0.0001(17) 0.0019(19) -0.0018(16) C15 0.030(2) 0.038(2) 0.039(3) -0.0002(19) -0.0014(19) -0.0004(18) N1 0.0292(18) 0.0279(18) 0.037(2) 0.0019(14) 0.0038(15) 0.0036(14) N2 0.0312(19) 0.0294(19) 0.037(2) 0.0033(14) -0.0012(16) -0.0006(14) N3 0.0290(18) 0.0266(18) 0.034(2) 0.0021(14) -0.0016(15) 0.0058(14) N4 0.0335(19) 0.0300(19) 0.036(2) -0.0056(15) 0.0036(16) -0.0007(15) N5 0.0295(18) 0.0279(18) 0.036(2) 0.0049(14) -0.0026(15) 0.0039(14) N6 0.0258(17) 0.0284(18) 0.0332(19) 0.0041(14) 0.0008(14) 0.0038(13) O1 0.0330(19) 0.036(2) 0.091(3) 0.0075(18) -0.0042(19) -0.0117(15) O1W 0.154(7) 0.094(5) 0.168(7) 0.025(5) 0.081(6) 0.043(5) O2 0.041(2) 0.037(2) 0.060(2) 0.0078(15) -0.0027(17) -0.0037(14) O2W 0.061(3) 0.204(7) 0.053(3) -0.043(3) -0.022(2) 0.043(4) O3 0.075(3) 0.109(5) 0.092(4) 0.057(3) 0.017(3) 0.007(3) O3W 0.056(3) 0.104(4) 0.059(3) -0.010(2) 0.015(2) -0.017(2) O4 0.043(2) 0.058(3) 0.087(3) 0.028(2) 0.012(2) -0.0029(18) O4W 0.052(2) 0.045(2) 0.054(2) 0.0069(16) -0.0078(18) 0.0019(17) O5 0.0313(17) 0.0239(16) 0.071(2) -0.0019(14) 0.0022(16) -0.0010(13) O6 0.0250(16) 0.0252(17) 0.104(3) -0.0003(17) 0.0036(17) -0.0038(13) O7 0.059(3) 0.072(3) 0.080(3) -0.042(2) 0.023(2) -0.027(2) O8 0.0300(18) 0.060(2) 0.076(3) -0.020(2) 0.0140(18) -0.0123(16) O9 0.0241(15) 0.0403(17) 0.0364(17) -0.0031(13) 0.0041(12) -0.0012(12) O10 0.0433(19) 0.0299(16) 0.0406(18) 0.0101(13) -0.0038(15) -0.0041(13) O11 0.0284(16) 0.0370(17) 0.0406(18) 0.0000(13) 0.0002(13) -0.0048(13) O12 0.052(2) 0.082(3) 0.059(3) -0.031(2) 0.018(2) -0.020(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca1 O7 2.307(4) 3_545 ? Ca1 O5 2.352(3) . ? Ca1 O3W 2.408(5) . ? Ca1 O2W 2.489(5) . ? Ca1 O11 2.512(3) 2_455 ? Ca1 O9 2.589(4) 6_655 ? Ca1 O12 2.644(4) 2_455 ? Ca1 O10 2.675(4) 6_655 ? Ca1 C15 2.947(5) 2_455 ? Ca1 C13 3.007(5) 6_655 ? Ca1 C11 3.222(5) 3_545 ? Ca1 Ca3 3.766(2) . ? Ca2 O8 2.276(4) 2 ? Ca2 O6 2.360(3) 2 ? Ca2 O10 2.404(3) 6_655 ? Ca2 O4W 2.416(4) . ? Ca2 O6 2.525(4) . ? Ca2 O5 2.532(4) . ? Ca2 O1W 2.623(9) . ? Ca2 O2W 2.757(7) . ? Ca2 C9 2.889(5) . ? Ca2 Ca2 3.963(3) 2 ? Ca3 O11 2.293(3) 6_655 ? Ca3 O11 2.293(3) 2_455 ? Ca3 O9 2.294(3) 2_455 ? Ca3 O9 2.294(3) 6_655 ? Ca3 O2 2.323(4) . ? Ca3 O2 2.323(4) 5 ? Ca3 C15 3.132(5) 2_455 ? Ca3 C15 3.132(5) 6_655 ? Ca3 Ca1 3.766(2) 5 ? C1 N1 1.340(6) . ? C1 N2 1.349(6) . ? C1 N4 1.368(6) . ? C2 N1 1.340(6) . ? C2 N3 1.342(5) . ? C2 N6 1.351(6) . ? C3 N2 1.340(6) . ? C3 N3 1.348(5) . ? C3 N5 1.378(5) . ? C4 N4 1.448(6) . ? C4 C5 1.510(7) . ? C5 O2 1.238(6) . ? C5 O1 1.271(6) . ? C6 N4 1.430(7) . ? C6 C7 1.506(8) . ? C7 O3 1.224(8) . ? C7 O4 1.294(8) . ? C8 N6 1.464(6) . ? C8 C9 1.506(6) . ? C9 O5 1.252(5) . ? C9 O6 1.256(5) . ? C10 N6 1.457(6) . ? C10 C11 1.509(6) . ? C11 O8 1.231(6) . ? C11 O7 1.251(6) . ? C11 Ca1 3.222(5) 3 ? C12 N5 1.451(6) . ? C12 C13 1.524(6) . ? C13 O10 1.249(5) . ? C13 O9 1.269(5) . ? C13 Ca1 3.007(5) 6_565 ? C14 N5 1.462(6) . ? C14 C15 1.520(6) . ? C15 O12 1.249(6) . ? C15 O11 1.255(6) . ? C15 Ca1 2.947(5) 2_455 ? C15 Ca3 3.132(5) 2_455 ? O6 Ca2 2.360(3) 2 ? O7 Ca1 2.307(4) 3 ? O8 Ca2 2.276(4) 2 ? O9 Ca3 2.294(3) 2_455 ? O9 Ca1 2.589(4) 6_565 ? O10 Ca2 2.404(3) 6_565 ? O10 Ca1 2.675(4) 6_565 ? O11 Ca3 2.293(3) 2_455 ? O11 Ca1 2.512(3) 2_455 ? O12 Ca1 2.644(4) 2_455 ? 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 O7 Ca1 O5 154.79(16) 3_545 . ? O7 Ca1 O3W 96.95(17) 3_545 . ? O5 Ca1 O3W 88.87(16) . . ? O7 Ca1 O2W 88.0(2) 3_545 . ? O5 Ca1 O2W 69.2(2) . . ? O3W Ca1 O2W 77.87(17) . . ? O7 Ca1 O11 120.23(16) 3_545 2_455 ? O5 Ca1 O11 83.15(12) . 2_455 ? O3W Ca1 O11 96.53(16) . 2_455 ? O2W Ca1 O11 151.72(19) . 2_455 ? O7 Ca1 O9 83.46(14) 3_545 6_655 ? O5 Ca1 O9 95.91(12) . 6_655 ? O3W Ca1 O9 167.83(14) . 6_655 ? O2W Ca1 O9 114.29(14) . 6_655 ? O11 Ca1 O9 73.04(11) 2_455 6_655 ? O7 Ca1 O12 82.58(16) 3_545 2_455 ? O5 Ca1 O12 122.16(13) . 2_455 ? O3W Ca1 O12 68.77(16) . 2_455 ? O2W Ca1 O12 143.80(17) . 2_455 ? O11 Ca1 O12 50.01(11) 2_455 2_455 ? O9 Ca1 O12 99.31(14) 6_655 2_455 ? O7 Ca1 O10 88.48(13) 3_545 6_655 ? O5 Ca1 O10 72.64(11) . 6_655 ? O3W Ca1 O10 142.78(14) . 6_655 ? O2W Ca1 O10 65.50(14) . 6_655 ? O11 Ca1 O10 112.40(11) 2_455 6_655 ? O9 Ca1 O10 49.30(10) 6_655 6_655 ? O12 Ca1 O10 148.30(14) 2_455 6_655 ? O7 Ca1 C15 102.65(17) 3_545 2_455 ? O5 Ca1 C15 102.47(13) . 2_455 ? O3W Ca1 C15 81.24(16) . 2_455 ? O2W Ca1 C15 157.55(15) . 2_455 ? O11 Ca1 C15 24.99(12) 2_455 2_455 ? O9 Ca1 C15 86.80(12) 6_655 2_455 ? O12 Ca1 C15 25.06(12) 2_455 2_455 ? O10 Ca1 C15 133.50(13) 6_655 2_455 ? O7 Ca1 C13 86.15(13) 3_545 6_655 ? O5 Ca1 C13 83.26(12) . 6_655 ? O3W Ca1 C13 167.17(14) . 6_655 ? O2W Ca1 C13 89.83(15) . 6_655 ? O11 Ca1 C13 92.59(12) 2_455 6_655 ? O9 Ca1 C13 24.80(10) 6_655 6_655 ? O12 Ca1 C13 124.05(14) 2_455 6_655 ? O10 Ca1 C13 24.52(10) 6_655 6_655 ? C15 Ca1 C13 110.32(13) 2_455 6_655 ? O7 Ca1 C11 18.01(14) 3_545 3_545 ? O5 Ca1 C11 150.23(14) . 3_545 ? O3W Ca1 C11 79.16(16) . 3_545 ? O2W Ca1 C11 81.6(2) . 3_545 ? O11 Ca1 C11 124.97(12) 2_455 3_545 ? O9 Ca1 C11 101.44(12) 6_655 3_545 ? O12 Ca1 C11 78.76(13) 2_455 3_545 ? O10 Ca1 C11 100.95(11) 6_655 3_545 ? C15 Ca1 C11 102.48(13) 2_455 3_545 ? C13 Ca1 C11 102.90(12) 6_655 3_545 ? O7 Ca1 Ca3 105.78(14) 3_545 . ? O5 Ca1 Ca3 87.46(10) . . ? O3W Ca1 Ca3 132.83(13) . . ? O2W Ca1 Ca3 142.13(15) . . ? O11 Ca1 Ca3 36.38(8) 2_455 . ? O9 Ca1 Ca3 36.76(7) 6_655 . ? O12 Ca1 Ca3 73.85(10) 2_455 . ? O10 Ca1 Ca3 79.53(8) 6_655 . ? C15 Ca1 Ca3 53.96(10) 2_455 . ? C13 Ca1 Ca3 57.13(8) 6_655 . ? C11 Ca1 Ca3 120.58(10) 3_545 . ? O8 Ca2 O6 88.56(13) 2 2 ? O8 Ca2 O10 82.16(14) 2 6_655 ? O6 Ca2 O10 151.31(14) 2 6_655 ? O8 Ca2 O4W 105.50(15) 2 . ? O6 Ca2 O4W 75.76(14) 2 . ? O10 Ca2 O4W 80.66(13) 6_655 . ? O8 Ca2 O6 153.05(15) 2 . ? O6 Ca2 O6 71.13(13) 2 . ? O10 Ca2 O6 123.99(12) 6_655 . ? O4W Ca2 O6 86.93(14) . . ? O8 Ca2 O5 148.76(13) 2 . ? O6 Ca2 O5 121.59(11) 2 . ? O10 Ca2 O5 74.46(11) 6_655 . ? O4W Ca2 O5 91.02(13) . . ? O6 Ca2 O5 51.25(10) . . ? O8 Ca2 O1W 72.4(2) 2 . ? O6 Ca2 O1W 79.83(19) 2 . ? O10 Ca2 O1W 122.19(17) 6_655 . ? O4W Ca2 O1W 155.56(19) . . ? O6 Ca2 O1W 86.36(18) . . ? O5 Ca2 O1W 102.9(2) . . ? O8 Ca2 O2W 89.11(15) 2 . ? O6 Ca2 O2W 142.04(16) 2 . ? O10 Ca2 O2W 65.23(15) 6_655 . ? O4W Ca2 O2W 140.77(14) . . ? O6 Ca2 O2W 96.15(15) . . ? O5 Ca2 O2W 62.48(13) . . ? O1W Ca2 O2W 63.4(2) . . ? O8 Ca2 C9 163.94(15) 2 . ? O6 Ca2 C9 96.69(12) 2 . ? O10 Ca2 C9 99.66(12) 6_655 . ? O4W Ca2 C9 90.52(13) . . ? O6 Ca2 C9 25.72(11) . . ? O5 Ca2 C9 25.63(11) . . ? O1W Ca2 C9 93.53(19) . . ? O2W Ca2 C9 77.40(14) . . ? O8 Ca2 Ca1 112.89(10) 2 . ? O6 Ca2 Ca1 158.12(9) 2 . ? O10 Ca2 Ca1 43.63(8) 6_655 . ? O4W Ca2 Ca1 101.21(10) . . ? O6 Ca2 Ca1 87.14(9) . . ? O5 Ca2 Ca1 36.56(8) . . ? O1W Ca2 Ca1 101.89(17) . . ? O2W Ca2 Ca1 40.32(10) . . ? C9 Ca2 Ca1 61.49(9) . . ? O8 Ca2 Ca2 121.75(11) 2 2 ? O6 Ca2 Ca2 37.20(9) 2 2 ? O10 Ca2 Ca2 154.50(9) 6_655 2 ? O4W Ca2 Ca2 83.98(9) . 2 ? O6 Ca2 Ca2 34.41(8) . 2 ? O5 Ca2 Ca2 85.64(8) . 2 ? O1W Ca2 Ca2 77.27(14) . 2 ? O2W Ca2 Ca2 119.25(13) . 2 ? C9 Ca2 Ca2 60.12(9) . 2 ? Ca1 Ca2 Ca2 121.39(5) . 2 ? O11 Ca3 O11 180 6_655 2_455 ? O11 Ca3 O9 82.88(12) 6_655 2_455 ? O11 Ca3 O9 97.12(12) 2_455 2_455 ? O11 Ca3 O9 97.12(12) 6_655 6_655 ? O11 Ca3 O9 82.88(12) 2_455 6_655 ? O9 Ca3 O9 180 2_455 6_655 ? O11 Ca3 O2 88.45(12) 6_655 . ? O11 Ca3 O2 91.55(12) 2_455 . ? O9 Ca3 O2 95.99(12) 2_455 . ? O9 Ca3 O2 84.01(12) 6_655 . ? O11 Ca3 O2 91.55(12) 6_655 5 ? O11 Ca3 O2 88.45(12) 2_455 5 ? O9 Ca3 O2 84.01(12) 2_455 5 ? O9 Ca3 O2 95.99(12) 6_655 5 ? O2 Ca3 O2 180 . 5 ? O11 Ca3 C15 159.93(11) 6_655 2_455 ? O11 Ca3 C15 20.07(11) 2_455 2_455 ? O9 Ca3 C15 92.15(13) 2_455 2_455 ? O9 Ca3 C15 87.85(13) 6_655 2_455 ? O2 Ca3 C15 111.46(13) . 2_455 ? O2 Ca3 C15 68.54(13) 5 2_455 ? O11 Ca3 C15 20.07(11) 6_655 6_655 ? O11 Ca3 C15 159.93(11) 2_455 6_655 ? O9 Ca3 C15 87.85(13) 2_455 6_655 ? O9 Ca3 C15 92.15(13) 6_655 6_655 ? O2 Ca3 C15 68.54(13) . 6_655 ? O2 Ca3 C15 111.46(13) 5 6_655 ? C15 Ca3 C15 180 2_455 6_655 ? O11 Ca3 Ca1 139.49(8) 6_655 . ? O11 Ca3 Ca1 40.51(8) 2_455 . ? O9 Ca3 Ca1 137.53(8) 2_455 . ? O9 Ca3 Ca1 42.47(8) 6_655 . ? O2 Ca3 Ca1 84.82(9) . . ? O2 Ca3 Ca1 95.18(9) 5 . ? C15 Ca3 Ca1 49.54(9) 2_455 . ? C15 Ca3 Ca1 130.46(9) 6_655 . ? O11 Ca3 Ca1 40.51(8) 6_655 5 ? O11 Ca3 Ca1 139.49(8) 2_455 5 ? O9 Ca3 Ca1 42.47(8) 2_455 5 ? O9 Ca3 Ca1 137.53(8) 6_655 5 ? O2 Ca3 Ca1 95.18(9) . 5 ? O2 Ca3 Ca1 84.82(9) 5 5 ? C15 Ca3 Ca1 130.46(9) 2_455 5 ? C15 Ca3 Ca1 49.54(9) 6_655 5 ? Ca1 Ca3 Ca1 180 . 5 ? N1 C1 N2 125.9(4) . . ? N1 C1 N4 117.5(4) . . ? N2 C1 N4 116.5(4) . . ? N1 C2 N3 126.0(4) . . ? N1 C2 N6 116.4(4) . . ? N3 C2 N6 117.5(4) . . ? N2 C3 N3 127.2(4) . . ? N2 C3 N5 116.5(4) . . ? N3 C3 N5 116.3(4) . . ? N4 C4 C5 115.4(4) . . ? O2 C5 O1 121.9(5) . . ? O2 C5 C4 118.7(4) . . ? O1 C5 C4 119.4(4) . . ? N4 C6 C7 116.4(5) . . ? O3 C7 O4 121.7(6) . . ? O3 C7 C6 118.0(6) . . ? O4 C7 C6 120.3(5) . . ? N6 C8 C9 116.7(3) . . ? O5 C9 O6 121.4(4) . . ? O5 C9 C8 117.3(4) . . ? O6 C9 C8 121.2(4) . . ? O5 C9 Ca2 61.1(2) . . ? O6 C9 Ca2 60.7(2) . . ? C8 C9 Ca2 170.3(3) . . ? N6 C10 C11 118.4(4) . . ? O8 C11 O7 125.4(5) . . ? O8 C11 C10 120.4(4) . . ? O7 C11 C10 114.1(4) . . ? O8 C11 Ca1 95.1(3) . 3 ? O7 C11 Ca1 34.8(2) . 3 ? C10 C11 Ca1 139.1(3) . 3 ? N5 C12 C13 117.9(4) . . ? O10 C13 O9 121.5(4) . . ? O10 C13 C12 117.0(4) . . ? O9 C13 C12 121.5(4) . . ? O10 C13 Ca1 62.7(2) . 6_565 ? O9 C13 Ca1 58.8(2) . 6_565 ? C12 C13 Ca1 178.4(3) . 6_565 ? N5 C14 C15 115.7(4) . . ? O12 C15 O11 121.3(4) . . ? O12 C15 C14 117.9(4) . . ? O11 C15 C14 120.7(4) . . ? O12 C15 Ca1 63.8(3) . 2_455 ? O11 C15 Ca1 57.7(2) . 2_455 ? C14 C15 Ca1 176.9(3) . 2_455 ? O12 C15 Ca3 123.0(4) . 2_455 ? O11 C15 Ca3 38.8(2) . 2_455 ? C14 C15 Ca3 104.0(3) . 2_455 ? Ca1 C15 Ca3 76.49(12) 2_455 2_455 ? C2 N1 C1 114.5(4) . . ? C3 N2 C1 113.0(4) . . ? C2 N3 C3 113.1(4) . . ? C1 N4 C6 118.9(4) . . ? C1 N4 C4 119.6(4) . . ? C6 N4 C4 120.9(4) . . ? C3 N5 C12 120.3(4) . . ? C3 N5 C14 118.0(4) . . ? C12 N5 C14 120.0(4) . . ? C2 N6 C10 121.2(4) . . ? C2 N6 C8 118.6(4) . . ? C10 N6 C8 119.5(4) . . ? C5 O2 Ca3 135.5(3) . . ? Ca1 O2W Ca2 93.90(18) . . ? C9 O5 Ca1 156.4(3) . . ? C9 O5 Ca2 93.3(3) . . ? Ca1 O5 Ca2 103.55(13) . . ? C9 O6 Ca2 158.0(3) . 2 ? C9 O6 Ca2 93.6(3) . . ? Ca2 O6 Ca2 108.40(13) 2 . ? C11 O7 Ca1 127.2(4) . 3 ? C11 O8 Ca2 147.5(4) . 2 ? C13 O9 Ca3 134.2(3) . 2_455 ? C13 O9 Ca1 96.4(3) . 6_565 ? Ca3 O9 Ca1 100.77(12) 2_455 6_565 ? C13 O10 Ca2 137.4(3) . 6_565 ? C13 O10 Ca1 92.8(3) . 6_565 ? Ca2 O10 Ca1 98.03(11) 6_565 6_565 ? C15 O11 Ca3 121.1(3) . 2_455 ? C15 O11 Ca1 97.3(3) . 2_455 ? Ca3 O11 Ca1 103.11(13) 2_455 2_455 ? C15 O12 Ca1 91.2(3) . 2_455 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.274 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.092 # Attachment 'complex-3.CIF' data_complex-3 #TrackingRef 'complex-3.CIF' _database_code_depnum_ccdc_archive 'CCDC 769619' #TrackingRef '- complex 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H20 Cd3 N6 O16' _chemical_formula_weight 877.57 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.993(5) _cell_length_b 20.997(10) _cell_length_c 22.177(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4653(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10252 _cell_measurement_theta_min 3.3583 _cell_measurement_theta_max 27.4719 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3392 _exptl_absorpt_coefficient_mu 2.813 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6643 _exptl_absorpt_correction_T_max 1.0000 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31326 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.66 _reflns_number_total 5268 _reflns_number_gt 4476 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0683P)^2^+54.9197P] 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_extinction_coef ? _refine_ls_number_reflns 5268 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1685 _refine_ls_wR_factor_gt 0.1474 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _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 Cd1 Cd 0.05300(7) 0.06236(3) 0.39032(3) 0.02931(19) Uani 1 1 d . . . Cd2 Cd -0.75583(7) 0.32181(3) 0.37062(3) 0.02663(18) Uani 1 1 d . . . Cd3 Cd -0.33321(7) 0.08599(3) 0.27423(3) 0.03031(19) Uani 1 1 d . . . N3 N -0.3700(7) 0.3102(3) 0.3644(3) 0.0240(14) Uani 1 1 d . . . N6 N -0.5521(7) 0.3127(3) 0.2976(3) 0.0221(14) Uani 1 1 d . . . O4 O -0.2018(7) 0.0837(3) 0.3586(3) 0.0367(15) Uani 1 1 d . . . C1 C -0.4207(9) 0.1868(4) 0.3852(4) 0.0237(17) Uani 1 1 d . . . O3 O -0.1420(7) 0.0519(3) 0.4485(3) 0.0361(15) Uani 1 1 d . . . N1 N -0.5028(8) 0.2167(3) 0.3452(3) 0.0271(15) Uani 1 1 d . . . N5 N -0.1978(8) 0.3028(3) 0.4337(3) 0.0282(15) Uani 1 1 d . . . N2 N -0.3182(7) 0.2126(3) 0.4153(3) 0.0230(14) Uani 1 1 d . . . N4 N -0.4511(7) 0.1231(3) 0.3964(3) 0.0296(16) Uani 1 1 d . . . C7 C -0.2272(10) 0.0734(4) 0.4136(4) 0.0281(18) Uani 1 1 d . . . C2 C -0.4674(9) 0.2780(4) 0.3375(3) 0.0233(16) Uani 1 1 d . . . C3 C -0.2989(8) 0.2746(4) 0.4033(3) 0.0209(15) Uani 1 1 d . . . O7 O -0.6683(7) 0.4174(3) 0.3515(3) 0.0379(15) Uani 1 1 d . . . C14 C -0.1698(9) 0.3706(4) 0.4285(4) 0.0293(18) Uani 1 1 d . . . H14A H -0.1695 0.3894 0.4685 0.035 Uiso 1 1 calc R . . H14B H -0.2410 0.3907 0.4056 0.035 Uiso 1 1 calc R . . C8 C -0.6077(8) 0.2768(4) 0.2465(4) 0.0235(16) Uani 1 1 d . . . H8A H -0.5352 0.2540 0.2270 0.028 Uiso 1 1 calc R . . H8B H -0.6434 0.3069 0.2175 0.028 Uiso 1 1 calc R . . C10 C -0.5024(10) 0.3772(4) 0.2821(4) 0.0287(18) Uani 1 1 d . . . H10A H -0.5287 0.3876 0.2411 0.034 Uiso 1 1 calc R . . H10B H -0.4054 0.3776 0.2840 0.034 Uiso 1 1 calc R . . C11 C -0.5586(10) 0.4275(4) 0.3255(4) 0.0270(18) Uani 1 1 d . . . C15 C -0.0350(11) 0.3848(4) 0.3976(4) 0.037(2) Uani 1 1 d . . . C6 C -0.3653(9) 0.0878(4) 0.4380(4) 0.0286(18) Uani 1 1 d . . . H6A H -0.4090 0.0480 0.4481 0.034 Uiso 1 1 calc R . . H6B H -0.3561 0.1122 0.4749 0.034 Uiso 1 1 calc R . . C12 C -0.1094(10) 0.2622(4) 0.4693(4) 0.0321(19) Uani 1 1 d . . . H12A H -0.0327 0.2872 0.4818 0.039 Uiso 1 1 calc R . . H12B H -0.0767 0.2282 0.4436 0.039 Uiso 1 1 calc R . . O11 O 0.0319(9) 0.3398(4) 0.3785(4) 0.058(2) Uani 1 1 d . . . O8 O -0.4919(7) 0.4783(3) 0.3302(3) 0.0385(16) Uani 1 1 d . . . O6 O -0.7958(7) 0.2424(3) 0.3039(3) 0.0324(14) Uani 1 1 d . . . O2 O -0.5520(7) 0.0736(4) 0.2844(3) 0.0391(16) Uani 1 1 d . . . C5 C -0.6311(10) 0.0801(4) 0.3267(4) 0.0313(19) Uani 1 1 d . . . C9 C -0.7159(8) 0.2297(4) 0.2621(3) 0.0231(16) Uani 1 1 d . . . C4 C -0.5903(9) 0.1025(4) 0.3889(4) 0.0293(18) Uani 1 1 d . . . H4A H -0.6481 0.1377 0.4000 0.035 Uiso 1 1 calc R . . H4B H -0.6072 0.0682 0.4171 0.035 Uiso 1 1 calc R . . C13 C -0.1727(10) 0.2328(4) 0.5249(4) 0.033(2) Uani 1 1 d . . . O12 O -0.0172(15) 0.4411(5) 0.3860(8) 0.135(7) Uani 1 1 d . . . O9 O -0.2655(7) 0.2595(3) 0.5526(3) 0.0352(15) Uani 1 1 d . . . O10 O -0.1196(7) 0.1817(3) 0.5435(3) 0.0367(15) Uani 1 1 d . . . O5 O -0.7273(6) 0.1819(3) 0.2280(3) 0.0290(13) Uani 1 1 d . . . O1 O -0.7563(6) 0.0712(3) 0.3212(3) 0.0318(14) Uani 1 1 d . . . O13 O 0.2009(8) 0.0013(3) 0.4439(3) 0.0391(16) Uani 1 1 d . . . O14 O 0.0916(7) 0.1324(3) 0.4689(3) 0.0429(17) Uani 1 1 d . . . O15 O -0.2813(10) -0.0212(3) 0.2874(4) 0.064(3) Uani 1 1 d . . . O16 O 0.0296(9) 0.1463(4) 0.3244(5) 0.078(3) 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 Cd1 0.0316(4) 0.0293(3) 0.0270(3) 0.0000(2) -0.0005(2) -0.0030(3) Cd2 0.0277(4) 0.0279(3) 0.0242(3) -0.0025(2) 0.0026(2) -0.0033(2) Cd3 0.0333(4) 0.0284(3) 0.0292(3) 0.0022(2) 0.0054(3) -0.0033(3) N3 0.018(4) 0.026(3) 0.028(3) -0.002(2) -0.006(3) 0.000(3) N6 0.018(4) 0.026(3) 0.023(3) 0.002(2) -0.004(3) -0.001(3) O4 0.040(4) 0.037(3) 0.034(3) 0.007(3) 0.008(3) 0.003(3) C1 0.027(5) 0.021(4) 0.024(4) 0.004(3) 0.006(3) 0.000(3) O3 0.023(3) 0.052(4) 0.033(3) 0.008(3) 0.003(3) 0.010(3) N1 0.031(4) 0.023(3) 0.027(3) 0.000(3) -0.003(3) -0.001(3) N5 0.024(4) 0.030(4) 0.031(4) -0.001(3) -0.003(3) -0.003(3) N2 0.018(4) 0.029(3) 0.022(3) -0.001(2) -0.005(3) 0.001(3) N4 0.021(4) 0.029(4) 0.038(4) 0.008(3) 0.002(3) -0.008(3) C7 0.038(5) 0.019(4) 0.027(4) 0.002(3) 0.003(4) -0.001(3) C2 0.027(5) 0.022(4) 0.021(3) -0.001(3) -0.003(3) 0.000(3) C3 0.014(4) 0.029(4) 0.020(3) -0.003(3) -0.002(3) 0.000(3) O7 0.036(4) 0.029(3) 0.049(4) -0.005(3) 0.006(3) -0.003(3) C14 0.021(5) 0.036(4) 0.031(4) -0.006(3) 0.005(3) -0.004(3) C8 0.014(4) 0.028(4) 0.028(4) -0.001(3) 0.010(3) -0.004(3) C10 0.037(5) 0.026(4) 0.024(4) 0.002(3) -0.009(4) 0.001(4) C11 0.033(5) 0.017(4) 0.030(4) 0.002(3) -0.003(4) 0.000(3) C15 0.044(6) 0.028(4) 0.038(5) -0.003(4) 0.009(4) -0.010(4) C6 0.024(5) 0.030(4) 0.032(4) 0.007(3) 0.006(3) -0.003(3) C12 0.038(5) 0.037(5) 0.021(4) 0.004(3) -0.006(4) -0.002(4) O11 0.042(5) 0.053(5) 0.078(6) 0.000(4) 0.020(4) 0.003(4) O8 0.045(4) 0.026(3) 0.045(4) -0.009(3) 0.007(3) -0.005(3) O6 0.034(4) 0.031(3) 0.032(3) -0.008(2) 0.004(3) 0.000(3) O2 0.018(4) 0.062(5) 0.038(4) -0.012(3) 0.013(3) -0.007(3) C5 0.037(6) 0.024(4) 0.032(4) 0.001(3) 0.007(4) 0.005(4) C9 0.021(4) 0.025(4) 0.023(4) -0.001(3) -0.005(3) -0.001(3) C4 0.024(5) 0.033(4) 0.030(4) 0.002(3) -0.004(3) -0.004(4) C13 0.045(6) 0.034(5) 0.020(4) -0.002(3) 0.000(4) -0.006(4) O12 0.120(11) 0.059(7) 0.226(18) -0.010(8) 0.119(12) -0.027(7) O9 0.028(4) 0.047(4) 0.031(3) -0.003(3) 0.011(3) 0.009(3) O10 0.037(4) 0.044(4) 0.029(3) 0.003(3) 0.000(3) 0.007(3) O5 0.023(3) 0.028(3) 0.036(3) -0.007(2) 0.008(3) -0.008(2) O1 0.008(3) 0.055(4) 0.033(3) -0.005(3) -0.004(2) -0.006(2) O13 0.049(5) 0.036(3) 0.033(3) 0.002(3) 0.004(3) 0.005(3) O14 0.038(4) 0.038(4) 0.052(4) -0.019(3) 0.005(3) -0.004(3) O15 0.085(7) 0.028(4) 0.080(6) -0.002(4) -0.037(5) -0.005(4) O16 0.043(5) 0.064(5) 0.126(9) 0.057(6) -0.039(5) -0.022(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O13 2.289(7) . ? Cd1 O8 2.295(6) 8 ? Cd1 O16 2.301(8) . ? Cd1 O14 2.311(6) . ? Cd1 O3 2.347(6) . ? Cd1 O1 2.453(6) 1_655 ? Cd2 O11 2.162(9) 1_455 ? Cd2 O7 2.231(6) . ? Cd2 O6 2.265(6) . ? Cd2 O10 2.342(7) 4_456 ? Cd2 O9 2.414(7) 4_456 ? Cd2 N6 2.608(7) . ? Cd2 C13 2.715(9) 4_456 ? Cd3 O2 2.213(7) . ? Cd3 O1 2.273(6) 6_656 ? Cd3 O5 2.276(6) 6_656 ? Cd3 O4 2.286(7) . ? Cd3 O15 2.329(8) . ? N3 C2 1.327(10) . ? N3 C3 1.346(10) . ? N6 C2 1.424(10) . ? N6 C8 1.470(10) . ? N6 C10 1.484(10) . ? O4 C7 1.265(10) . ? C1 N2 1.337(11) . ? C1 N1 1.362(11) . ? C1 N4 1.393(10) . ? O3 C7 1.236(11) . ? N1 C2 1.346(10) . ? N5 C3 1.351(10) . ? N5 C14 1.457(11) . ? N5 C12 1.458(11) . ? N2 C3 1.343(10) . ? N4 C4 1.466(11) . ? N4 C6 1.460(11) . ? C7 C6 1.513(13) . ? O7 C11 1.256(11) . ? C14 C15 1.540(13) . ? C8 C9 1.506(11) . ? C10 C11 1.536(12) . ? C11 O8 1.261(10) . ? C15 O11 1.232(13) . ? C15 O12 1.223(14) . ? C12 C13 1.518(11) . ? O11 Cd2 2.162(9) 1_655 ? O8 Cd1 2.295(6) 8_565 ? O6 C9 1.251(10) . ? O2 C5 1.235(11) . ? C5 O1 1.270(11) . ? C5 C4 1.512(12) . ? C9 O5 1.262(9) . ? C13 O10 1.266(11) . ? C13 O9 1.246(11) . ? C13 Cd2 2.715(9) 4_556 ? O9 Cd2 2.414(7) 4_556 ? O10 Cd2 2.342(7) 4_556 ? O5 Cd3 2.276(6) 6_556 ? O1 Cd3 2.273(6) 6_556 ? O1 Cd1 2.453(6) 1_455 ? 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 O13 Cd1 O8 92.4(2) . 8 ? O13 Cd1 O16 145.5(3) . . ? O8 Cd1 O16 101.2(3) 8 . ? O13 Cd1 O14 81.8(3) . . ? O8 Cd1 O14 166.2(3) 8 . ? O16 Cd1 O14 90.5(4) . . ? O13 Cd1 O3 101.4(2) . . ? O8 Cd1 O3 91.5(3) 8 . ? O16 Cd1 O3 109.7(3) . . ? O14 Cd1 O3 77.5(3) . . ? O13 Cd1 O1 82.3(2) . 1_655 ? O8 Cd1 O1 84.4(2) 8 1_655 ? O16 Cd1 O1 67.9(3) . 1_655 ? O14 Cd1 O1 107.1(2) . 1_655 ? O3 Cd1 O1 174.6(2) . 1_655 ? O11 Cd2 O7 104.0(3) 1_455 . ? O11 Cd2 O6 90.5(3) 1_455 . ? O7 Cd2 O6 127.4(2) . . ? O11 Cd2 O10 120.7(3) 1_455 4_456 ? O7 Cd2 O10 87.4(3) . 4_456 ? O6 Cd2 O10 127.6(2) . 4_456 ? O11 Cd2 O9 91.6(3) 1_455 4_456 ? O7 Cd2 O9 141.9(2) . 4_456 ? O6 Cd2 O9 86.2(2) . 4_456 ? O10 Cd2 O9 55.1(2) 4_456 4_456 ? O11 Cd2 N6 146.0(3) 1_455 . ? O7 Cd2 N6 69.0(2) . . ? O6 Cd2 N6 71.2(2) . . ? O10 Cd2 N6 92.8(2) 4_456 . ? O9 Cd2 N6 114.7(2) 4_456 . ? O11 Cd2 C13 107.7(3) 1_455 4_456 ? O7 Cd2 C13 115.0(3) . 4_456 ? O6 Cd2 C13 107.5(2) . 4_456 ? O10 Cd2 C13 27.8(3) 4_456 4_456 ? O9 Cd2 C13 27.3(2) 4_456 4_456 ? N6 Cd2 C13 105.0(3) . 4_456 ? O2 Cd3 O1 114.4(2) . 6_656 ? O2 Cd3 O5 124.4(3) . 6_656 ? O1 Cd3 O5 86.8(2) 6_656 6_656 ? O2 Cd3 O4 118.8(3) . . ? O1 Cd3 O4 124.4(2) 6_656 . ? O5 Cd3 O4 76.6(2) 6_656 . ? O2 Cd3 O15 95.4(3) . . ? O1 Cd3 O15 84.8(3) 6_656 . ? O5 Cd3 O15 139.0(3) 6_656 . ? O4 Cd3 O15 75.5(3) . . ? C2 N3 C3 113.0(7) . . ? C2 N6 C8 116.2(6) . . ? C2 N6 C10 114.3(6) . . ? C8 N6 C10 114.5(6) . . ? C2 N6 Cd2 96.7(5) . . ? C8 N6 Cd2 102.8(4) . . ? C10 N6 Cd2 109.8(5) . . ? C7 O4 Cd3 132.7(7) . . ? N2 C1 N1 126.9(7) . . ? N2 C1 N4 117.8(7) . . ? N1 C1 N4 115.3(7) . . ? C7 O3 Cd1 101.2(6) . . ? C2 N1 C1 111.4(7) . . ? C3 N5 C14 122.2(7) . . ? C3 N5 C12 117.8(7) . . ? C14 N5 C12 119.9(7) . . ? C3 N2 C1 113.8(7) . . ? C1 N4 C4 118.0(7) . . ? C1 N4 C6 118.1(7) . . ? C4 N4 C6 118.6(7) . . ? O3 C7 O4 121.9(9) . . ? O3 C7 C6 118.6(8) . . ? O4 C7 C6 119.5(8) . . ? N3 C2 N1 128.6(7) . . ? N3 C2 N6 117.0(7) . . ? N1 C2 N6 114.3(7) . . ? N2 C3 N3 126.2(7) . . ? N2 C3 N5 115.7(7) . . ? N3 C3 N5 118.1(7) . . ? C11 O7 Cd2 125.5(5) . . ? N5 C14 C15 113.1(7) . . ? N6 C8 C9 115.5(6) . . ? N6 C10 C11 111.1(7) . . ? O7 C11 O8 124.4(8) . . ? O7 C11 C10 119.4(7) . . ? O8 C11 C10 116.1(8) . . ? O11 C15 O12 126.1(11) . . ? O11 C15 C14 118.6(8) . . ? O12 C15 C14 114.0(10) . . ? N4 C6 C7 114.3(7) . . ? N5 C12 C13 115.2(8) . . ? C15 O11 Cd2 134.0(8) . 1_655 ? C11 O8 Cd1 123.9(6) . 8_565 ? C9 O6 Cd2 121.9(5) . . ? C5 O2 Cd3 134.2(7) . . ? O2 C5 O1 122.7(9) . . ? O2 C5 C4 123.6(9) . . ? O1 C5 C4 113.6(8) . . ? O6 C9 O5 123.8(8) . . ? O6 C9 C8 119.2(7) . . ? O5 C9 C8 116.6(7) . . ? N4 C4 C5 116.9(8) . . ? O10 C13 O9 122.2(8) . . ? O10 C13 C12 115.8(8) . . ? O9 C13 C12 121.8(8) . . ? O10 C13 Cd2 59.5(4) . 4_556 ? O9 C13 Cd2 62.8(5) . 4_556 ? C12 C13 Cd2 173.2(7) . 4_556 ? C13 O9 Cd2 89.9(5) . 4_556 ? C13 O10 Cd2 92.8(5) . 4_556 ? C9 O5 Cd3 139.3(5) . 6_556 ? C5 O1 Cd3 113.8(6) . 6_556 ? C5 O1 Cd1 135.7(6) . 1_455 ? Cd3 O1 Cd1 109.2(2) 6_556 1_455 ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.781 _refine_diff_density_min -1.289 _refine_diff_density_rms 0.242 # Attachment '- complex 1.CIF' data_complex-1 #TrackingRef 'complex-1.CIF' _database_code_depnum_ccdc_archive 'CCDC 769620' #TrackingRef '- complex 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H64 Co3 N12 Na2 O42' _chemical_formula_weight 1487.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' Co Co 0.3490 0.9720 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0360 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 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 10.005(5) _cell_length_b 10.433(5) _cell_length_c 14.519(7) _cell_angle_alpha 94.798(4) _cell_angle_beta 109.001(7) _cell_angle_gamma 99.623(7) _cell_volume 1397.2(12) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4424 _cell_measurement_theta_min 2.2003 _cell_measurement_theta_max 27.4700 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.2200 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1600 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 727 _exptl_absorpt_coefficient_mu 1.018 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8464 _exptl_absorpt_correction_T_max 1.0000 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11771 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.45 _reflns_number_total 6265 _reflns_number_gt 4927 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0934P)^2^+0.5591P] 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_extinction_coef ? _refine_ls_number_reflns 6265 _refine_ls_number_parameters 412 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1688 _refine_ls_wR_factor_gt 0.1531 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 Co1 Co 0.0000 0.5000 0.5000 0.02237(17) Uani 1 2 d S . . Co2 Co 0.75840(5) 0.86611(5) 0.36249(3) 0.02626(15) Uani 1 1 d . . . Na1 Na -0.59545(18) 0.74439(17) -0.21638(13) 0.0410(4) Uani 1 1 d . . . N1 N -0.0044(3) 0.6710(3) 0.1439(2) 0.0263(6) Uani 1 1 d . . . N2 N -0.0294(3) 0.7372(3) -0.0146(2) 0.0282(6) Uani 1 1 d . . . N3 N 0.1596(3) 0.8578(3) 0.1307(2) 0.0256(6) Uani 1 1 d . . . N4 N 0.1271(3) 0.9260(3) -0.0193(2) 0.0261(6) Uani 1 1 d . . . N5 N 0.1728(3) 0.7971(3) 0.2818(2) 0.0249(6) Uani 1 1 d . . . N6 N -0.1738(3) 0.5495(3) 0.0023(2) 0.0269(6) Uani 1 1 d . . . O1 O 0.4168(3) 0.7124(3) 0.2904(3) 0.0515(9) Uani 1 1 d . . . O1W O 0.4442(8) 0.2527(8) 0.4625(6) 0.156(3) Uani 1 1 d . . . O2 O 0.5626(3) 0.9040(3) 0.3692(2) 0.0335(6) Uani 1 1 d . . . O2WA O 0.2488(9) 0.3686(11) 0.3475(6) 0.083(3) Uani 0.50 1 d P . . O2WB O 0.3626(12) 0.4899(9) 0.3918(8) 0.092(3) Uani 0.50 1 d P . . O3 O -0.3990(4) 0.6365(4) -0.2223(2) 0.0518(8) Uani 1 1 d . . . O3W O -0.6413(5) 0.7678(5) -0.3806(3) 0.0776(13) Uani 1 1 d . . . O4 O -0.2787(3) 0.4962(3) 0.21127(19) 0.0366(6) Uani 1 1 d . . . O5 O 0.0296(3) 0.8073(3) -0.2788(2) 0.0429(7) Uani 1 1 d . . . O6 O 0.4848(3) 1.0290(3) 0.15062(19) 0.0364(6) Uani 1 1 d . . . O7 O 0.2280(3) 0.8045(3) -0.15322(19) 0.0338(6) Uani 1 1 d . . . O8 O -0.4109(3) 0.6666(3) -0.07490(18) 0.0324(6) Uani 1 1 d . . . O9 O 0.4033(3) 0.8695(3) 0.0240(2) 0.0341(6) Uani 1 1 d . . . O10 O -0.3541(3) 0.6232(3) 0.09825(19) 0.0343(6) Uani 1 1 d . . . O11 O -0.0411(3) 0.8407(3) 0.3562(2) 0.0364(6) Uani 1 1 d . . . O12 O -0.0062(3) 0.6852(2) 0.45135(18) 0.0276(5) Uani 1 1 d . . . O13 O 0.6709(3) 0.6601(2) 0.34221(19) 0.0300(5) Uani 1 1 d . . . O14 O 0.6934(3) 0.8712(3) 0.20955(19) 0.0341(6) Uani 1 1 d . . . O15 O 0.8309(3) 1.0683(3) 0.3901(2) 0.0392(7) Uani 1 1 d . . . O16 O 0.8394(3) 0.8652(4) 0.5174(2) 0.0534(9) Uani 1 1 d . . . O17 O 0.2178(3) 0.4952(3) 0.5121(2) 0.0337(6) Uani 1 1 d . . . O18 O 0.0760(3) 0.5868(3) 0.64509(18) 0.0406(7) Uani 1 1 d . . . C1 C -0.0648(4) 0.6564(3) 0.0454(3) 0.0241(7) Uani 1 1 d . . . C2 C 0.1078(3) 0.7733(3) 0.1829(2) 0.0230(7) Uani 1 1 d . . . C3 C 0.0841(4) 0.8363(3) 0.0341(2) 0.0233(7) Uani 1 1 d . . . C4 C 0.0504(4) 0.9157(4) -0.1249(3) 0.0295(8) Uani 1 1 d . . . H4A H 0.0551 1.0036 -0.1426 0.035 Uiso 1 1 calc R . . H4B H -0.0506 0.8768 -0.1390 0.035 Uiso 1 1 calc R . . C5 C -0.2208(4) 0.4656(3) 0.0647(3) 0.0280(7) Uani 1 1 d . . . H5A H -0.1388 0.4343 0.1058 0.034 Uiso 1 1 calc R . . H5B H -0.2914 0.3897 0.0236 0.034 Uiso 1 1 calc R . . C6 C -0.2487(4) 0.5308(4) -0.1035(3) 0.0309(8) Uani 1 1 d . . . H6A H -0.2976 0.4394 -0.1251 0.037 Uiso 1 1 calc R . . H6B H -0.1777 0.5486 -0.1355 0.037 Uiso 1 1 calc R . . C7 C 0.3088(4) 0.8908(4) 0.3262(3) 0.0273(7) Uani 1 1 d . . . H7A H 0.3190 0.9244 0.3930 0.033 Uiso 1 1 calc R . . H7B H 0.3079 0.9642 0.2894 0.033 Uiso 1 1 calc R . . C8 C 0.2544(4) 1.0279(3) 0.0301(3) 0.0287(7) Uani 1 1 d . . . H8A H 0.2382 1.0805 0.0823 0.034 Uiso 1 1 calc R . . H8B H 0.2693 1.0851 -0.0165 0.034 Uiso 1 1 calc R . . C9 C 0.1300(4) 0.7087(3) 0.3441(3) 0.0258(7) Uani 1 1 d . . . H9A H 0.2157 0.7029 0.3980 0.031 Uiso 1 1 calc R . . H9B H 0.0900 0.6218 0.3059 0.031 Uiso 1 1 calc R . . C10 C 0.4395(4) 0.8290(4) 0.3282(3) 0.0291(8) Uani 1 1 d . . . C11 C -0.3582(4) 0.6162(4) -0.1370(3) 0.0316(8) Uani 1 1 d . . . C12 C 0.3896(4) 0.9746(3) 0.0738(3) 0.0281(7) Uani 1 1 d . . . C13 C 0.1083(4) 0.8353(3) -0.1889(3) 0.0290(7) Uani 1 1 d . . . C14 C -0.2871(4) 0.5337(3) 0.1303(3) 0.0276(7) Uani 1 1 d . . . C15 C 0.0190(4) 0.7484(3) 0.3873(2) 0.0229(7) 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 Co1 0.0259(4) 0.0240(3) 0.0208(3) 0.0067(2) 0.0102(3) 0.0091(3) Co2 0.0204(3) 0.0285(3) 0.0324(3) 0.0075(2) 0.0105(2) 0.00780(19) Na1 0.0383(9) 0.0427(9) 0.0486(9) 0.0074(7) 0.0207(7) 0.0146(7) N1 0.0203(14) 0.0297(15) 0.0303(14) 0.0097(12) 0.0099(12) 0.0039(12) N2 0.0272(16) 0.0298(15) 0.0300(14) 0.0065(12) 0.0121(13) 0.0071(13) N3 0.0226(15) 0.0291(15) 0.0283(14) 0.0076(12) 0.0123(12) 0.0047(12) N4 0.0249(15) 0.0277(15) 0.0293(14) 0.0083(12) 0.0129(12) 0.0057(12) N5 0.0148(13) 0.0337(15) 0.0280(14) 0.0082(12) 0.0100(11) 0.0035(12) N6 0.0225(15) 0.0257(14) 0.0305(14) 0.0020(12) 0.0073(12) 0.0046(12) O1 0.0234(14) 0.0360(16) 0.087(2) -0.0126(16) 0.0132(15) 0.0062(12) O1W 0.142(5) 0.207(8) 0.195(7) 0.101(6) 0.131(5) 0.065(5) O2 0.0181(12) 0.0353(14) 0.0438(14) -0.0014(12) 0.0088(11) 0.0038(11) O2WA 0.060(5) 0.135(9) 0.053(4) 0.000(5) 0.029(4) 0.004(5) O2WB 0.138(8) 0.071(5) 0.135(8) 0.052(5) 0.116(7) 0.048(6) O3 0.059(2) 0.073(2) 0.0370(15) 0.0201(15) 0.0216(15) 0.0360(18) O3W 0.084(3) 0.115(4) 0.0477(19) 0.022(2) 0.022(2) 0.056(3) O4 0.0392(16) 0.0440(16) 0.0312(13) 0.0097(12) 0.0132(12) 0.0169(13) O5 0.0486(18) 0.0431(16) 0.0331(14) -0.0003(12) 0.0074(13) 0.0152(14) O6 0.0341(15) 0.0348(14) 0.0355(14) 0.0045(12) 0.0074(12) 0.0046(12) O7 0.0320(14) 0.0355(14) 0.0385(14) 0.0026(11) 0.0154(12) 0.0144(11) O8 0.0333(14) 0.0345(14) 0.0329(13) 0.0081(11) 0.0125(11) 0.0130(11) O9 0.0304(14) 0.0323(14) 0.0426(14) 0.0049(11) 0.0137(12) 0.0128(11) O10 0.0402(16) 0.0358(14) 0.0320(13) 0.0063(11) 0.0134(12) 0.0187(12) O11 0.0315(14) 0.0429(15) 0.0516(16) 0.0277(13) 0.0251(13) 0.0206(12) O12 0.0322(14) 0.0283(12) 0.0301(12) 0.0120(10) 0.0172(11) 0.0107(10) O13 0.0253(13) 0.0303(13) 0.0373(13) 0.0079(11) 0.0128(11) 0.0082(10) O14 0.0359(15) 0.0352(14) 0.0310(13) 0.0071(11) 0.0083(11) 0.0129(12) O15 0.0390(16) 0.0305(14) 0.0418(15) -0.0002(12) 0.0095(13) 0.0020(12) O16 0.0373(17) 0.083(2) 0.0392(16) 0.0237(16) 0.0094(13) 0.0115(16) O17 0.0287(14) 0.0398(15) 0.0408(14) 0.0173(12) 0.0172(12) 0.0132(12) O18 0.0600(19) 0.0370(15) 0.0230(12) 0.0014(11) 0.0079(12) 0.0199(14) C1 0.0181(16) 0.0245(16) 0.0327(17) 0.0064(13) 0.0111(13) 0.0070(13) C2 0.0170(16) 0.0287(17) 0.0276(16) 0.0082(13) 0.0106(13) 0.0083(13) C3 0.0201(16) 0.0269(16) 0.0295(16) 0.0089(13) 0.0140(13) 0.0092(13) C4 0.0295(19) 0.0349(19) 0.0309(17) 0.0131(15) 0.0141(15) 0.0134(15) C5 0.0256(18) 0.0227(16) 0.0365(18) 0.0050(14) 0.0115(15) 0.0050(14) C6 0.0279(19) 0.0294(18) 0.0330(18) -0.0020(15) 0.0086(15) 0.0063(15) C7 0.0208(17) 0.0317(18) 0.0308(17) 0.0019(14) 0.0110(14) 0.0063(14) C8 0.0295(19) 0.0250(17) 0.0388(19) 0.0098(14) 0.0188(16) 0.0078(14) C9 0.0203(16) 0.0320(18) 0.0307(16) 0.0137(14) 0.0115(14) 0.0105(14) C10 0.0203(17) 0.0341(19) 0.0342(18) 0.0052(15) 0.0107(15) 0.0064(15) C11 0.030(2) 0.0296(18) 0.0350(19) 0.0056(15) 0.0115(16) 0.0054(15) C12 0.0286(19) 0.0284(17) 0.0326(18) 0.0113(14) 0.0161(15) 0.0056(15) C13 0.0309(19) 0.0238(16) 0.0337(18) 0.0083(14) 0.0124(15) 0.0053(14) C14 0.0226(18) 0.0266(17) 0.0297(17) 0.0013(14) 0.0049(14) 0.0046(14) C15 0.0207(16) 0.0245(16) 0.0248(15) 0.0065(13) 0.0086(13) 0.0053(13) _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 Co1 O18 2.060(3) . ? Co1 O18 2.060(3) 2_566 ? Co1 O12 2.116(3) 2_566 ? Co1 O12 2.116(3) . ? Co1 O17 2.138(3) 2_566 ? Co1 O17 2.138(3) . ? Co2 O15 2.072(3) . ? Co2 O2 2.093(3) . ? Co2 O11 2.097(3) 1_655 ? Co2 O14 2.109(3) . ? Co2 O16 2.129(3) . ? Co2 O13 2.138(3) . ? N1 C2 1.343(5) . ? N1 C1 1.343(4) . ? N2 C1 1.348(5) . ? N2 C3 1.350(5) . ? N3 C3 1.337(4) . ? N3 C2 1.354(4) . ? N4 C3 1.366(4) . ? N4 C8 1.447(5) . ? N4 C4 1.460(4) . ? N5 C2 1.352(4) . ? N5 C7 1.449(5) . ? N5 C9 1.452(4) . ? N6 C1 1.363(4) . ? N6 C5 1.442(5) . ? N6 C6 1.452(4) . ? O1 C10 1.244(5) . ? O2 C10 1.267(4) . ? O2WA O2WB 1.490(13) . ? O3 C11 1.220(5) . ? O4 C14 1.251(5) . ? O5 C13 1.264(4) . ? O6 C12 1.222(4) . ? O7 C13 1.248(4) . ? O8 C11 1.301(5) . ? O9 C12 1.314(4) . ? O10 C14 1.271(4) . ? O11 C15 1.258(4) . ? O11 Co2 2.097(3) 1_455 ? O12 C15 1.250(4) . ? C4 C13 1.512(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C14 1.520(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C11 1.511(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C10 1.545(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C12 1.514(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C15 1.537(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? 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 O18 Co1 O18 180 . 2_566 ? O18 Co1 O12 88.82(11) . 2_566 ? O18 Co1 O12 91.18(11) 2_566 2_566 ? O18 Co1 O12 91.18(11) . . ? O18 Co1 O12 88.82(11) 2_566 . ? O12 Co1 O12 180 2_566 . ? O18 Co1 O17 91.49(12) . 2_566 ? O18 Co1 O17 88.51(12) 2_566 2_566 ? O12 Co1 O17 97.47(10) 2_566 2_566 ? O12 Co1 O17 82.53(10) . 2_566 ? O18 Co1 O17 88.51(12) . . ? O18 Co1 O17 91.49(12) 2_566 . ? O12 Co1 O17 82.53(10) 2_566 . ? O12 Co1 O17 97.47(10) . . ? O17 Co1 O17 180 2_566 . ? O15 Co2 O2 86.07(11) . . ? O15 Co2 O11 90.43(12) . 1_655 ? O2 Co2 O11 176.46(11) . 1_655 ? O15 Co2 O14 90.37(11) . . ? O2 Co2 O14 92.40(11) . . ? O11 Co2 O14 87.15(11) 1_655 . ? O15 Co2 O16 88.03(13) . . ? O2 Co2 O16 91.20(12) . . ? O11 Co2 O16 89.15(12) 1_655 . ? O14 Co2 O16 175.96(12) . . ? O15 Co2 O13 174.55(11) . . ? O2 Co2 O13 89.28(10) . . ? O11 Co2 O13 94.25(10) 1_655 . ? O14 Co2 O13 92.66(10) . . ? O16 Co2 O13 89.24(12) . . ? C2 N1 C1 114.4(3) . . ? C1 N2 C3 112.7(3) . . ? C3 N3 C2 114.2(3) . . ? C3 N4 C8 118.6(3) . . ? C3 N4 C4 120.8(3) . . ? C8 N4 C4 120.6(3) . . ? C2 N5 C7 120.2(3) . . ? C2 N5 C9 121.0(3) . . ? C7 N5 C9 117.0(3) . . ? C1 N6 C5 118.6(3) . . ? C1 N6 C6 119.3(3) . . ? C5 N6 C6 121.8(3) . . ? C10 O2 Co2 125.9(2) . . ? C15 O11 Co2 124.5(2) . 1_455 ? C15 O12 Co1 141.5(2) . . ? N1 C1 N2 126.6(3) . . ? N1 C1 N6 116.3(3) . . ? N2 C1 N6 117.1(3) . . ? N1 C2 N5 118.3(3) . . ? N1 C2 N3 125.0(3) . . ? N5 C2 N3 116.7(3) . . ? N3 C3 N2 126.8(3) . . ? N3 C3 N4 115.5(3) . . ? N2 C3 N4 117.7(3) . . ? N4 C4 C13 114.4(3) . . ? N4 C4 H4A 108.7 . . ? C13 C4 H4A 108.7 . . ? N4 C4 H4B 108.7 . . ? C13 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? N6 C5 C14 113.4(3) . . ? N6 C5 H5A 108.9 . . ? C14 C5 H5A 108.9 . . ? N6 C5 H5B 108.9 . . ? C14 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N6 C6 C11 114.5(3) . . ? N6 C6 H6A 108.6 . . ? C11 C6 H6A 108.6 . . ? N6 C6 H6B 108.6 . . ? C11 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? N5 C7 C10 112.2(3) . . ? N5 C7 H7A 109.2 . . ? C10 C7 H7A 109.2 . . ? N5 C7 H7B 109.2 . . ? C10 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? N4 C8 C12 113.2(3) . . ? N4 C8 H8A 108.9 . . ? C12 C8 H8A 108.9 . . ? N4 C8 H8B 108.9 . . ? C12 C8 H8B 108.9 . . ? H8A C8 H8B 107.8 . . ? N5 C9 C15 115.2(3) . . ? N5 C9 H9A 108.5 . . ? C15 C9 H9A 108.5 . . ? N5 C9 H9B 108.5 . . ? C15 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? O1 C10 O2 125.6(3) . . ? O1 C10 C7 118.6(3) . . ? O2 C10 C7 115.7(3) . . ? O3 C11 O8 119.8(3) . . ? O3 C11 C6 120.4(4) . . ? O8 C11 C6 119.7(3) . . ? O6 C12 O9 120.9(3) . . ? O6 C12 C8 121.8(3) . . ? O9 C12 C8 117.3(3) . . ? O7 C13 O5 124.3(4) . . ? O7 C13 C4 120.5(3) . . ? O5 C13 C4 115.2(3) . . ? O4 C14 O10 122.9(3) . . ? O4 C14 C5 119.0(3) . . ? O10 C14 C5 118.0(3) . . ? O12 C15 O11 124.2(3) . . ? O12 C15 C9 117.1(3) . . ? O11 C15 C9 118.6(3) . . ? 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 O15 Co2 O2 C10 155.2(3) . . . . ? O11 Co2 O2 C10 147.5(16) 1_655 . . . ? O14 Co2 O2 C10 65.0(3) . . . . ? O16 Co2 O2 C10 -116.9(3) . . . . ? O13 Co2 O2 C10 -27.7(3) . . . . ? O18 Co1 O12 C15 140.5(4) . . . . ? O18 Co1 O12 C15 -39.5(4) 2_566 . . . ? O12 Co1 O12 C15 73(100) 2_566 . . . ? O17 Co1 O12 C15 -128.1(4) 2_566 . . . ? O17 Co1 O12 C15 51.9(4) . . . . ? C2 N1 C1 N2 -4.3(5) . . . . ? C2 N1 C1 N6 176.4(3) . . . . ? C3 N2 C1 N1 3.8(5) . . . . ? C3 N2 C1 N6 -176.9(3) . . . . ? C5 N6 C1 N1 3.3(5) . . . . ? C6 N6 C1 N1 177.1(3) . . . . ? C5 N6 C1 N2 -176.0(3) . . . . ? C6 N6 C1 N2 -2.3(5) . . . . ? C1 N1 C2 N5 178.5(3) . . . . ? C1 N1 C2 N3 0.3(5) . . . . ? C7 N5 C2 N1 169.1(3) . . . . ? C9 N5 C2 N1 4.6(5) . . . . ? C7 N5 C2 N3 -12.5(5) . . . . ? C9 N5 C2 N3 -177.0(3) . . . . ? C3 N3 C2 N1 3.5(5) . . . . ? C3 N3 C2 N5 -174.8(3) . . . . ? C2 N3 C3 N2 -4.0(5) . . . . ? C2 N3 C3 N4 175.2(3) . . . . ? C1 N2 C3 N3 0.7(5) . . . . ? C1 N2 C3 N4 -178.5(3) . . . . ? C8 N4 C3 N3 4.8(5) . . . . ? C4 N4 C3 N3 -178.0(3) . . . . ? C8 N4 C3 N2 -175.9(3) . . . . ? C4 N4 C3 N2 1.3(5) . . . . ? C3 N4 C4 C13 -90.4(4) . . . . ? C8 N4 C4 C13 86.8(4) . . . . ? C1 N6 C5 C14 64.3(4) . . . . ? C6 N6 C5 C14 -109.3(4) . . . . ? C1 N6 C6 C11 -77.6(4) . . . . ? C5 N6 C6 C11 95.9(4) . . . . ? C2 N5 C7 C10 -83.5(4) . . . . ? C9 N5 C7 C10 81.6(4) . . . . ? C3 N4 C8 C12 60.4(4) . . . . ? C4 N4 C8 C12 -116.8(3) . . . . ? C2 N5 C9 C15 -95.4(4) . . . . ? C7 N5 C9 C15 99.6(4) . . . . ? Co2 O2 C10 O1 12.2(6) . . . . ? Co2 O2 C10 C7 -167.9(2) . . . . ? N5 C7 C10 O1 2.4(5) . . . . ? N5 C7 C10 O2 -177.5(3) . . . . ? N6 C6 C11 O3 160.2(4) . . . . ? N6 C6 C11 O8 -21.0(5) . . . . ? N4 C8 C12 O6 -145.8(3) . . . . ? N4 C8 C12 O9 36.7(4) . . . . ? N4 C4 C13 O7 -13.4(5) . . . . ? N4 C4 C13 O5 168.9(3) . . . . ? N6 C5 C14 O4 -151.5(3) . . . . ? N6 C5 C14 O10 31.4(5) . . . . ? Co1 O12 C15 O11 154.1(3) . . . . ? Co1 O12 C15 C9 -25.4(5) . . . . ? Co2 O11 C15 O12 -23.2(5) 1_455 . . . ? Co2 O11 C15 C9 156.3(2) 1_455 . . . ? N5 C9 C15 O12 -170.8(3) . . . . ? N5 C9 C15 O11 9.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.211 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.145 # Attachment 'complex-2.CIF' data_complex-2 #TrackingRef 'complex-2.CIF' _database_code_depnum_ccdc_archive 'CCDC 769621' #TrackingRef '- complex 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H59 Cu4 N12 Na O40' _chemical_formula_weight 1505.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 20.063(8) _cell_length_b 12.640(5) _cell_length_c 21.168(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.742(7) _cell_angle_gamma 90.00 _cell_volume 5368(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7859 _cell_measurement_theta_min 2.0303 _cell_measurement_theta_max 27.4855 _exptl_crystal_description rhombus _exptl_crystal_colour green _exptl_crystal_size_max 0.1200 _exptl_crystal_size_mid 0.1200 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.862 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3080 _exptl_absorpt_coefficient_mu 1.696 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7082 _exptl_absorpt_correction_T_max 1.0000 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22672 _diffrn_reflns_av_R_equivalents 0.1011 _diffrn_reflns_av_sigmaI/netI 0.1086 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9044 _reflns_number_gt 7327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. O17 and C26 are non-positive definite, the following restraint was applied: ISOR 0.01 O17 C26 ; _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^)+(0.1060P)^2^+92.7130P] 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_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.12(3) _refine_ls_number_reflns 9044 _refine_ls_number_parameters 784 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1173 _refine_ls_R_factor_gt 0.1000 _refine_ls_wR_factor_ref 0.2497 _refine_ls_wR_factor_gt 0.2311 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.003 _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 0.11116(9) 0.40102(14) 0.05328(9) 0.0353(4) Uani 1 1 d . . . Cu2 Cu -0.15971(8) 0.33120(12) 0.18315(7) 0.0255(4) Uani 1 1 d . . . Cu3 Cu 0.30974(8) 0.68782(12) -0.02288(7) 0.0260(4) Uani 1 1 d . . . Cu4 Cu 0.04544(9) 0.61370(14) 0.12455(8) 0.0326(4) Uani 1 1 d . . . Na1 Na -0.0630(5) 0.6510(7) -0.1979(4) 0.084(3) Uani 1 1 d . . . C1 C 0.2238(7) 0.2582(9) 0.0836(6) 0.027(3) Uani 1 1 d . . . C2 C 0.1827(6) 0.1136(8) 0.1269(6) 0.019(2) Uani 1 1 d . . . C3 C 0.2050(7) 0.1162(10) 0.0231(6) 0.024(3) Uani 1 1 d . . . C4 C 0.2434(8) 0.4155(10) 0.1475(7) 0.031(3) Uani 1 1 d . . . H4A H 0.2841 0.4569 0.1496 0.037 Uiso 1 1 calc R . . H4B H 0.2463 0.3623 0.1805 0.037 Uiso 1 1 calc R . . C5 C 0.1850(10) 0.4886(13) 0.1623(7) 0.045(4) Uani 1 1 d . . . C6 C 0.2757(8) 0.4108(10) 0.0339(7) 0.035(3) Uani 1 1 d . . . H6A H 0.2944 0.3552 0.0080 0.043 Uiso 1 1 calc R . . H6B H 0.3123 0.4539 0.0496 0.043 Uiso 1 1 calc R . . C7 C 0.2295(8) 0.4803(12) -0.0078(7) 0.039(4) Uani 1 1 d . . . C8 C 0.1556(8) 0.1113(12) 0.2409(7) 0.033(3) Uani 1 1 d . . . H8A H 0.1306 0.0663 0.2692 0.039 Uiso 1 1 calc R . . H8B H 0.1312 0.1772 0.2363 0.039 Uiso 1 1 calc R . . C9 C 0.2236(9) 0.1352(13) 0.2716(7) 0.041(4) Uani 1 1 d . . . C10 C 0.1450(7) -0.0511(8) 0.1707(7) 0.027(3) Uani 1 1 d . . . H10A H 0.1129 -0.0587 0.1363 0.033 Uiso 1 1 calc R . . H10B H 0.1247 -0.0788 0.2086 0.033 Uiso 1 1 calc R . . C11 C 0.2040(7) -0.1150(10) 0.1564(6) 0.025(3) Uani 1 1 d . . . C12 C 0.2294(9) 0.1145(10) -0.0888(7) 0.039(4) Uani 1 1 d . . . H12A H 0.2670 0.0750 -0.1048 0.046 Uiso 1 1 calc R . . H12B H 0.2449 0.1848 -0.0776 0.046 Uiso 1 1 calc R . . C13 C 0.1772(7) 0.1230(11) -0.1394(6) 0.030(3) Uani 1 1 d . . . C14 C 0.1873(7) -0.0468(10) -0.0349(6) 0.028(3) Uani 1 1 d . . . H14A H 0.1688 -0.0624 -0.0764 0.034 Uiso 1 1 calc R . . H14B H 0.1528 -0.0604 -0.0043 0.034 Uiso 1 1 calc R . . C15 C 0.2433(7) -0.1192(10) -0.0224(6) 0.024(3) Uani 1 1 d . . . C16 C -0.0677(7) 0.7614(9) 0.0892(7) 0.025(3) Uani 1 1 d . . . C17 C -0.0508(6) 0.9073(8) 0.1465(6) 0.019(2) Uani 1 1 d . . . C18 C -0.0271(7) 0.9082(9) 0.0435(5) 0.020(2) Uani 1 1 d . . . C19 C -0.1137(7) 0.6038(10) 0.1381(7) 0.034(3) Uani 1 1 d . . . H19A H -0.1505 0.5629 0.1208 0.041 Uiso 1 1 calc R . . H19B H -0.1327 0.6588 0.1642 0.041 Uiso 1 1 calc R . . C20 C -0.0723(8) 0.5302(10) 0.1816(6) 0.028(3) Uani 1 1 d . . . C21 C -0.0843(8) 0.6006(10) 0.0259(7) 0.032(3) Uani 1 1 d . . . H21A H -0.0847 0.6531 -0.0075 0.038 Uiso 1 1 calc R . . H21B H -0.1261 0.5622 0.0234 0.038 Uiso 1 1 calc R . . C22 C -0.0289(7) 0.5256(12) 0.0149(6) 0.032(3) Uani 1 1 d . . . C23 C -0.0773(7) 0.9083(11) 0.2588(5) 0.027(3) Uani 1 1 d . . . H23A H -0.1019 0.8453 0.2467 0.033 Uiso 1 1 calc R . . H23B H -0.1085 0.9562 0.2784 0.033 Uiso 1 1 calc R . . C24 C -0.0283(9) 0.8782(13) 0.3059(6) 0.039(4) Uani 1 1 d . . . C25 C -0.0358(8) 1.0712(9) 0.2068(6) 0.028(3) Uani 1 1 d . . . H25A H 0.0023 1.0846 0.1802 0.033 Uiso 1 1 calc R . . H25B H -0.0226 1.0867 0.2501 0.033 Uiso 1 1 calc R . . C26 C -0.0929(7) 1.1463(10) 0.1871(6) 0.026(3) Uani 1 1 d U . . C27 C 0.0015(9) 0.9027(11) -0.0678(7) 0.040(4) Uani 1 1 d . . . H27A H 0.0291 0.9458 -0.0950 0.048 Uiso 1 1 calc R . . H27B H 0.0255 0.8373 -0.0598 0.048 Uiso 1 1 calc R . . C28 C -0.0591(10) 0.8776(11) -0.1018(8) 0.039(4) Uani 1 1 d . . . C29 C 0.0111(7) 1.0718(10) -0.0018(6) 0.028(3) Uani 1 1 d . . . H29A H 0.0302 1.0955 -0.0412 0.034 Uiso 1 1 calc R . . H29B H 0.0440 1.0822 0.0316 0.034 Uiso 1 1 calc R . . C30 C -0.0535(7) 1.1380(10) 0.0127(6) 0.023(3) Uani 1 1 d . . . N1 N 0.2039(7) 0.2110(8) 0.1370(6) 0.036(3) Uani 1 1 d . . . N2 N 0.2228(6) 0.2154(7) 0.0262(5) 0.027(2) Uani 1 1 d . . . N3 N 0.1816(6) 0.0578(8) 0.0738(5) 0.027(2) Uani 1 1 d . . . N4 N 0.2414(7) 0.3623(9) 0.0880(7) 0.038(3) Uani 1 1 d . . . N5 N 0.2042(7) 0.0619(9) -0.0324(5) 0.032(3) Uani 1 1 d . . . N6 N 0.1588(6) 0.0604(8) 0.1799(5) 0.025(2) Uani 1 1 d . . . N7 N -0.0716(7) 0.8067(8) 0.1458(5) 0.030(3) Uani 1 1 d . . . N8 N -0.0484(5) 0.8047(8) 0.0361(5) 0.023(2) Uani 1 1 d . . . N9 N -0.0279(7) 0.9609(9) 0.0974(6) 0.033(3) Uani 1 1 d . . . N10 N -0.0805(7) 0.6545(8) 0.0862(5) 0.026(2) Uani 1 1 d . . . N11 N -0.0540(6) 0.9576(9) 0.2020(5) 0.027(2) Uani 1 1 d . . . N12 N -0.0063(6) 0.9594(8) -0.0064(5) 0.025(2) Uani 1 1 d . . . O1 O 0.1923(6) 0.5498(11) 0.2067(6) 0.059(4) Uani 1 1 d . . . O1W O 0.1137(7) 0.6709(11) -0.0472(6) 0.058(3) Uani 1 1 d . . . O2 O 0.1334(6) 0.4824(9) 0.1275(6) 0.047(3) Uani 1 1 d . . . O2W O 0.0232(12) 0.6398(15) 0.3153(8) 0.121(9) Uani 1 1 d . . . O3 O 0.1686(7) 0.4830(9) -0.0009(6) 0.050(3) Uani 1 1 d . . . O3W O 0.1472(12) 0.3662(17) -0.1306(9) 0.109(7) Uani 1 1 d . . . O4 O 0.2586(5) 0.5342(8) -0.0500(5) 0.036(2) Uani 1 1 d . . . O4W O -0.2145(9) 0.0920(12) 0.3034(8) 0.093(6) Uani 1 1 d . . . O5 O 0.2256(9) 0.2021(13) 0.3132(7) 0.081(5) Uani 1 1 d . . . O5W O 0.1697(18) 0.591(2) -0.1735(16) 0.201(15) Uani 1 1 d . . . O6 O 0.2737(6) 0.0749(9) 0.2592(6) 0.046(3) Uani 1 1 d . . . O7 O 0.2618(5) -0.0804(7) 0.1752(4) 0.0249(19) Uani 1 1 d . . . O8 O 0.1985(6) -0.1993(8) 0.1246(5) 0.039(3) Uani 1 1 d . . . O9 O 0.1145(6) 0.1136(10) -0.1238(5) 0.050(3) Uani 1 1 d . . . O10 O 0.1925(6) 0.1397(11) -0.1940(5) 0.050(3) Uani 1 1 d . . . O11 O 0.2974(6) -0.0852(8) -0.0013(5) 0.044(3) Uani 1 1 d . . . O12 O 0.2342(5) -0.2197(7) -0.0339(5) 0.031(2) Uani 1 1 d . . . O13 O -0.1006(6) 0.4714(8) 0.2194(5) 0.039(3) Uani 1 1 d . . . O14 O -0.0087(6) 0.5293(9) 0.1777(5) 0.041(3) Uani 1 1 d . . . O15 O 0.0258(6) 0.5273(8) 0.0499(6) 0.042(3) Uani 1 1 d . . . O16 O -0.0315(7) 0.4610(10) -0.0298(6) 0.052(3) Uani 1 1 d . . . O17 O 0.0311(5) 0.9060(9) 0.2941(5) 0.042(3) Uani 1 1 d U . . O18 O -0.0441(6) 0.8262(10) 0.3517(5) 0.051(3) Uani 1 1 d . . . O19 O -0.1428(6) 1.1103(8) 0.1615(5) 0.037(2) Uani 1 1 d . . . O20 O -0.0803(6) 1.2428(7) 0.1986(5) 0.036(2) Uani 1 1 d . . . O21 O -0.0629(8) 0.8076(10) -0.1413(6) 0.060(4) Uani 1 1 d . . . O22 O -0.1134(6) 0.9357(9) -0.0907(5) 0.044(3) Uani 1 1 d . . . O23 O -0.0465(5) 1.2209(7) 0.0434(5) 0.029(2) Uani 1 1 d . . . O24 O -0.1068(5) 1.1046(7) -0.0130(4) 0.030(2) Uani 1 1 d . . . O25 O 0.0640(6) 0.2972(9) 0.1042(6) 0.050(3) Uani 1 1 d . . . O26 O 0.0747(8) 0.3283(9) -0.0226(6) 0.061(4) Uani 1 1 d . . . O27 O -0.1294(5) 0.3587(7) 0.0966(5) 0.030(2) Uani 1 1 d . . . O28 O -0.1872(6) 0.2962(9) 0.2720(5) 0.044(3) Uani 1 1 d . . . O29 O 0.3365(7) 0.7235(10) -0.1095(5) 0.052(3) Uani 1 1 d . . . O30 O 0.2815(6) 0.6640(7) 0.0655(5) 0.034(2) Uani 1 1 d . . . O31 O 0.0894(7) 0.7225(9) 0.0751(5) 0.050(3) Uani 1 1 d . . . O32 O 0.0843(6) 0.6828(9) 0.2011(5) 0.044(3) Uani 1 1 d . . . O33 O -0.1117(13) 0.4974(17) -0.1404(8) 0.129(8) Uani 1 1 d . . . O34 O 0.0504(12) 0.6472(18) -0.2716(12) 0.134(9) Uani 1 1 d . . . O35 O 0.0307(17) 0.586(3) -0.1493(18) 0.213(17) 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 0.0247(10) 0.0355(9) 0.0458(10) -0.0059(8) 0.0010(8) -0.0042(7) Cu2 0.0211(8) 0.0253(7) 0.0302(7) -0.0014(6) 0.0006(6) -0.0004(6) Cu3 0.0247(9) 0.0256(7) 0.0277(7) 0.0008(6) 0.0034(7) 0.0034(6) Cu4 0.0243(9) 0.0367(9) 0.0369(9) -0.0055(7) 0.0033(7) -0.0063(7) Na1 0.105(7) 0.064(5) 0.081(6) -0.042(4) -0.052(6) 0.030(5) C1 0.035(8) 0.019(5) 0.026(6) 0.001(5) 0.011(6) 0.013(5) C2 0.016(6) 0.015(5) 0.027(6) 0.013(4) 0.004(5) 0.002(4) C3 0.017(6) 0.029(6) 0.025(6) 0.005(5) -0.004(5) -0.002(5) C4 0.025(7) 0.029(6) 0.040(7) -0.006(6) 0.004(6) -0.007(6) C5 0.049(11) 0.044(8) 0.042(8) -0.024(7) 0.017(8) 0.016(8) C6 0.040(9) 0.018(6) 0.048(8) 0.018(6) -0.002(7) -0.004(6) C7 0.034(9) 0.044(8) 0.040(8) -0.010(7) 0.018(7) 0.004(7) C8 0.022(8) 0.047(8) 0.029(7) 0.005(6) 0.006(6) 0.013(6) C9 0.034(9) 0.054(9) 0.034(7) -0.026(7) -0.002(7) 0.003(7) C10 0.035(8) 0.009(5) 0.038(7) 0.006(5) 0.008(6) 0.001(5) C11 0.025(7) 0.027(6) 0.021(6) 0.005(5) -0.006(5) -0.005(5) C12 0.054(11) 0.018(6) 0.044(8) -0.008(6) -0.001(8) 0.010(6) C13 0.018(7) 0.045(8) 0.026(6) -0.004(6) 0.009(5) -0.009(6) C14 0.022(7) 0.031(6) 0.031(6) -0.003(5) -0.017(6) 0.010(5) C15 0.017(6) 0.030(6) 0.025(6) -0.002(5) 0.005(5) 0.003(5) C16 0.023(7) 0.011(5) 0.042(7) -0.001(5) -0.004(6) 0.005(4) C17 0.015(6) 0.016(5) 0.025(6) 0.009(4) 0.004(5) -0.001(4) C18 0.018(6) 0.021(5) 0.022(5) 0.005(4) 0.001(5) 0.002(5) C19 0.024(7) 0.026(6) 0.053(8) -0.005(6) 0.032(7) -0.006(5) C20 0.031(8) 0.025(6) 0.029(6) -0.006(5) -0.011(6) -0.005(6) C21 0.039(9) 0.023(6) 0.033(7) -0.006(5) 0.007(6) 0.000(6) C22 0.024(8) 0.043(7) 0.028(6) -0.006(6) 0.004(6) -0.009(6) C23 0.028(7) 0.042(7) 0.012(5) -0.006(5) 0.003(5) -0.017(6) C24 0.045(10) 0.056(9) 0.016(6) 0.004(6) 0.005(6) 0.015(8) C25 0.035(8) 0.020(5) 0.028(6) -0.009(5) 0.009(6) 0.000(5) C26 0.024(6) 0.034(6) 0.021(5) -0.001(5) 0.011(5) 0.008(5) C27 0.059(12) 0.025(7) 0.038(8) -0.017(6) 0.017(8) 0.008(7) C28 0.048(10) 0.031(7) 0.038(8) -0.005(6) 0.010(7) 0.005(7) C29 0.024(7) 0.029(6) 0.031(6) 0.007(5) -0.006(6) -0.007(5) C30 0.029(7) 0.022(5) 0.019(5) -0.004(5) 0.008(5) -0.001(5) N1 0.047(9) 0.022(5) 0.039(6) 0.002(5) -0.010(6) 0.002(5) N2 0.039(7) 0.015(4) 0.027(5) 0.002(4) 0.016(5) 0.002(5) N3 0.028(7) 0.025(5) 0.027(5) -0.004(4) -0.001(5) 0.003(5) N4 0.041(8) 0.020(5) 0.052(8) -0.005(5) -0.001(7) 0.000(5) N5 0.054(9) 0.031(6) 0.013(5) 0.006(4) 0.007(5) -0.006(6) N6 0.027(6) 0.026(5) 0.023(5) -0.007(4) -0.003(5) 0.001(4) N7 0.039(8) 0.018(5) 0.035(6) 0.004(4) 0.000(5) -0.002(5) N8 0.016(5) 0.017(4) 0.037(6) 0.001(4) 0.013(5) 0.000(4) N9 0.033(7) 0.032(6) 0.032(6) 0.004(5) -0.008(5) -0.007(5) N10 0.037(7) 0.019(5) 0.023(5) -0.002(4) 0.007(5) -0.002(5) N11 0.028(7) 0.032(6) 0.022(5) -0.003(4) -0.008(5) -0.007(5) N12 0.036(7) 0.018(5) 0.021(5) -0.009(4) 0.007(5) -0.003(4) O1 0.026(7) 0.090(9) 0.061(8) -0.043(7) 0.003(6) 0.005(6) O1W 0.040(7) 0.078(8) 0.055(7) 0.012(6) 0.011(6) -0.017(6) O2 0.025(6) 0.053(7) 0.064(7) -0.016(6) 0.007(6) -0.007(5) O2W 0.19(2) 0.082(11) 0.099(13) 0.003(9) 0.103(15) 0.004(13) O3 0.044(8) 0.040(6) 0.066(8) 0.014(5) 0.020(6) -0.001(5) O3W 0.111(18) 0.110(14) 0.106(14) -0.012(11) 0.019(14) -0.009(13) O4 0.021(5) 0.045(5) 0.042(5) -0.003(4) 0.012(5) -0.013(4) O4W 0.109(14) 0.068(9) 0.100(12) 0.027(9) -0.063(11) -0.031(9) O5 0.079(12) 0.096(11) 0.067(9) -0.060(8) -0.025(8) 0.038(9) O5W 0.21(3) 0.16(2) 0.24(3) -0.06(2) 0.09(3) -0.06(2) O6 0.027(6) 0.050(6) 0.062(7) -0.014(6) -0.003(6) -0.008(5) O7 0.016(5) 0.032(4) 0.027(4) -0.005(4) 0.001(4) -0.001(4) O8 0.041(7) 0.036(5) 0.041(6) -0.009(4) 0.011(5) -0.006(5) O9 0.037(7) 0.079(8) 0.033(5) 0.022(5) 0.013(5) 0.023(6) O10 0.039(7) 0.087(8) 0.025(5) -0.006(5) 0.006(5) -0.013(6) O11 0.039(7) 0.044(6) 0.050(6) 0.013(5) -0.010(5) -0.009(5) O12 0.032(6) 0.026(4) 0.036(5) 0.004(4) 0.009(4) -0.005(4) O13 0.044(7) 0.035(5) 0.037(5) -0.004(4) -0.001(5) -0.007(5) O14 0.022(6) 0.052(6) 0.049(6) 0.017(5) -0.008(5) 0.000(5) O15 0.024(6) 0.040(5) 0.061(7) -0.012(5) -0.014(5) 0.004(5) O16 0.054(8) 0.056(7) 0.046(6) -0.032(6) 0.008(6) 0.004(6) O17 0.016(5) 0.064(6) 0.047(5) 0.014(5) 0.002(4) -0.006(4) O18 0.041(7) 0.084(9) 0.029(5) 0.029(5) 0.011(5) 0.005(6) O19 0.025(5) 0.038(5) 0.048(6) 0.010(4) -0.011(5) 0.005(4) O20 0.039(7) 0.024(4) 0.046(6) -0.002(4) 0.000(5) 0.003(4) O21 0.065(10) 0.053(7) 0.061(8) -0.031(6) 0.000(7) 0.012(6) O22 0.031(6) 0.052(6) 0.047(6) -0.015(5) -0.008(5) 0.010(5) O23 0.013(5) 0.031(5) 0.044(5) -0.016(4) 0.007(4) 0.004(4) O24 0.028(6) 0.028(4) 0.034(5) -0.008(4) 0.007(4) -0.002(4) O25 0.031(6) 0.049(6) 0.070(8) 0.001(6) -0.004(6) -0.012(5) O26 0.081(11) 0.049(7) 0.053(7) -0.030(6) 0.009(7) -0.010(7) O27 0.024(5) 0.022(4) 0.043(5) 0.000(4) 0.014(4) -0.001(4) O28 0.043(7) 0.051(6) 0.037(5) 0.019(5) 0.008(5) 0.004(5) O29 0.047(8) 0.068(8) 0.041(6) 0.012(6) 0.005(6) 0.016(6) O30 0.046(7) 0.021(4) 0.035(5) 0.000(4) 0.003(5) 0.001(4) O31 0.058(9) 0.049(6) 0.043(6) 0.000(5) 0.002(6) -0.018(6) O32 0.034(6) 0.051(6) 0.048(6) -0.024(5) 0.006(5) 0.000(5) O33 0.19(3) 0.126(16) 0.067(10) 0.008(10) -0.045(14) 0.013(16) O34 0.109(19) 0.125(16) 0.17(2) -0.076(16) -0.013(16) -0.014(14) O35 0.18(3) 0.20(3) 0.26(4) -0.02(3) -0.09(3) 0.06(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O2 1.926(12) . ? Cu1 O3 1.936(12) . ? Cu1 O25 1.950(12) . ? Cu1 O26 1.982(12) . ? Cu1 O15 2.342(11) . ? Cu2 O7 1.937(9) 3_455 ? Cu2 O27 1.968(10) . ? Cu2 O20 1.970(11) 1_545 ? Cu2 O28 2.016(10) . ? Cu2 O13 2.261(10) . ? Cu2 Na1 3.167(8) 2_565 ? Cu3 O12 1.925(10) 1_565 ? Cu3 O29 1.970(12) . ? Cu3 O30 1.984(10) . ? Cu3 O24 1.987(10) 3_545 ? Cu3 O4 2.267(10) . ? Cu4 O14 1.901(11) . ? Cu4 O31 1.947(12) . ? Cu4 O15 1.957(10) . ? Cu4 O32 1.991(11) . ? Cu4 O2 2.423(12) . ? Na1 O35 2.28(3) . ? Na1 O21 2.314(13) . ? Na1 O13 2.448(13) 2_564 ? Na1 O33 2.50(2) . ? Na1 O20 2.588(14) 2_574 ? Na1 O28 2.650(15) 2_564 ? Na1 O34 2.78(3) . ? Na1 Cu2 3.167(8) 2_564 ? C1 N2 1.330(16) . ? C1 N1 1.343(18) . ? C1 N4 1.365(16) . ? C2 N1 1.319(16) . ? C2 N3 1.328(16) . ? C2 N6 1.397(16) . ? C3 N2 1.306(15) . ? C3 N5 1.361(16) . ? C3 N3 1.388(17) . ? C4 N4 1.428(18) . ? C4 C5 1.53(2) . ? C5 O1 1.224(18) . ? C5 O2 1.27(2) . ? C6 N4 1.48(2) . ? C6 C7 1.55(2) . ? C7 O3 1.23(2) . ? C7 O4 1.271(18) . ? C8 N6 1.445(17) . ? C8 C9 1.53(2) . ? C9 O5 1.221(18) . ? C9 O6 1.29(2) . ? C10 N6 1.450(15) . ? C10 C11 1.47(2) . ? C11 O8 1.265(16) . ? C11 O7 1.297(16) . ? C12 N5 1.463(19) . ? C12 C13 1.49(2) . ? C13 O10 1.219(17) . ? C13 O9 1.310(19) . ? C14 N5 1.415(17) . ? C14 C15 1.471(17) . ? C15 O11 1.244(17) . ? C15 O12 1.306(15) . ? C16 N8 1.314(17) . ? C16 N7 1.331(18) . ? C16 N10 1.376(15) . ? C17 N9 1.328(16) . ? C17 N7 1.338(15) . ? C17 N11 1.339(16) . ? C18 N12 1.310(16) . ? C18 N9 1.321(16) . ? C18 N8 1.384(15) . ? C19 N10 1.442(17) . ? C19 C20 1.54(2) . ? C20 O13 1.236(18) . ? C20 O14 1.279(19) . ? C21 N10 1.448(17) . ? C21 C22 1.48(2) . ? C22 O16 1.252(17) . ? C22 O15 1.316(17) . ? C23 N11 1.437(16) . ? C23 C24 1.44(2) . ? C24 O18 1.215(18) . ? C24 O17 1.27(2) . ? C25 N11 1.484(16) . ? C25 C26 1.541(19) . ? C26 O19 1.219(17) . ? C26 O20 1.270(16) . ? C27 C28 1.44(3) . ? C27 N12 1.496(16) . ? C28 O21 1.219(18) . ? C28 O22 1.34(2) . ? C29 N12 1.466(15) . ? C29 C30 1.577(19) . ? C30 O23 1.240(15) . ? C30 O24 1.266(17) . ? O7 Cu2 1.937(9) 3_545 ? O12 Cu3 1.925(10) 1_545 ? O13 Na1 2.448(13) 2_565 ? O20 Cu2 1.970(11) 1_565 ? O20 Na1 2.588(14) 2_575 ? O24 Cu3 1.987(10) 3_455 ? O28 Na1 2.650(15) 2_565 ? 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 O2 Cu1 O3 93.6(5) . . ? O2 Cu1 O25 91.0(5) . . ? O3 Cu1 O25 169.7(5) . . ? O2 Cu1 O26 171.2(6) . . ? O3 Cu1 O26 89.1(6) . . ? O25 Cu1 O26 87.7(5) . . ? O2 Cu1 O15 79.8(4) . . ? O3 Cu1 O15 93.3(5) . . ? O25 Cu1 O15 96.6(5) . . ? O26 Cu1 O15 91.7(5) . . ? O7 Cu2 O27 94.4(4) 3_455 . ? O7 Cu2 O20 175.4(4) 3_455 1_545 ? O27 Cu2 O20 89.8(4) . 1_545 ? O7 Cu2 O28 88.6(4) 3_455 . ? O27 Cu2 O28 176.8(4) . . ? O20 Cu2 O28 87.2(5) 1_545 . ? O7 Cu2 O13 90.0(4) 3_455 . ? O27 Cu2 O13 90.6(4) . . ? O20 Cu2 O13 88.2(4) 1_545 . ? O28 Cu2 O13 90.2(4) . . ? O7 Cu2 Na1 121.2(3) 3_455 2_565 ? O27 Cu2 Na1 122.3(4) . 2_565 ? O20 Cu2 Na1 54.7(4) 1_545 2_565 ? O28 Cu2 Na1 56.4(4) . 2_565 ? O13 Cu2 Na1 50.3(3) . 2_565 ? O12 Cu3 O29 88.4(5) 1_565 . ? O12 Cu3 O30 88.4(4) 1_565 . ? O29 Cu3 O30 175.5(5) . . ? O12 Cu3 O24 174.4(4) 1_565 3_545 ? O29 Cu3 O24 88.8(5) . 3_545 ? O30 Cu3 O24 94.1(4) . 3_545 ? O12 Cu3 O4 97.9(4) 1_565 . ? O29 Cu3 O4 95.1(5) . . ? O30 Cu3 O4 88.6(4) . . ? O24 Cu3 O4 87.2(4) 3_545 . ? O14 Cu4 O31 168.8(5) . . ? O14 Cu4 O15 93.1(5) . . ? O31 Cu4 O15 92.7(5) . . ? O14 Cu4 O32 89.2(5) . . ? O31 Cu4 O32 87.3(5) . . ? O15 Cu4 O32 167.1(5) . . ? O14 Cu4 O2 91.3(5) . . ? O31 Cu4 O2 99.4(5) . . ? O15 Cu4 O2 77.2(4) . . ? O32 Cu4 O2 90.1(4) . . ? O35 Na1 O21 94.6(10) . . ? O35 Na1 O13 109.8(10) . 2_564 ? O21 Na1 O13 155.4(6) . 2_564 ? O35 Na1 O33 79.9(11) . . ? O21 Na1 O33 114.2(7) . . ? O13 Na1 O33 74.9(6) 2_564 . ? O35 Na1 O20 132.0(12) . 2_574 ? O21 Na1 O20 89.6(5) . 2_574 ? O13 Na1 O20 71.7(4) 2_564 2_574 ? O33 Na1 O20 140.1(6) . 2_574 ? O35 Na1 O28 164.8(12) . 2_564 ? O21 Na1 O28 84.5(5) . 2_564 ? O13 Na1 O28 73.0(4) 2_564 2_564 ? O33 Na1 O28 86.6(7) . 2_564 ? O20 Na1 O28 63.3(4) 2_574 2_564 ? O35 Na1 O34 64.6(12) . . ? O21 Na1 O34 108.1(7) . . ? O13 Na1 O34 80.5(5) 2_564 . ? O33 Na1 O34 126.1(8) . . ? O20 Na1 O34 68.6(7) 2_574 . ? O28 Na1 O34 130.1(7) 2_564 . ? O35 Na1 Cu2 151.1(10) . 2_564 ? O21 Na1 Cu2 110.3(5) . 2_564 ? O13 Na1 Cu2 45.3(3) 2_564 2_564 ? O33 Na1 Cu2 101.7(5) . 2_564 ? O20 Na1 Cu2 38.4(3) 2_574 2_564 ? O28 Na1 Cu2 39.3(2) 2_564 2_564 ? O34 Na1 Cu2 93.0(6) . 2_564 ? N2 C1 N1 126.0(12) . . ? N2 C1 N4 117.0(12) . . ? N1 C1 N4 116.8(12) . . ? N1 C2 N3 129.4(12) . . ? N1 C2 N6 115.6(11) . . ? N3 C2 N6 115.0(10) . . ? N2 C3 N5 121.9(11) . . ? N2 C3 N3 124.5(11) . . ? N5 C3 N3 113.5(10) . . ? N4 C4 C5 117.0(13) . . ? O1 C5 O2 125.1(15) . . ? O1 C5 C4 117.1(16) . . ? O2 C5 C4 117.8(12) . . ? N4 C6 C7 113.4(14) . . ? O3 C7 O4 122.3(16) . . ? O3 C7 C6 122.4(15) . . ? O4 C7 C6 115.3(14) . . ? N6 C8 C9 114.6(12) . . ? O5 C9 O6 122.4(16) . . ? O5 C9 C8 117.6(15) . . ? O6 C9 C8 119.3(12) . . ? N6 C10 C11 114.1(12) . . ? O8 C11 O7 121.3(14) . . ? O8 C11 C10 120.5(13) . . ? O7 C11 C10 118.1(11) . . ? N5 C12 C13 111.8(14) . . ? O10 C13 O9 120.6(14) . . ? O10 C13 C12 120.7(14) . . ? O9 C13 C12 118.7(13) . . ? N5 C14 C15 114.6(12) . . ? O11 C15 O12 121.5(13) . . ? O11 C15 C14 120.7(12) . . ? O12 C15 C14 117.8(12) . . ? N8 C16 N7 127.8(11) . . ? N8 C16 N10 115.2(12) . . ? N7 C16 N10 116.8(12) . . ? N9 C17 N7 126.0(12) . . ? N9 C17 N11 117.7(11) . . ? N7 C17 N11 116.3(11) . . ? N12 C18 N9 117.0(11) . . ? N12 C18 N8 118.5(11) . . ? N9 C18 N8 124.5(11) . . ? N10 C19 C20 118.2(12) . . ? O13 C20 O14 120.2(13) . . ? O13 C20 C19 120.0(14) . . ? O14 C20 C19 119.7(12) . . ? N10 C21 C22 114.1(13) . . ? O16 C22 O15 117.5(14) . . ? O16 C22 C21 120.8(14) . . ? O15 C22 C21 121.6(12) . . ? N11 C23 C24 117.8(13) . . ? O18 C24 O17 124.2(15) . . ? O18 C24 C23 120.7(17) . . ? O17 C24 C23 115.0(13) . . ? N11 C25 C26 113.4(12) . . ? O19 C26 O20 127.2(13) . . ? O19 C26 C25 119.6(12) . . ? O20 C26 C25 113.2(12) . . ? C28 C27 N12 116.2(14) . . ? O21 C28 O22 118.4(17) . . ? O21 C28 C27 123.1(16) . . ? O22 C28 C27 118.5(13) . . ? N12 C29 C30 109.3(11) . . ? O23 C30 O24 126.6(13) . . ? O23 C30 C29 117.6(12) . . ? O24 C30 C29 115.5(10) . . ? C2 N1 C1 112.1(11) . . ? C3 N2 C1 115.9(11) . . ? C2 N3 C3 111.7(10) . . ? C1 N4 C4 121.2(13) . . ? C1 N4 C6 118.1(12) . . ? C4 N4 C6 118.7(12) . . ? C3 N5 C14 121.5(11) . . ? C3 N5 C12 118.3(11) . . ? C14 N5 C12 119.7(11) . . ? C2 N6 C8 121.6(11) . . ? C2 N6 C10 115.2(10) . . ? C8 N6 C10 122.9(12) . . ? C16 N7 C17 113.3(11) . . ? C16 N8 C18 113.0(10) . . ? C18 N9 C17 115.3(11) . . ? C16 N10 C19 119.2(11) . . ? C16 N10 C21 120.7(11) . . ? C19 N10 C21 116.3(11) . . ? C17 N11 C23 123.2(10) . . ? C17 N11 C25 120.4(11) . . ? C23 N11 C25 116.4(11) . . ? C18 N12 C29 120.3(10) . . ? C18 N12 C27 120.1(11) . . ? C29 N12 C27 119.6(11) . . ? C5 O2 Cu1 133.4(10) . . ? C5 O2 Cu4 124.3(9) . . ? Cu1 O2 Cu4 100.6(5) . . ? C7 O3 Cu1 130.8(12) . . ? C7 O4 Cu3 119.5(9) . . ? C11 O7 Cu2 123.7(8) . 3_545 ? C15 O12 Cu3 117.4(9) . 1_545 ? C20 O13 Cu2 119.7(8) . . ? C20 O13 Na1 134.7(11) . 2_565 ? Cu2 O13 Na1 84.4(4) . 2_565 ? C20 O14 Cu4 127.7(9) . . ? C22 O15 Cu4 128.4(10) . . ? C22 O15 Cu1 127.7(9) . . ? Cu4 O15 Cu1 102.5(4) . . ? C26 O20 Cu2 110.8(10) . 1_565 ? C26 O20 Na1 133.3(9) . 2_575 ? Cu2 O20 Na1 86.9(4) 1_565 2_575 ? C28 O21 Na1 167.3(13) . . ? C30 O24 Cu3 125.1(8) . 3_455 ? Cu2 O28 Na1 84.3(5) . 2_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.648 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.149