Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_ind160 _database_code_CSD 173525 _audit_creation_method SHELXL-97 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Chaudhuri, Nirmalendu Ray' 'Dalai, Sudipta' 'Lloret, F.' 'Mukherjee, Partha Sarathi' 'Zangrando, Ennio' _publ_contact_author_name 'Prof Nirmalendu Ray Chaudhuri' _publ_contact_author_address ; Department of Inorganic Chemistry Indian Association for the Cultivation of Science Calcutta 700 032 INDIA ; _publ_contact_author_email 'ICNRC@MAHENDRA.IACS.RES.IN' _publ_section_title ; A novel class of interpenetrated 3-D network of dimeric cupric-tetracarboxylate unit ; _chemical_name_systematic ; bis-(fumarate-copper(II))-(4,4'-bipyridine) hemihydrated ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? ' (Cu2 4+) 2(C4 H2 O4 2-) (C10 H8 N2) 0.5(H2 O)' _chemical_formula_sum 'C18 H13 Cu2 N2 O8.50' _chemical_formula_weight 520.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 13.063(4) _cell_length_b 11.596(3) _cell_length_c 14.022(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.96(2) _cell_angle_gamma 90.00 _cell_volume 2052.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'emerald green' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 2.123 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8360 _exptl_absorpt_correction_T_max 0.9715 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _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 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4406 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 29.07 _reflns_number_total 2809 _reflns_number_gt 2149 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'MOSFLM (J. Appl. Cryst., 1993, 21, 67)' _computing_data_reduction 'MOSFLM (J. Appl. Cryst., 1993, 21, 67)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3/Windows (Farrugia,1997)' _computing_publication_material 'WinGX 1.63 (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+3.0855P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2809 _refine_ls_number_parameters 258 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1276 _refine_ls_wR_factor_gt 0.1186 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.74244(4) 0.5000 0.10333(4) 0.03027(17) Uani 1 2 d S . . Cu2 Cu 0.76583(4) 0.5000 0.29824(4) 0.03051(17) Uani 1 2 d S . . N1 N 0.7410(3) 0.5000 -0.0504(3) 0.0392(9) Uani 1 2 d SD . . C5 C 0.7836(9) 0.4142(8) -0.0894(6) 0.069(3) Uani 0.50 1 d PD . . C6 C 0.7868(10) 0.4092(9) -0.1866(7) 0.069(3) Uani 0.50 1 d PD . . C7 C 0.7491(4) 0.5000 -0.2469(3) 0.0402(10) Uani 1 2 d SD . . C8 C 0.6998(11) 0.5857(10) -0.2080(7) 0.080(4) Uani 0.50 1 d PD . . C9 C 0.6990(10) 0.5818(9) -0.1097(7) 0.074(3) Uani 0.50 1 d PD . . N2 N 0.7682(4) 0.5000 0.4519(3) 0.0447(10) Uani 1 2 d SD . . C10 C 0.8144(12) 0.4303(11) 0.5172(8) 0.140(8) Uani 0.50 1 d PD . . C11 C 0.8103(17) 0.4254(13) 0.6118(8) 0.174(10) Uani 0.50 1 d PD . . C12 C 0.7550(4) 0.5000 0.6480(3) 0.0433(11) Uani 1 2 d SD . . C14 C 0.7207(15) 0.5820(10) 0.4880(7) 0.113(7) Uani 0.50 1 d PD . . C13 C 0.7091(15) 0.5836(11) 0.5853(8) 0.111(6) Uani 0.50 1 d PD . . O1A O 0.6515(8) 0.3693(13) 0.1010(12) 0.048(2) Uani 0.50 1 d P . . O2A O 0.6768(5) 0.3600(6) 0.2641(5) 0.0453(15) Uani 0.50 1 d P . . O3A O 0.3680(7) 0.1007(10) 0.1409(10) 0.047(2) Uani 0.50 1 d P . . O4A O 0.3920(5) 0.0978(7) 0.3065(6) 0.0450(18) Uani 0.50 1 d P . . C1A C 0.6306(6) 0.3293(7) 0.1774(6) 0.0371(15) Uani 0.50 1 d P . . C2A C 0.5457(7) 0.2414(8) 0.1667(5) 0.0469(17) Uani 0.50 1 d P . . C3A C 0.5110(6) 0.2054(7) 0.2404(6) 0.0413(15) Uani 0.50 1 d P . . C4A C 0.4165(6) 0.1278(7) 0.2273(6) 0.0386(16) Uani 0.50 1 d P . . O1B O 0.6199(7) 0.6051(13) 0.0993(11) 0.044(2) Uani 0.50 1 d P . . O2B O 0.6377(6) 0.5951(7) 0.2615(6) 0.0513(17) Uani 0.50 1 d P . . O3B O 0.3366(8) 0.8656(9) 0.1384(9) 0.046(2) Uani 0.50 1 d P . . O4B O 0.3551(6) 0.8641(7) 0.2998(7) 0.0478(17) Uani 0.50 1 d P . . C1B C 0.5924(6) 0.6271(7) 0.1756(6) 0.0388(16) Uani 0.50 1 d P . . C2B C 0.4970(6) 0.7029(7) 0.1611(6) 0.0465(17) Uani 0.50 1 d P . . C3B C 0.4637(7) 0.7405(7) 0.2362(5) 0.0434(15) Uani 0.50 1 d P . . C4B C 0.3779(6) 0.8278(7) 0.2236(6) 0.0379(15) Uani 0.50 1 d P . . O1W O 1.0000 0.2918(10) 0.5000 0.102(4) Uani 0.50 2 d SP . . 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 0.0305(3) 0.0327(3) 0.0299(3) 0.000 0.0120(2) 0.000 Cu2 0.0308(3) 0.0325(3) 0.0305(3) 0.000 0.0120(2) 0.000 N1 0.045(2) 0.043(2) 0.0324(18) 0.000 0.0148(16) 0.000 C5 0.112(8) 0.068(6) 0.031(4) 0.010(4) 0.026(5) 0.029(6) C6 0.113(8) 0.056(5) 0.049(5) 0.010(4) 0.043(6) 0.031(6) C7 0.049(3) 0.046(3) 0.029(2) 0.000 0.0153(19) 0.000 C8 0.118(9) 0.084(7) 0.042(4) 0.016(4) 0.026(6) 0.058(7) C9 0.114(9) 0.073(6) 0.044(4) 0.019(4) 0.037(6) 0.056(7) N2 0.047(2) 0.055(3) 0.036(2) 0.000 0.0163(18) 0.000 C10 0.238(18) 0.155(14) 0.040(5) 0.041(7) 0.058(8) 0.146(14) C11 0.35(3) 0.147(13) 0.048(6) 0.050(7) 0.091(11) 0.179(16) C12 0.051(3) 0.052(3) 0.031(2) 0.000 0.019(2) 0.000 C14 0.241(19) 0.068(7) 0.042(6) 0.026(5) 0.058(9) 0.082(10) C13 0.208(16) 0.090(9) 0.050(6) 0.019(6) 0.059(8) 0.091(11) O1A 0.044(6) 0.059(6) 0.044(4) 0.000(4) 0.017(5) -0.016(5) O2A 0.049(4) 0.050(4) 0.039(3) -0.003(3) 0.015(3) -0.017(3) O3A 0.039(5) 0.059(6) 0.047(3) -0.010(4) 0.016(4) -0.021(3) O4A 0.036(4) 0.063(5) 0.034(3) 0.007(3) 0.006(3) -0.015(3) C1A 0.036(4) 0.036(4) 0.039(4) -0.003(3) 0.011(3) -0.006(3) C2A 0.046(4) 0.052(5) 0.043(4) -0.002(3) 0.010(3) -0.018(4) C3A 0.039(3) 0.038(4) 0.049(4) 0.000(3) 0.015(3) -0.008(3) C4A 0.038(4) 0.040(4) 0.039(4) 0.003(3) 0.011(3) 0.001(3) O1B 0.029(4) 0.064(7) 0.039(3) -0.002(4) 0.006(4) 0.019(4) O2B 0.048(4) 0.060(5) 0.052(3) 0.006(3) 0.024(3) 0.022(3) O3B 0.047(5) 0.050(5) 0.045(3) 0.006(4) 0.021(4) 0.019(3) O4B 0.049(5) 0.048(4) 0.045(3) 0.000(3) 0.011(4) 0.018(3) C1B 0.034(4) 0.039(4) 0.046(4) 0.001(3) 0.014(3) 0.007(3) C2B 0.039(4) 0.038(4) 0.067(5) 0.000(3) 0.021(3) 0.008(3) C3B 0.048(4) 0.038(4) 0.046(4) -0.002(3) 0.016(3) 0.011(3) C4B 0.035(4) 0.037(4) 0.045(4) 0.003(3) 0.015(3) 0.007(3) O1W 0.124(10) 0.082(8) 0.101(8) 0.000 0.032(7) 0.000 _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. NOTE: FUMARATE ANION AND BIPY LIGAND WERE FOUND DISORDER OVER TWO POSITIONS AND REFINED WITH AN OCCUPANCY FACTOR OF 0.5, NEGLECTING THE CONTRIBUTION OF HYDROGEN ATOMS. THE STATISTIC DISTRIBUTION OF E FACTORS INDICATED A CENTROSYMMETRIC STRUCTURE, FINALLY CORROBORATED BY THE SATISFACTORY REFINEMENT RESULTS USING THE CENTROSYMMETRIC SPACE GROUP C 2/M RATHER THAN C 2. THUS, MANY OF THE BOND LENGTHS AND DISTANCES ARE MEANINGLESS. ; 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 O1A 1.921(16) . ? Cu1 O1A 1.921(16) 6_565 ? Cu1 O3B 1.968(12) 8_565 ? Cu1 O3B 1.968(12) 3_545 ? Cu1 O3A 1.971(11) 3 ? Cu1 O3A 1.971(11) 8 ? Cu1 O1B 2.001(14) 6_565 ? Cu1 O1B 2.001(14) . ? Cu1 N1 2.150(4) . ? Cu1 Cu2 2.6704(10) . ? Cu2 O4B 1.957(8) 8_565 ? Cu2 O4B 1.957(8) 3_545 ? Cu2 O2B 1.959(7) 6_565 ? Cu2 O2B 1.959(7) . ? Cu2 O4A 1.979(8) 3 ? Cu2 O4A 1.979(8) 8 ? Cu2 O2A 1.982(7) . ? Cu2 O2A 1.982(7) 6_565 ? Cu2 N2 2.147(4) . ? N1 C9 1.288(9) 6_565 ? N1 C9 1.288(9) . ? N1 C5 1.325(10) 6_565 ? N1 C5 1.325(10) . ? C5 C9 1.069(14) 6_565 ? C5 C6 1.375(11) . ? C5 C8 1.739(14) 6_565 ? C5 C5 1.99(2) 6_565 ? C6 C8 1.099(16) 6_565 ? C6 C7 1.360(9) . ? C6 C9 1.768(14) 6_565 ? C7 C6 1.360(9) 6_565 ? C7 C8 1.371(10) . ? C7 C8 1.371(10) 6_565 ? C7 C12 1.496(6) 1_554 ? C8 C6 1.099(16) 6_565 ? C8 C9 1.382(12) . ? C8 C5 1.739(14) 6_565 ? C8 C8 1.99(2) 6_565 ? C9 C5 1.069(14) 6_565 ? C9 C6 1.768(14) 6_565 ? C9 C9 1.90(2) 6_565 ? N2 C10 1.252(10) . ? N2 C10 1.252(10) 6_565 ? N2 C14 1.307(11) 6_565 ? N2 C14 1.307(11) . ? C10 C14 1.20(2) 6_565 ? C10 C11 1.343(14) . ? C10 C10 1.62(3) 6_565 ? C10 C13 1.87(2) 6_565 ? C11 C13 1.28(2) 6_565 ? C11 C12 1.311(12) . ? C11 C11 1.73(3) 6_565 ? C11 C14 1.829(18) 6_565 ? C12 C11 1.311(12) 6_565 ? C12 C13 1.343(11) 6_565 ? C12 C13 1.343(11) . ? C12 C7 1.496(6) 1_556 ? C14 C10 1.20(2) 6_565 ? C14 C13 1.411(15) . ? C14 C11 1.829(18) 6_565 ? C14 C14 1.90(2) 6_565 ? C13 C11 1.28(2) 6_565 ? C13 C10 1.87(2) 6_565 ? C13 C13 1.94(3) 6_565 ? O1A O1B 0.504(15) 6_565 ? O1A C1A 1.261(18) . ? O1A C1B 1.453(16) 6_565 ? O2A O2B 0.724(8) 6_565 ? O2A C1A 1.262(10) . ? O2A C1B 1.440(11) 6_565 ? O3A O3B 0.562(11) 6_565 ? O3A C4A 1.253(14) . ? O3A C4B 1.404(14) 6_565 ? O3A Cu1 1.971(11) 3_445 ? O4A O4B 0.642(8) 6_565 ? O4A C4A 1.281(11) . ? O4A C4B 1.421(11) 6_565 ? O4A Cu2 1.979(8) 3_445 ? C1A C1B 0.706(8) 6_565 ? C1A O1B 1.311(17) 6_565 ? C1A O2B 1.453(11) 6_565 ? C1A C2A 1.485(10) . ? C1A C2B 1.741(11) 6_565 ? C2A C2B 0.896(10) 6_565 ? C2A C3A 1.300(11) . ? C2A C1B 1.636(11) 6_565 ? C2A C3B 1.637(11) 6_565 ? C3A C3B 0.871(10) 6_565 ? C3A C4A 1.500(10) . ? C3A C2B 1.516(11) 6_565 ? C3A C4B 1.737(10) 6_565 ? C4A C4B 0.713(8) 6_565 ? C4A O3B 1.406(14) 6_565 ? C4A O4B 1.452(12) 6_565 ? C4A C3B 1.639(11) 6_565 ? O1B O1A 0.504(15) 6_565 ? O1B C1B 1.240(17) . ? O1B C1A 1.311(17) 6_565 ? O2B O2A 0.724(8) 6_565 ? O2B C1B 1.253(11) . ? O2B C1A 1.453(11) 6_565 ? O3B O3A 0.562(11) 6_565 ? O3B C4B 1.256(15) . ? O3B C4A 1.406(14) 6_565 ? O3B Cu1 1.968(12) 3_455 ? O4B O4A 0.642(8) 6_565 ? O4B C4B 1.254(12) . ? O4B C4A 1.452(12) 6_565 ? O4B Cu2 1.957(8) 3_455 ? C1B C1A 0.706(8) 6_565 ? C1B O2A 1.440(11) 6_565 ? C1B O1A 1.453(16) 6_565 ? C1B C2B 1.496(10) . ? C1B C2A 1.636(11) 6_565 ? C2B C2A 0.896(11) 6_565 ? C2B C3B 1.314(11) . ? C2B C3A 1.516(11) 6_565 ? C2B C1A 1.741(11) 6_565 ? C3B C3A 0.871(10) 6_565 ? C3B C4B 1.487(10) . ? C3B C2A 1.637(11) 6_565 ? C3B C4A 1.639(11) 6_565 ? C4B C4A 0.713(8) 6_565 ? C4B O3A 1.404(14) 6_565 ? C4B O4A 1.421(11) 6_565 ? C4B C3A 1.737(10) 6_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 O1A Cu1 O1A 104.2(6) . 6_565 ? O1A Cu1 O3B 166.8(6) . 8_565 ? O1A Cu1 O3B 73.9(4) 6_565 8_565 ? O1A Cu1 O3B 73.9(4) . 3_545 ? O1A Cu1 O3B 166.8(6) 6_565 3_545 ? O3B Cu1 O3B 104.8(5) 8_565 3_545 ? O1A Cu1 O3A 160.1(5) . 3 ? O1A Cu1 O3A 90.3(4) 6_565 3 ? O3B Cu1 O3A 16.4(3) 8_565 3 ? O3B Cu1 O3A 88.8(4) 3_545 3 ? O1A Cu1 O3A 90.3(4) . 8 ? O1A Cu1 O3A 160.1(5) 6_565 8 ? O3B Cu1 O3A 88.8(4) 8_565 8 ? O3B Cu1 O3A 16.4(3) 3_545 8 ? O3A Cu1 O3A 72.6(5) 3 8 ? O1A Cu1 O1B 14.6(5) . 6_565 ? O1A Cu1 O1B 89.6(4) 6_565 6_565 ? O3B Cu1 O1B 159.0(5) 8_565 6_565 ? O3B Cu1 O1B 88.2(4) 3_545 6_565 ? O3A Cu1 O1B 166.6(6) 3 6_565 ? O3A Cu1 O1B 104.6(4) 8 6_565 ? O1A Cu1 O1B 89.6(4) . . ? O1A Cu1 O1B 14.6(5) 6_565 . ? O3B Cu1 O1B 88.2(4) 8_565 . ? O3B Cu1 O1B 159.0(5) 3_545 . ? O3A Cu1 O1B 104.6(4) 3 . ? O3A Cu1 O1B 166.6(6) 8 . ? O1B Cu1 O1B 75.0(6) 6_565 . ? O1A Cu1 N1 97.9(5) . . ? O1A Cu1 N1 97.9(5) 6_565 . ? O3B Cu1 N1 95.4(4) 8_565 . ? O3B Cu1 N1 95.4(4) 3_545 . ? O3A Cu1 N1 93.4(4) 3 . ? O3A Cu1 N1 93.4(4) 8 . ? O1B Cu1 N1 99.9(4) 6_565 . ? O1B Cu1 N1 99.9(4) . . ? O1A Cu1 Cu2 85.7(5) . . ? O1A Cu1 Cu2 85.7(5) 6_565 . ? O3B Cu1 Cu2 81.1(4) 8_565 . ? O3B Cu1 Cu2 81.1(4) 3_545 . ? O3A Cu1 Cu2 81.9(4) 3 . ? O3A Cu1 Cu2 81.9(4) 8 . ? O1B Cu1 Cu2 84.7(4) 6_565 . ? O1B Cu1 Cu2 84.7(4) . . ? N1 Cu1 Cu2 174.15(11) . . ? O4B Cu2 O4B 107.3(5) 8_565 3_545 ? O4B Cu2 O2B 157.2(3) 8_565 6_565 ? O4B Cu2 O2B 90.9(3) 3_545 6_565 ? O4B Cu2 O2B 90.9(3) 8_565 . ? O4B Cu2 O2B 157.2(3) 3_545 . ? O2B Cu2 O2B 68.5(5) 6_565 . ? O4B Cu2 O4A 18.8(2) 8_565 3 ? O4B Cu2 O4A 88.6(4) 3_545 3 ? O2B Cu2 O4A 168.5(3) 6_565 3 ? O2B Cu2 O4A 109.6(3) . 3 ? O4B Cu2 O4A 88.6(4) 8_565 8 ? O4B Cu2 O4A 18.8(2) 3_545 8 ? O2B Cu2 O4A 109.6(3) 6_565 8 ? O2B Cu2 O4A 168.5(3) . 8 ? O4A Cu2 O4A 69.9(4) 3 8 ? O4B Cu2 O2A 166.6(3) 8_565 . ? O4B Cu2 O2A 69.7(3) 3_545 . ? O2B Cu2 O2A 21.2(2) 6_565 . ? O2B Cu2 O2A 89.4(4) . . ? O4A Cu2 O2A 155.6(3) 3 . ? O4A Cu2 O2A 88.4(3) 8 . ? O4B Cu2 O2A 69.7(3) 8_565 6_565 ? O4B Cu2 O2A 166.6(3) 3_545 6_565 ? O2B Cu2 O2A 89.4(4) 6_565 6_565 ? O2B Cu2 O2A 21.2(2) . 6_565 ? O4A Cu2 O2A 88.4(3) 3 6_565 ? O4A Cu2 O2A 155.6(3) 8 6_565 ? O2A Cu2 O2A 110.0(4) . 6_565 ? O4B Cu2 N2 97.7(3) 8_565 . ? O4B Cu2 N2 97.7(3) 3_545 . ? O2B Cu2 N2 93.1(2) 6_565 . ? O2B Cu2 N2 93.1(2) . . ? O4A Cu2 N2 98.4(3) 3 . ? O4A Cu2 N2 98.4(3) 8 . ? O2A Cu2 N2 95.6(2) . . ? O2A Cu2 N2 95.6(2) 6_565 . ? O4B Cu2 Cu1 85.5(3) 8_565 . ? O4B Cu2 Cu1 85.5(3) 3_545 . ? O2B Cu2 Cu1 82.3(2) 6_565 . ? O2B Cu2 Cu1 82.3(2) . . ? O4A Cu2 Cu1 86.2(3) 3 . ? O4A Cu2 Cu1 86.2(3) 8 . ? O2A Cu2 Cu1 81.3(2) . . ? O2A Cu2 Cu1 81.3(2) 6_565 . ? N2 Cu2 Cu1 174.47(12) . . ? C9 N1 C9 94.9(11) 6_565 . ? C9 N1 C5 116.1(6) 6_565 6_565 ? C9 N1 C5 48.3(7) . 6_565 ? C9 N1 C5 48.3(7) 6_565 . ? C9 N1 C5 116.1(6) . . ? C5 N1 C5 97.3(9) 6_565 . ? C9 N1 Cu1 122.7(4) 6_565 . ? C9 N1 Cu1 122.7(4) . . ? C5 N1 Cu1 121.2(4) 6_565 . ? C5 N1 Cu1 121.2(4) . . ? C9 C5 N1 64.0(8) 6_565 . ? C9 C5 C6 91.8(9) 6_565 . ? N1 C5 C6 124.3(8) . . ? C9 C5 C8 52.6(8) 6_565 6_565 ? N1 C5 C8 99.6(8) . 6_565 ? C6 C5 C8 39.2(6) . 6_565 ? C9 C5 C5 87.5(9) 6_565 6_565 ? N1 C5 C5 41.3(4) . 6_565 ? C6 C5 C5 92.4(6) . 6_565 ? C8 C5 C5 90.0(5) 6_565 6_565 ? C8 C6 C7 66.8(8) 6_565 . ? C8 C6 C5 88.6(9) 6_565 . ? C7 C6 C5 119.0(8) . . ? C8 C6 C9 51.4(7) 6_565 6_565 ? C7 C6 C9 98.4(7) . 6_565 ? C5 C6 C9 37.2(5) . 6_565 ? C6 C7 C6 101.4(10) . 6_565 ? C6 C7 C8 116.5(6) . . ? C6 C7 C8 47.5(7) 6_565 . ? C6 C7 C8 47.5(7) . 6_565 ? C6 C7 C8 116.5(6) 6_565 6_565 ? C8 C7 C8 92.9(12) . 6_565 ? C6 C7 C12 120.7(4) . 1_554 ? C6 C7 C12 120.7(4) 6_565 1_554 ? C8 C7 C12 122.7(5) . 1_554 ? C8 C7 C12 122.7(5) 6_565 1_554 ? C6 C8 C7 65.7(8) 6_565 . ? C6 C8 C9 90.1(10) 6_565 . ? C7 C8 C9 119.8(8) . . ? C6 C8 C5 52.2(7) 6_565 6_565 ? C7 C8 C5 97.8(7) . 6_565 ? C9 C8 C5 37.9(6) . 6_565 ? C6 C8 C8 93.0(9) 6_565 6_565 ? C7 C8 C8 43.5(6) . 6_565 ? C9 C8 C8 88.1(7) . 6_565 ? C5 C8 C8 90.0(5) 6_565 6_565 ? C5 C9 N1 67.7(8) 6_565 . ? C5 C9 C8 89.5(10) 6_565 . ? N1 C9 C8 123.9(8) . . ? C5 C9 C6 51.0(7) 6_565 6_565 ? N1 C9 C6 101.6(7) . 6_565 ? C8 C9 C6 38.4(7) . 6_565 ? C5 C9 C9 92.5(9) 6_565 6_565 ? N1 C9 C9 42.6(6) . 6_565 ? C8 C9 C9 91.9(7) . 6_565 ? C6 C9 C9 93.4(5) 6_565 6_565 ? C10 N2 C10 80.3(13) . 6_565 ? C10 N2 C14 55.6(9) . 6_565 ? C10 N2 C14 112.0(7) 6_565 6_565 ? C10 N2 C14 112.0(7) . . ? C10 N2 C14 55.6(9) 6_565 . ? C14 N2 C14 93.4(14) 6_565 . ? C10 N2 Cu2 127.8(6) . . ? C10 N2 Cu2 127.8(6) 6_565 . ? C14 N2 Cu2 120.2(4) 6_565 . ? C14 N2 Cu2 120.2(4) . . ? C14 C10 N2 64.5(8) 6_565 . ? C14 C10 C11 92.0(12) 6_565 . ? N2 C10 C11 127.9(11) . . ? C14 C10 C10 96.9(10) 6_565 6_565 ? N2 C10 C10 49.8(7) . 6_565 ? C11 C10 C10 92.5(7) . 6_565 ? C14 C10 C13 48.8(9) 6_565 6_565 ? N2 C10 C13 98.6(9) . 6_565 ? C11 C10 C13 43.2(8) . 6_565 ? C10 C10 C13 95.0(6) 6_565 6_565 ? C13 C11 C12 62.4(9) 6_565 . ? C13 C11 C10 91.0(11) 6_565 . ? C12 C11 C10 121.4(10) . . ? C13 C11 C11 94.7(10) 6_565 6_565 ? C12 C11 C11 48.7(9) . 6_565 ? C10 C11 C11 87.5(7) . 6_565 ? C13 C11 C14 50.3(9) 6_565 6_565 ? C12 C11 C14 96.7(10) . 6_565 ? C10 C11 C14 40.8(7) . 6_565 ? C11 C11 C14 92.7(6) 6_565 6_565 ? C11 C12 C11 82.7(17) 6_565 . ? C11 C12 C13 114.9(7) 6_565 6_565 ? C11 C12 C13 57.8(10) . 6_565 ? C11 C12 C13 57.8(10) 6_565 . ? C11 C12 C13 114.9(7) . . ? C13 C12 C13 92.5(14) 6_565 . ? C11 C12 C7 123.8(5) 6_565 1_556 ? C11 C12 C7 123.8(5) . 1_556 ? C13 C12 C7 121.2(5) 6_565 1_556 ? C13 C12 C7 121.2(5) . 1_556 ? C10 C14 N2 59.9(9) 6_565 . ? C10 C14 C13 91.5(12) 6_565 . ? N2 C14 C13 124.3(8) . . ? C10 C14 C11 47.2(8) 6_565 6_565 ? N2 C14 C11 94.7(9) . 6_565 ? C13 C14 C11 44.4(9) . 6_565 ? C10 C14 C14 83.1(10) 6_565 6_565 ? N2 C14 C14 43.3(7) . 6_565 ? C13 C14 C14 90.8(7) . 6_565 ? C11 C14 C14 87.3(6) 6_565 6_565 ? C11 C13 C12 59.8(8) 6_565 . ? C11 C13 C14 85.4(13) 6_565 . ? C12 C13 C14 118.9(9) . . ? C11 C13 C10 45.8(8) 6_565 6_565 ? C12 C13 C10 90.5(8) . 6_565 ? C14 C13 C10 39.6(8) . 6_565 ? C11 C13 C13 85.3(10) 6_565 6_565 ? C12 C13 C13 43.8(7) . 6_565 ? C14 C13 C13 89.2(7) . 6_565 ? C10 C13 C13 85.0(6) 6_565 6_565 ? O1B O1A C1A 84(3) 6_565 . ? O1B O1A C1B 56(3) 6_565 6_565 ? C1A O1A C1B 29.1(5) . 6_565 ? O1B O1A Cu1 92(4) 6_565 . ? C1A O1A Cu1 123.0(11) . . ? C1B O1A Cu1 114.0(10) 6_565 . ? O2B O2A C1A 89.9(11) 6_565 . ? O2B O2A C1B 60.5(10) 6_565 6_565 ? C1A O2A C1B 29.4(4) . 6_565 ? O2B O2A Cu2 77.6(10) 6_565 . ? C1A O2A Cu2 124.7(6) . . ? C1B O2A Cu2 113.2(5) 6_565 . ? O3B O3A C4A 94(3) 6_565 . ? O3B O3A C4B 63(2) 6_565 6_565 ? C4A O3A C4B 30.5(5) . 6_565 ? O3B O3A Cu1 81(2) 6_565 3_445 ? C4A O3A Cu1 125.8(9) . 3_445 ? C4B O3A Cu1 117.6(7) 6_565 3_445 ? O4B O4A C4A 91.9(15) 6_565 . ? O4B O4A C4B 61.9(14) 6_565 6_565 ? C4A O4A C4B 30.0(4) . 6_565 ? O4B O4A Cu2 78.7(13) 6_565 3_445 ? C4A O4A Cu2 119.7(6) . 3_445 ? C4B O4A Cu2 111.7(5) 6_565 3_445 ? C1B C1A O1A 90.7(12) 6_565 . ? C1B C1A O2A 89.4(11) 6_565 . ? O1A C1A O2A 124.1(10) . . ? C1B C1A O1B 68.5(11) 6_565 6_565 ? O1A C1A O1B 22.5(6) . 6_565 ? O2A C1A O1B 124.2(10) . 6_565 ? C1B C1A O2B 59.5(10) 6_565 6_565 ? O1A C1A O2B 119.0(10) . 6_565 ? O2A C1A O2B 29.9(4) . 6_565 ? O1B C1A O2B 107.3(9) 6_565 6_565 ? C1B C1A C2A 89.2(11) 6_565 . ? O1A C1A C2A 119.1(9) . . ? O2A C1A C2A 116.8(7) . . ? O1B C1A C2A 113.5(8) 6_565 . ? O2B C1A C2A 112.7(7) 6_565 . ? C1B C1A C2B 58.3(9) 6_565 6_565 ? O1A C1A C2B 113.4(8) . 6_565 ? O2A C1A C2B 113.7(7) . 6_565 ? O1B C1A C2B 97.3(7) 6_565 6_565 ? O2B C1A C2B 95.0(6) 6_565 6_565 ? C2A C1A C2B 31.0(4) . 6_565 ? C2B C2A C3A 85.2(9) 6_565 . ? C2B C2A C1A 90.5(9) 6_565 . ? C3A C2A C1A 123.0(7) . . ? C2B C2A C1B 64.9(8) 6_565 6_565 ? C3A C2A C1B 116.0(7) . 6_565 ? C1A C2A C1B 25.6(3) . 6_565 ? C2B C2A C3B 53.2(8) 6_565 6_565 ? C3A C2A C3B 32.0(4) . 6_565 ? C1A C2A C3B 116.0(7) . 6_565 ? C1B C2A C3B 97.1(6) 6_565 6_565 ? C3B C3A C2A 95.9(9) 6_565 . ? C3B C3A C4A 82.9(8) 6_565 . ? C2A C3A C4A 122.6(7) . . ? C3B C3A C2B 59.8(8) 6_565 6_565 ? C2A C3A C2B 36.1(5) . 6_565 ? C4A C3A C2B 113.0(6) . 6_565 ? C3B C3A C4B 58.9(7) 6_565 6_565 ? C2A C3A C4B 120.4(7) . 6_565 ? C4A C3A C4B 24.0(3) . 6_565 ? C2B C3A C4B 97.4(6) 6_565 6_565 ? C4B C4A O3A 86.5(11) 6_565 . ? C4B C4A O4A 85.9(11) 6_565 . ? O3A C4A O4A 126.3(9) . . ? C4B C4A O3B 63.0(10) 6_565 6_565 ? O3A C4A O3B 23.5(5) . 6_565 ? O4A C4A O3B 119.3(8) . 6_565 ? C4B C4A O4B 59.7(10) 6_565 6_565 ? O3A C4A O4B 117.4(8) . 6_565 ? O4A C4A O4B 26.2(4) . 6_565 ? O3B C4A O4B 101.5(7) 6_565 6_565 ? C4B C4A C3A 97.0(11) 6_565 . ? O3A C4A C3A 117.6(8) . . ? O4A C4A C3A 116.0(7) . . ? O3B C4A C3A 118.4(8) 6_565 . ? O4B C4A C3A 117.5(7) 6_565 . ? C4B C4A C3B 65.1(10) 6_565 6_565 ? O3A C4A C3B 113.2(8) . 6_565 ? O4A C4A C3B 111.1(7) . 6_565 ? O3B C4A C3B 101.3(7) 6_565 6_565 ? O4B C4A C3B 98.7(7) 6_565 6_565 ? C3A C4A C3B 31.8(4) . 6_565 ? O1A O1B C1B 105(4) 6_565 . ? O1A O1B C1A 73(3) 6_565 6_565 ? C1B O1B C1A 32.0(5) . 6_565 ? O1A O1B Cu1 74(3) 6_565 . ? C1B O1B Cu1 120.6(10) . . ? C1A O1B Cu1 114.7(8) 6_565 . ? O2A O2B C1B 89.3(11) 6_565 . ? O2A O2B C1A 60.3(10) 6_565 6_565 ? C1B O2B C1A 29.1(4) . 6_565 ? O2A O2B Cu2 81.2(10) 6_565 . ? C1B O2B Cu2 125.4(6) . . ? C1A O2B Cu2 115.1(5) 6_565 . ? O3A O3B C4B 93(3) 6_565 . ? O3A O3B C4A 63(2) 6_565 6_565 ? C4B O3B C4A 30.4(5) . 6_565 ? O3A O3B Cu1 82(2) 6_565 3_455 ? C4B O3B Cu1 126.9(9) . 3_455 ? C4A O3B Cu1 116.8(8) 6_565 3_455 ? O4A O4B C4B 91.2(16) 6_565 . ? O4A O4B C4A 61.9(14) 6_565 6_565 ? C4B O4B C4A 29.4(4) . 6_565 ? O4A O4B Cu2 82.6(14) 6_565 3_455 ? C4B O4B Cu2 122.2(7) . 3_455 ? C4A O4B Cu2 112.1(6) 6_565 3_455 ? C1A C1B O1B 79.5(12) 6_565 . ? C1A C1B O2B 91.4(12) 6_565 . ? O1B C1B O2B 126.7(9) . . ? C1A C1B O2A 61.2(10) 6_565 6_565 ? O1B C1B O2A 115.9(8) . 6_565 ? O2B C1B O2A 30.2(4) . 6_565 ? C1A C1B O1A 60.2(11) 6_565 6_565 ? O1B C1B O1A 19.6(8) . 6_565 ? O2B C1B O1A 119.6(9) . 6_565 ? O2A C1B O1A 100.8(8) 6_565 6_565 ? C1A C1B C2B 98.0(11) 6_565 . ? O1B C1B C2B 114.8(9) . . ? O2B C1B C2B 118.4(7) . . ? O2A C1B C2B 118.9(7) 6_565 . ? O1A C1B C2B 117.6(9) 6_565 . ? C1A C1B C2A 65.2(10) 6_565 6_565 ? O1B C1B C2A 108.1(10) . 6_565 ? O2B C1B C2A 115.1(7) . 6_565 ? O2A C1B C2A 99.0(6) 6_565 6_565 ? O1A C1B C2A 100.1(9) 6_565 6_565 ? C2B C1B C2A 32.9(4) . 6_565 ? C2A C2B C3B 93.7(9) 6_565 . ? C2A C2B C1B 82.2(8) 6_565 . ? C3B C2B C1B 121.5(8) . . ? C2A C2B C3A 58.7(8) 6_565 6_565 ? C3B C2B C3A 35.0(5) . 6_565 ? C1B C2B C3A 112.0(7) . 6_565 ? C2A C2B C1A 58.5(7) 6_565 6_565 ? C3B C2B C1A 119.6(7) . 6_565 ? C1B C2B C1A 23.7(4) . 6_565 ? C3A C2B C1A 97.3(6) 6_565 6_565 ? C3A C3B C2B 85.3(9) 6_565 . ? C3A C3B C4B 91.0(8) 6_565 . ? C2B C3B C4B 121.7(7) . . ? C3A C3B C2A 52.2(8) 6_565 6_565 ? C2B C3B C2A 33.1(5) . 6_565 ? C4B C3B C2A 115.5(6) . 6_565 ? C3A C3B C4A 65.2(7) 6_565 6_565 ? C2B C3B C4A 116.3(7) . 6_565 ? C4B C3B C4A 25.8(3) . 6_565 ? C2A C3B C4A 97.2(6) 6_565 6_565 ? C4A C4B O4B 90.9(12) 6_565 . ? C4A C4B O3B 86.6(11) 6_565 . ? O4B C4B O3B 123.8(9) . . ? C4A C4B O3A 63.0(10) 6_565 6_565 ? O4B C4B O3A 121.0(9) . 6_565 ? O3B C4B O3A 23.6(6) . 6_565 ? C4A C4B O4A 64.1(10) 6_565 6_565 ? O4B C4B O4A 26.9(4) . 6_565 ? O3B C4B O4A 120.0(9) . 6_565 ? O3A C4B O4A 106.4(8) 6_565 6_565 ? C4A C4B C3B 89.1(11) 6_565 . ? O4B C4B C3B 117.7(7) . . ? O3B C4B C3B 118.4(8) . . ? O3A C4B C3B 114.0(8) 6_565 . ? O4A C4B C3B 112.4(7) 6_565 . ? C4A C4B C3A 59.0(9) 6_565 6_565 ? O4B C4B C3A 114.1(7) . 6_565 ? O3B C4B C3A 112.1(7) . 6_565 ? O3A C4B C3A 96.8(7) 6_565 6_565 ? O4A C4B C3A 96.3(6) 6_565 6_565 ? C3B C4B C3A 30.1(4) . 6_565 ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 29.07 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.900 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.111