# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Satoshi Takamizawa' _publ_contact_author_email STAKA@YOKOHAMA-CU.AC.JP _publ_section_title ; Switch of channel geometry by 1D component slide responding to slight structural stimuli of adsorbed guest ; loop_ _publ_author_name 'Satoshi Takamizawa' 'Takamasa Akatsuka' 'Ryosuke Miyake' # Attachment 'revised2_cif.txt' data_60724a1_1b_298K _database_code_depnum_ccdc_archive 'CCDC 736067' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 Cu2 N2 O8' _chemical_formula_weight 691.61 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/c 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' '-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 17.998(16) _cell_length_b 9.697(8) _cell_length_c 18.903(17) _cell_angle_alpha 90.00 _cell_angle_beta 97.339(18) _cell_angle_gamma 90.00 _cell_volume 3272(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 1.350 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7037 _exptl_absorpt_correction_T_max 0.9735 _exptl_absorpt_process_details ; SADABS; sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9009 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2903 _reflns_number_gt 2047 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1047P)^2^+3.1363P] 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 2903 _refine_ls_number_parameters 177 _refine_ls_number_restraints 270 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.1869 _refine_ls_wR_factor_gt 0.1704 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.123 _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 C1 C 0.1293(3) 0.7287(6) 0.2120(3) 0.0478(14) Uani 1 1 d U . . C2 C 0.2037(2) 0.7286(4) 0.1883(3) 0.0548(15) Uani 1 1 d GU . . C3 C 0.2296(3) 0.8472(4) 0.1581(3) 0.085(2) Uani 1 1 d GU . . H3 H 0.2016 0.9279 0.1566 0.102 Uiso 1 1 calc R . . C4 C 0.2975(3) 0.8450(5) 0.1303(3) 0.110(3) Uani 1 1 d GU . . H4 H 0.3148 0.9244 0.1101 0.132 Uiso 1 1 calc R . . C5 C 0.3394(2) 0.7244(6) 0.1327(3) 0.100(2) Uani 1 1 d GU . . H5 H 0.3848 0.7229 0.1141 0.121 Uiso 1 1 calc R . . C6 C 0.3135(2) 0.6058(5) 0.1628(3) 0.085(2) Uani 1 1 d GU . . H6 H 0.3416 0.5251 0.1644 0.102 Uiso 1 1 calc R . . C7 C 0.2457(3) 0.6080(4) 0.1907(3) 0.0645(17) Uani 1 1 d GU . . H7 H 0.2283 0.5286 0.2108 0.077 Uiso 1 1 calc R . . C8 C 0.0584(4) 0.7211(6) 0.3788(4) 0.0530(15) Uani 1 1 d U . . C9 C 0.0979(3) 0.7173(5) 0.4518(2) 0.0607(16) Uani 1 1 d GU . . C10 C 0.1014(3) 0.5934(4) 0.4890(3) 0.0731(19) Uani 1 1 d GU . . H10 H 0.0767 0.5160 0.4688 0.088 Uiso 1 1 calc R . . C11 C 0.1419(3) 0.5852(5) 0.5567(3) 0.094(2) Uani 1 1 d GU . . H11 H 0.1442 0.5023 0.5816 0.113 Uiso 1 1 calc R . . C12 C 0.1788(3) 0.7009(7) 0.5870(2) 0.099(2) Uani 1 1 d GU . . H12 H 0.2059 0.6954 0.6322 0.118 Uiso 1 1 calc R . . C13 C 0.1754(3) 0.8247(6) 0.5497(3) 0.104(3) Uani 1 1 d GU . . H13 H 0.2001 0.9021 0.5700 0.125 Uiso 1 1 calc R . . C14 C 0.1349(3) 0.8330(4) 0.4821(3) 0.087(2) Uani 1 1 d GU . . H14 H 0.1326 0.9158 0.4572 0.105 Uiso 1 1 calc R . . C15 C 0.0317(3) 0.2978(5) 0.2037(3) 0.0500(15) Uani 1 1 d U . . H15 H 0.0547 0.3439 0.1692 0.060 Uiso 1 1 calc R . . C16 C 0.0324(3) 0.1561(6) 0.2037(4) 0.0531(15) Uani 1 1 d U . . H16 H 0.0566 0.1103 0.1700 0.064 Uiso 1 1 calc R . . Cu1 Cu 0.0000 0.85959(8) 0.2500 0.0462(4) Uani 1 2 d SU . . Cu2 Cu 0.0000 0.59227(8) 0.2500 0.0440(4) Uani 1 2 d SU . . N1 N 0.0000 0.3715(6) 0.2500 0.0428(16) Uani 1 2 d SU . . N2 N 0.0000 0.0826(6) 0.2500 0.0450(16) Uani 1 2 d SU . . O1 O 0.0962(2) 0.8429(4) 0.2140(2) 0.0571(11) Uani 1 1 d U . . O2 O 0.1030(2) 0.6154(4) 0.2287(2) 0.0547(11) Uani 1 1 d U . . O3 O 0.0353(3) 0.6095(4) 0.3508(2) 0.0576(11) Uani 1 1 d U . . O4 O 0.0514(3) 0.8364(4) 0.3475(2) 0.0605(12) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.048(3) 0.027(3) 0.071(3) 0.002(2) 0.016(3) 0.001(2) C2 0.050(3) 0.038(3) 0.079(4) 0.003(3) 0.014(3) 0.004(2) C3 0.070(4) 0.072(4) 0.121(5) 0.020(4) 0.042(4) 0.013(3) C4 0.086(5) 0.107(5) 0.146(6) 0.027(5) 0.045(4) 0.004(4) C5 0.065(4) 0.105(5) 0.136(5) 0.003(4) 0.030(4) 0.021(4) C6 0.057(4) 0.077(4) 0.120(5) -0.011(4) 0.009(4) 0.020(3) C7 0.051(3) 0.048(3) 0.094(4) -0.008(3) 0.006(3) 0.009(3) C8 0.060(3) 0.038(3) 0.064(3) 0.000(3) 0.020(3) -0.003(3) C9 0.065(3) 0.058(3) 0.063(4) -0.011(3) 0.022(3) -0.010(3) C10 0.079(4) 0.076(4) 0.065(4) 0.004(3) 0.012(3) 0.005(3) C11 0.101(5) 0.101(5) 0.081(5) 0.001(4) 0.010(4) 0.011(4) C12 0.096(5) 0.113(5) 0.085(5) -0.008(4) 0.008(4) -0.004(4) C13 0.105(5) 0.107(5) 0.098(5) -0.026(4) 0.007(4) -0.021(4) C14 0.097(5) 0.082(4) 0.083(4) -0.014(4) 0.008(4) -0.020(4) C15 0.063(3) 0.018(3) 0.074(4) 0.006(2) 0.029(3) 0.001(2) C16 0.060(3) 0.026(3) 0.077(4) -0.002(3) 0.027(3) 0.003(2) Cu1 0.0538(7) 0.0063(5) 0.0824(8) 0.000 0.0237(5) 0.000 Cu2 0.0571(7) 0.0084(5) 0.0680(8) 0.000 0.0132(5) 0.000 N1 0.052(4) 0.007(3) 0.072(4) 0.000 0.016(3) 0.000 N2 0.049(4) 0.019(3) 0.069(4) 0.000 0.017(3) 0.000 O1 0.058(2) 0.022(2) 0.098(3) 0.0042(19) 0.033(2) 0.0039(17) O2 0.057(2) 0.023(2) 0.086(3) 0.0030(19) 0.017(2) 0.0009(17) O3 0.073(3) 0.032(2) 0.067(3) 0.0008(19) 0.007(2) -0.0044(19) O4 0.075(3) 0.032(2) 0.076(3) -0.004(2) 0.012(2) -0.010(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 C1 O2 1.252(7) . ? C1 O1 1.261(7) . ? C1 C2 1.466(7) . ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C6 C7 1.3900 . ? C8 O3 1.252(7) . ? C8 O4 1.265(7) . ? C8 C9 1.469(7) . ? C9 C10 1.3900 . ? C9 C14 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C15 N1 1.315(6) . ? C15 C16 1.374(8) . ? C16 N2 1.321(7) . ? Cu1 O1 1.946(4) 2 ? Cu1 O1 1.946(4) . ? Cu1 O4 1.966(5) . ? Cu1 O4 1.966(5) 2 ? Cu1 N2 2.163(6) 1_565 ? Cu1 Cu2 2.592(2) . ? Cu2 O3 1.938(5) . ? Cu2 O3 1.938(5) 2 ? Cu2 O2 1.960(4) 2 ? Cu2 O2 1.960(4) . ? Cu2 N1 2.141(6) . ? N1 C15 1.315(6) 2 ? N2 C16 1.321(7) 2 ? N2 Cu1 2.163(6) 1_545 ? 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 C1 O1 124.6(6) . . ? O2 C1 C2 117.8(5) . . ? O1 C1 C2 117.6(5) . . ? C3 C2 C7 120.0 . . ? C3 C2 C1 119.5(3) . . ? C7 C2 C1 120.3(3) . . ? C2 C3 C4 120.0 . . ? C3 C4 C5 120.0 . . ? C6 C5 C4 120.0 . . ? C7 C6 C5 120.0 . . ? C6 C7 C2 120.0 . . ? O3 C8 O4 124.0(6) . . ? O3 C8 C9 118.0(5) . . ? O4 C8 C9 118.0(5) . . ? C10 C9 C14 120.0 . . ? C10 C9 C8 118.8(4) . . ? C14 C9 C8 121.1(4) . . ? C11 C10 C9 120.0 . . ? C10 C11 C12 120.0 . . ? C13 C12 C11 120.0 . . ? C12 C13 C14 120.0 . . ? C13 C14 C9 120.0 . . ? N1 C15 C16 123.2(6) . . ? N2 C16 C15 122.4(6) . . ? O1 Cu1 O1 170.5(2) 2 . ? O1 Cu1 O4 89.8(2) 2 . ? O1 Cu1 O4 89.1(2) . . ? O1 Cu1 O4 89.1(2) 2 2 ? O1 Cu1 O4 89.8(2) . 2 ? O4 Cu1 O4 166.9(2) . 2 ? O1 Cu1 N2 94.77(11) 2 1_565 ? O1 Cu1 N2 94.77(11) . 1_565 ? O4 Cu1 N2 96.56(12) . 1_565 ? O4 Cu1 N2 96.56(12) 2 1_565 ? O1 Cu1 Cu2 85.23(11) 2 . ? O1 Cu1 Cu2 85.23(11) . . ? O4 Cu1 Cu2 83.44(12) . . ? O4 Cu1 Cu2 83.44(12) 2 . ? N2 Cu1 Cu2 180.000(1) 1_565 . ? O3 Cu2 O3 170.1(2) . 2 ? O3 Cu2 O2 89.34(19) . 2 ? O3 Cu2 O2 89.53(19) 2 2 ? O3 Cu2 O2 89.53(19) . . ? O3 Cu2 O2 89.34(19) 2 . ? O2 Cu2 O2 166.9(2) 2 . ? O3 Cu2 N1 94.94(12) . . ? O3 Cu2 N1 94.94(12) 2 . ? O2 Cu2 N1 96.57(11) 2 . ? O2 Cu2 N1 96.57(11) . . ? O3 Cu2 Cu1 85.06(12) . . ? O3 Cu2 Cu1 85.06(12) 2 . ? O2 Cu2 Cu1 83.43(11) 2 . ? O2 Cu2 Cu1 83.43(11) . . ? N1 Cu2 Cu1 180.000(1) . . ? C15 N1 C15 114.2(6) 2 . ? C15 N1 Cu2 122.9(3) 2 . ? C15 N1 Cu2 122.9(3) . . ? C16 N2 C16 114.7(7) 2 . ? C16 N2 Cu1 122.7(3) 2 1_545 ? C16 N2 Cu1 122.7(3) . 1_545 ? C1 O1 Cu1 121.9(4) . . ? C1 O2 Cu2 123.3(4) . . ? C8 O3 Cu2 122.6(4) . . ? C8 O4 Cu1 123.2(4) . . ? 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 O2 C1 C2 C3 169.3(5) . . . . ? O1 C1 C2 C3 -10.6(7) . . . . ? O2 C1 C2 C7 -5.5(8) . . . . ? O1 C1 C2 C7 174.6(5) . . . . ? C7 C2 C3 C4 0.0 . . . . ? C1 C2 C3 C4 -174.9(5) . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 C7 0.0 . . . . ? C5 C6 C7 C2 0.0 . . . . ? C3 C2 C7 C6 0.0 . . . . ? C1 C2 C7 C6 174.8(5) . . . . ? O3 C8 C9 C10 -6.4(7) . . . . ? O4 C8 C9 C10 175.3(4) . . . . ? O3 C8 C9 C14 170.1(5) . . . . ? O4 C8 C9 C14 -8.2(7) . . . . ? C14 C9 C10 C11 0.0 . . . . ? C8 C9 C10 C11 176.5(5) . . . . ? C9 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C9 0.0 . . . . ? C10 C9 C14 C13 0.0 . . . . ? C8 C9 C14 C13 -176.4(5) . . . . ? N1 C15 C16 N2 1.2(9) . . . . ? O1 Cu1 Cu2 O3 -81.4(2) 2 . . . ? O1 Cu1 Cu2 O3 98.6(2) . . . . ? O4 Cu1 Cu2 O3 8.97(18) . . . . ? O4 Cu1 Cu2 O3 -171.03(18) 2 . . . ? N2 Cu1 Cu2 O3 160(97) 1_565 . . . ? O1 Cu1 Cu2 O3 98.6(2) 2 . . 2 ? O1 Cu1 Cu2 O3 -81.4(2) . . . 2 ? O4 Cu1 Cu2 O3 -171.03(18) . . . 2 ? O4 Cu1 Cu2 O3 8.97(18) 2 . . 2 ? N2 Cu1 Cu2 O3 -20(42) 1_565 . . 2 ? O1 Cu1 Cu2 O2 8.54(18) 2 . . 2 ? O1 Cu1 Cu2 O2 -171.46(18) . . . 2 ? O4 Cu1 Cu2 O2 98.87(19) . . . 2 ? O4 Cu1 Cu2 O2 -81.13(19) 2 . . 2 ? N2 Cu1 Cu2 O2 -110(100) 1_565 . . 2 ? O1 Cu1 Cu2 O2 -171.46(18) 2 . . . ? O1 Cu1 Cu2 O2 8.54(18) . . . . ? O4 Cu1 Cu2 O2 -81.13(19) . . . . ? O4 Cu1 Cu2 O2 98.87(19) 2 . . . ? N2 Cu1 Cu2 O2 70(43) 1_565 . . . ? O1 Cu1 Cu2 N1 20(100) 2 . . . ? O1 Cu1 Cu2 N1 -160(100) . . . . ? O4 Cu1 Cu2 N1 111(100) . . . . ? O4 Cu1 Cu2 N1 -69(100) 2 . . . ? N2 Cu1 Cu2 N1 0(58) 1_565 . . . ? C16 C15 N1 C15 -0.6(4) . . . 2 ? C16 C15 N1 Cu2 179.4(4) . . . . ? O3 Cu2 N1 C15 49.8(4) . . . 2 ? O3 Cu2 N1 C15 -130.2(4) 2 . . 2 ? O2 Cu2 N1 C15 -40.1(4) 2 . . 2 ? O2 Cu2 N1 C15 139.9(4) . . . 2 ? Cu1 Cu2 N1 C15 -52(100) . . . 2 ? O3 Cu2 N1 C15 -130.2(4) . . . . ? O3 Cu2 N1 C15 49.8(4) 2 . . . ? O2 Cu2 N1 C15 139.9(4) 2 . . . ? O2 Cu2 N1 C15 -40.1(4) . . . . ? Cu1 Cu2 N1 C15 128(100) . . . . ? C15 C16 N2 C16 -0.6(4) . . . 2 ? C15 C16 N2 Cu1 179.4(4) . . . 1_545 ? O2 C1 O1 Cu1 4.0(9) . . . . ? C2 C1 O1 Cu1 -176.1(4) . . . . ? O1 Cu1 O1 C1 -9.3(5) 2 . . . ? O4 Cu1 O1 C1 74.1(5) . . . . ? O4 Cu1 O1 C1 -92.8(5) 2 . . . ? N2 Cu1 O1 C1 170.7(5) 1_565 . . . ? Cu2 Cu1 O1 C1 -9.3(5) . . . . ? O1 C1 O2 Cu2 7.8(9) . . . . ? C2 C1 O2 Cu2 -172.1(4) . . . . ? O3 Cu2 O2 C1 -96.2(5) . . . . ? O3 Cu2 O2 C1 74.0(5) 2 . . . ? O2 Cu2 O2 C1 -11.1(5) 2 . . . ? N1 Cu2 O2 C1 168.9(5) . . . . ? Cu1 Cu2 O2 C1 -11.1(5) . . . . ? O4 C8 O3 Cu2 10.4(9) . . . . ? C9 C8 O3 Cu2 -167.8(4) . . . . ? O3 Cu2 O3 C8 -12.8(5) 2 . . . ? O2 Cu2 O3 C8 -96.3(5) 2 . . . ? O2 Cu2 O3 C8 70.6(5) . . . . ? N1 Cu2 O3 C8 167.2(5) . . . . ? Cu1 Cu2 O3 C8 -12.8(5) . . . . ? O3 C8 O4 Cu1 2.0(9) . . . . ? C9 C8 O4 Cu1 -179.9(4) . . . . ? O1 Cu1 O4 C8 76.5(5) 2 . . . ? O1 Cu1 O4 C8 -94.0(5) . . . . ? O4 Cu1 O4 C8 -8.7(5) 2 . . . ? N2 Cu1 O4 C8 171.3(5) 1_565 . . . ? Cu2 Cu1 O4 C8 -8.7(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.049 _refine_diff_density_min -1.018 _refine_diff_density_rms 0.115 #===END data_61104a1_1b_2(acetone)_90K _database_code_depnum_ccdc_archive 'CCDC 736068' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H36 Cu2 N2 O10' _chemical_formula_weight 807.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 17.757(3) _cell_length_b 9.6260(16) _cell_length_c 10.8050(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.603(4) _cell_angle_gamma 90.00 _cell_volume 1838.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 90 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 1.217 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6685 _exptl_absorpt_correction_T_max 0.9089 _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6902 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 28.36 _reflns_number_total 2430 _reflns_number_gt 1738 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+2.6405P] 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 2430 _refine_ls_number_parameters 188 _refine_ls_number_restraints 275 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1282 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.096 _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 C1 C 0.3658(2) 1.0000 0.0604(4) 0.0246(8) Uani 1 2 d SU . . C2 C 0.2893(2) 1.0000 0.1067(4) 0.0252(8) Uani 1 2 d SU . . C3 C 0.25371(16) 0.8755(3) 0.1293(3) 0.0318(7) Uani 1 1 d U . . H3 H 0.2771 0.7900 0.1117 0.038 Uiso 1 1 calc R . . C4 C 0.18450(17) 0.8753(3) 0.1770(3) 0.0409(8) Uani 1 1 d U . . H4 H 0.1602 0.7899 0.1919 0.049 Uiso 1 1 calc R . . C5 C 0.1504(2) 1.0000 0.2032(5) 0.0428(11) Uani 1 2 d SU . . H5 H 0.1037 1.0000 0.2392 0.051 Uiso 1 2 calc SR . . C7 C 0.5669(3) 0.9318(5) 0.3619(6) 0.0309(12) Uani 0.50 1 d PDU . -1 C8 C 0.5906(3) 1.0335(5) 0.4459(6) 0.0387(15) Uani 0.50 1 d PDU . -1 H8 H 0.5942 1.1270 0.4188 0.046 Uiso 0.50 1 calc PR . -1 C9 C 0.6092(3) 1.0005(13) 0.5697(5) 0.0455(11) Uani 1 2 d SDU . -1 C10 C 0.6030(4) 0.8647(6) 0.6098(6) 0.0441(15) Uani 0.50 1 d PDU . -1 H10 H 0.6155 0.8424 0.6950 0.053 Uiso 0.50 1 calc PR . -1 H9 H 0.6263 1.0705 0.6275 0.053 Uiso 0.50 1 d PR . -1 C11 C 0.5787(4) 0.7617(6) 0.5265(6) 0.0418(15) Uani 0.50 1 d PDU . -1 H11 H 0.5741 0.6686 0.5541 0.050 Uiso 0.50 1 calc PR . -1 C12 C 0.5611(3) 0.7951(6) 0.4024(5) 0.0360(13) Uani 0.50 1 d PDU . -1 H12 H 0.5451 0.7244 0.3445 0.043 Uiso 0.50 1 calc PR . -1 C13 C 0.46131(16) 0.5714(3) 0.0769(3) 0.0374(8) Uani 1 1 d U . . H13 H 0.4329 0.6196 0.1334 0.045 Uiso 1 1 calc R . . C1S C 0.3154(4) 0.5637(9) 0.3437(7) 0.0556(19) Uani 0.50 1 d PU A -1 C2S C 0.2591(4) 0.492(5) 0.2530(7) 0.070(3) Uani 0.50 1 d PU A -1 H2S1 H 0.2833 0.4665 0.1786 0.104 Uiso 0.50 1 calc PR A -1 H2S2 H 0.2166 0.5549 0.2297 0.104 Uiso 0.50 1 calc PR A -1 H2S3 H 0.2404 0.4083 0.2914 0.104 Uiso 0.50 1 calc PR A -1 C3S C 0.2891(6) 0.6193(10) 0.4547(9) 0.080(3) Uani 0.50 1 d PU A -1 H3S1 H 0.3309 0.6669 0.5035 0.121 Uiso 0.50 1 calc PR A -1 H3S2 H 0.2704 0.5436 0.5041 0.121 Uiso 0.50 1 calc PR A -1 H3S3 H 0.2481 0.6855 0.4325 0.121 Uiso 0.50 1 calc PR A -1 Cu1 Cu 0.4950(2) 0.86724(5) -0.0213(3) 0.0254(6) Uani 0.50 1 d PDU . -1 N1 N 0.5000 0.6432(3) 0.0000 0.0430(10) Uani 1 2 d SU . . O1 O 0.39577(13) 0.88578(19) 0.0442(3) 0.0478(7) Uani 1 1 d DU . . O2 O 0.5301(3) 0.8645(5) 0.1526(5) 0.0285(13) Uani 0.50 1 d PDU . . C6 C 0.5452(4) 0.9645(6) 0.2307(7) 0.0253(17) Uani 0.50 1 d PU . -1 O1S O 0.3790(4) 0.5793(8) 0.3185(6) 0.086(2) Uani 0.50 1 d PU A -1 O3 O 0.5408(3) 1.0919(6) 0.1948(5) 0.0260(13) Uani 0.50 1 d PU . -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0260(18) 0.0104(13) 0.036(2) 0.000 -0.0017(16) 0.000 C2 0.0228(17) 0.0169(15) 0.035(2) 0.000 -0.0028(16) 0.000 C3 0.0275(14) 0.0224(12) 0.0448(18) 0.0005(12) 0.0000(12) -0.0016(10) C4 0.0276(14) 0.0335(15) 0.061(2) 0.0031(14) 0.0012(14) -0.0081(11) C5 0.023(2) 0.043(2) 0.062(3) 0.000 0.002(2) 0.000 C7 0.031(3) 0.029(3) 0.033(3) -0.006(2) 0.002(2) 0.004(2) C8 0.040(3) 0.031(4) 0.045(3) -0.006(2) 0.003(3) -0.003(2) C9 0.044(3) 0.048(3) 0.044(3) -0.001(6) 0.000(2) 0.001(6) C10 0.045(3) 0.050(3) 0.037(3) 0.003(3) 0.002(3) 0.004(3) C11 0.048(3) 0.037(3) 0.040(3) 0.002(3) 0.005(3) 0.011(3) C12 0.042(3) 0.028(2) 0.037(3) 0.000(2) 0.002(3) 0.008(2) C13 0.0288(15) 0.0163(13) 0.069(2) -0.0094(13) 0.0154(14) 0.0002(10) C1S 0.048(4) 0.065(4) 0.054(4) 0.010(3) 0.006(3) 0.002(3) C2S 0.082(4) 0.050(7) 0.078(4) -0.015(8) 0.015(3) 0.000(7) C3S 0.074(5) 0.091(6) 0.075(6) -0.027(5) 0.005(4) -0.011(4) Cu1 0.0239(9) 0.0044(2) 0.047(2) -0.0003(3) 0.0020(12) -0.0009(3) N1 0.0309(18) 0.0072(13) 0.094(3) 0.000 0.0196(18) 0.000 O1 0.0341(12) 0.0125(9) 0.100(2) 0.0008(10) 0.0243(12) 0.0008(7) O2 0.036(3) 0.017(2) 0.031(4) -0.006(2) -0.004(2) 0.0011(19) C6 0.023(2) 0.025(4) 0.027(3) -0.009(2) 0.003(2) -0.001(2) O1S 0.063(4) 0.120(5) 0.075(4) 0.005(4) 0.013(3) 0.005(4) O3 0.037(3) 0.024(4) 0.015(4) 0.003(2) -0.010(3) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.242(3) 6_575 ? C1 O1 1.242(3) . ? C1 C2 1.492(5) . ? C2 C3 1.387(3) 6_575 ? C2 C3 1.387(3) . ? C3 C4 1.378(4) . ? C4 C5 1.385(4) . ? C5 C4 1.385(4) 6_575 ? C7 C8 1.372(7) . ? C7 C12 1.394(7) . ? C7 C6 1.467(10) . ? C8 C9 1.384(7) . ? C9 C10 1.385(12) . ? C10 C11 1.379(8) . ? C11 C12 1.385(8) . ? C13 N1 1.324(3) . ? C13 C13 1.374(5) 6_565 ? C1S O1S 1.197(9) . ? C1S C3S 1.433(12) . ? C1S C2S 1.50(2) . ? Cu1 O2 1.921(6) . ? Cu1 O1 1.971(5) . ? Cu1 O1 1.987(5) 2_655 ? Cu1 N1 2.169(3) . ? N1 C13 1.324(3) 2_655 ? N1 Cu1 2.169(3) 2_655 ? O1 Cu1 1.987(5) 2_655 ? O2 O3 0.636(5) 6_575 ? O2 C6 1.292(7) . ? O2 C6 1.857(8) 6_575 ? C6 O3 1.286(9) . ? C6 O2 1.857(8) 6_575 ? O3 O2 0.636(5) 6_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O1 124.6(4) 6_575 . ? O1 C1 C2 117.66(19) 6_575 . ? O1 C1 C2 117.66(19) . . ? C3 C2 C3 119.4(4) 6_575 . ? C3 C2 C1 120.28(19) 6_575 . ? C3 C2 C1 120.28(19) . . ? C4 C3 C2 120.4(3) . . ? C3 C4 C5 119.9(3) . . ? C4 C5 C4 120.0(4) 6_575 . ? C8 C7 C12 119.5(5) . . ? C8 C7 C6 121.4(5) . . ? C12 C7 C6 119.1(5) . . ? C7 C8 C9 120.3(6) . . ? C8 C9 C10 120.0(7) . . ? C11 C10 C9 120.3(5) . . ? C10 C11 C12 119.4(5) . . ? C11 C12 C7 120.5(5) . . ? N1 C13 C13 121.51(16) . 6_565 ? O1S C1S C3S 122.4(8) . . ? O1S C1S C2S 119.6(8) . . ? C3S C1S C2S 117.9(8) . . ? O2 Cu1 O2 177.9(3) 2_655 . ? O2 Cu1 O1 98.8(3) 2_655 . ? O2 Cu1 O1 82.3(2) . . ? O2 Cu1 O1 95.2(3) 2_655 2_655 ? O2 Cu1 O1 84.0(2) . 2_655 ? O1 Cu1 O1 162.69(13) . 2_655 ? O2 Cu1 N1 95.2(2) 2_655 . ? O2 Cu1 N1 82.90(17) . . ? O1 Cu1 N1 94.61(14) . . ? O1 Cu1 N1 94.15(13) 2_655 . ? C13 N1 C13 117.0(3) . 2_655 ? C13 N1 Cu1 118.10(19) . 2_655 ? C13 N1 Cu1 124.6(2) 2_655 2_655 ? C13 N1 Cu1 124.6(2) . . ? C13 N1 Cu1 118.10(19) 2_655 . ? Cu1 N1 Cu1 12.62(12) 2_655 . ? C1 O1 Cu1 122.8(2) . . ? C1 O1 Cu1 122.3(2) . 2_655 ? Cu1 O1 Cu1 13.84(13) . 2_655 ? O3 O2 C6 7.8(7) 6_575 . ? O3 O2 Cu1 137.2(10) 6_575 2_655 ? C6 O2 Cu1 130.7(6) . 2_655 ? O3 O2 C6 21.2(7) 6_575 6_575 ? C6 O2 C6 14.2(3) . 6_575 ? Cu1 O2 C6 116.5(4) 2_655 6_575 ? O3 O2 Cu1 137.6(9) 6_575 . ? C6 O2 Cu1 131.0(6) . . ? C6 O2 Cu1 116.8(4) 6_575 . ? O3 C6 O2 120.7(8) . . ? O3 C6 C7 119.9(5) . . ? O2 C6 C7 119.3(6) . . ? O2 C6 O2 110.6(8) . 6_575 ? C7 C6 O2 130.0(5) . 6_575 ? O2 O3 C6 148.5(10) 6_575 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 0.6(6) 6_575 . . 6_575 ? O1 C1 C2 C3 178.5(4) . . . 6_575 ? O1 C1 C2 C3 -178.5(4) 6_575 . . . ? O1 C1 C2 C3 -0.6(6) . . . . ? C3 C2 C3 C4 -1.8(6) 6_575 . . . ? C1 C2 C3 C4 177.3(3) . . . . ? C2 C3 C4 C5 -0.3(6) . . . . ? C3 C4 C5 C4 2.5(7) . . . 6_575 ? C12 C7 C8 C9 0.4(8) . . . . ? C6 C7 C8 C9 178.6(5) . . . . ? C7 C8 C9 C10 -0.8(8) . . . . ? C8 C9 C10 C11 0.4(10) . . . . ? C9 C10 C11 C12 0.5(10) . . . . ? C10 C11 C12 C7 -0.9(10) . . . . ? C8 C7 C12 C11 0.4(9) . . . . ? C6 C7 C12 C11 -177.8(6) . . . . ? C13 C13 N1 C13 0.0 6_565 . . 2_655 ? C13 C13 N1 Cu1 -173.88(8) 6_565 . . 2_655 ? C13 C13 N1 Cu1 173.43(8) 6_565 . . . ? O2 Cu1 N1 C13 -121.2(3) 2_655 . . . ? O2 Cu1 N1 C13 59.7(3) . . . . ? O1 Cu1 N1 C13 -21.9(2) . . . . ? O1 Cu1 N1 C13 143.1(2) 2_655 . . . ? O2 Cu1 N1 C13 52.1(4) 2_655 . . 2_655 ? O2 Cu1 N1 C13 -127.0(3) . . . 2_655 ? O1 Cu1 N1 C13 151.43(19) . . . 2_655 ? O1 Cu1 N1 C13 -43.5(2) 2_655 . . 2_655 ? O2 Cu1 N1 Cu1 176.3(13) 2_655 . . 2_655 ? O2 Cu1 N1 Cu1 -2.8(10) . . . 2_655 ? O1 Cu1 N1 Cu1 -84.4(11) . . . 2_655 ? O1 Cu1 N1 Cu1 80.7(10) 2_655 . . 2_655 ? O1 C1 O1 Cu1 -4.2(7) 6_575 . . . ? C2 C1 O1 Cu1 178.1(3) . . . . ? O1 C1 O1 Cu1 12.3(7) 6_575 . . 2_655 ? C2 C1 O1 Cu1 -165.5(3) . . . 2_655 ? O2 Cu1 O1 C1 -88.3(4) 2_655 . . . ? O2 Cu1 O1 C1 93.5(3) . . . . ? O1 Cu1 O1 C1 55.4(5) 2_655 . . . ? N1 Cu1 O1 C1 175.6(3) . . . . ? O2 Cu1 O1 Cu1 179.3(2) 2_655 . . 2_655 ? O2 Cu1 O1 Cu1 1.05(17) . . . 2_655 ? O1 Cu1 O1 Cu1 -37.0(4) 2_655 . . 2_655 ? N1 Cu1 O1 Cu1 83.23(12) . . . 2_655 ? O2 Cu1 O2 O3 149(10) 2_655 . . 6_575 ? O1 Cu1 O2 O3 -89.7(14) . . . 6_575 ? O1 Cu1 O2 O3 79.7(14) 2_655 . . 6_575 ? N1 Cu1 O2 O3 174.7(14) . . . 6_575 ? O2 Cu1 O2 C6 154(10) 2_655 . . . ? O1 Cu1 O2 C6 -84.0(8) . . . . ? O1 Cu1 O2 C6 85.4(8) 2_655 . . . ? N1 Cu1 O2 C6 -179.7(8) . . . . ? O2 Cu1 O2 Cu1 80(17) 2_655 . . 2_655 ? O1 Cu1 O2 Cu1 -159(7) . . . 2_655 ? O1 Cu1 O2 Cu1 11(7) 2_655 . . 2_655 ? N1 Cu1 O2 Cu1 106(7) . . . 2_655 ? O2 Cu1 O2 C6 154(10) 2_655 . . 6_575 ? O1 Cu1 O2 C6 -84.3(5) . . . 6_575 ? O1 Cu1 O2 C6 85.1(5) 2_655 . . 6_575 ? N1 Cu1 O2 C6 -179.9(5) . . . 6_575 ? O3 O2 C6 O3 147(6) 6_575 . . . ? Cu1 O2 C6 O3 -2.0(13) 2_655 . . . ? C6 O2 C6 O3 -2.3(4) 6_575 . . . ? Cu1 O2 C6 O3 -3.2(12) . . . . ? O3 O2 C6 C7 -33(5) 6_575 . . . ? Cu1 O2 C6 C7 177.3(5) 2_655 . . . ? C6 O2 C6 C7 177.1(11) 6_575 . . . ? Cu1 O2 C6 C7 176.1(4) . . . . ? O3 O2 C6 O2 149(5) 6_575 . . 6_575 ? Cu1 O2 C6 O2 0.2(13) 2_655 . . 6_575 ? C6 O2 C6 O2 0.000(10) 6_575 . . 6_575 ? Cu1 O2 C6 O2 -1.0(12) . . . 6_575 ? C8 C7 C6 O3 -7.1(9) . . . . ? C12 C7 C6 O3 171.1(6) . . . . ? C8 C7 C6 O2 173.5(7) . . . . ? C12 C7 C6 O2 -8.3(10) . . . . ? C8 C7 C6 O2 -10.0(10) . . . 6_575 ? C12 C7 C6 O2 168.2(6) . . . 6_575 ? O2 C6 O3 O2 12(2) . . . 6_575 ? C7 C6 O3 O2 -167.4(19) . . . 6_575 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.800 _refine_diff_density_min -0.477 _refine_diff_density_rms 0.085 #===END data_60723a1_1b_90K _database_code_depnum_ccdc_archive 'CCDC 745355' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 Cu2 N2 O8' _chemical_formula_weight 691.61 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/c 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' '-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 17.485(3) _cell_length_b 9.6876(19) _cell_length_c 19.213(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.432(4) _cell_angle_gamma 90.00 _cell_volume 3219.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 90 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 1.372 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6999 _exptl_absorpt_correction_T_max 0.9731 _exptl_absorpt_process_details ; SADABS; sheldrick, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11425 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3999 _reflns_number_gt 2987 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0814P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3999 _refine_ls_number_parameters 201 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1462 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.136 _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 C1 C 0.1340(2) 0.7337(3) 0.2152(2) 0.0174(7) Uani 1 1 d . . . C2 C 0.2099(2) 0.7342(4) 0.1894(2) 0.0186(7) Uani 1 1 d . . . C3 C 0.2392(2) 0.8551(4) 0.1650(2) 0.0255(9) Uani 1 1 d . . . H3 H 0.2123 0.9396 0.1680 0.031 Uiso 1 1 calc R . . C4 C 0.3074(2) 0.8536(4) 0.1362(2) 0.0321(10) Uani 1 1 d . . . H4 H 0.3272 0.9367 0.1195 0.039 Uiso 1 1 calc R . . C5 C 0.3464(2) 0.7303(4) 0.1318(2) 0.0307(10) Uani 1 1 d . . . H5 H 0.3921 0.7282 0.1104 0.037 Uiso 1 1 calc R . . C6 C 0.3194(2) 0.6105(4) 0.1584(2) 0.0276(9) Uani 1 1 d . . . H6 H 0.3472 0.5267 0.1566 0.033 Uiso 1 1 calc R . . C7 C 0.2519(2) 0.6123(4) 0.1875(2) 0.0216(8) Uani 1 1 d . . . H7 H 0.2339 0.5299 0.2064 0.026 Uiso 1 1 calc R . . C8 C 0.0589(2) 0.7228(4) 0.3785(2) 0.0189(8) Uani 1 1 d . . . C9 C 0.0985(2) 0.7176(4) 0.4518(2) 0.0202(8) Uani 1 1 d . . . C10 C 0.1010(2) 0.5960(4) 0.4908(2) 0.0241(8) Uani 1 1 d . . . H10 H 0.0745 0.5166 0.4707 0.029 Uiso 1 1 calc R . . C11 C 0.1410(2) 0.5889(4) 0.5576(2) 0.0311(10) Uani 1 1 d . . . H11 H 0.1415 0.5055 0.5836 0.037 Uiso 1 1 calc R . . C12 C 0.1808(3) 0.7033(5) 0.5872(2) 0.0341(10) Uani 1 1 d . . . H12 H 0.2097 0.6977 0.6331 0.041 Uiso 1 1 calc R . . C13 C 0.1784(3) 0.8249(5) 0.5500(2) 0.0359(11) Uani 1 1 d . . . H13 H 0.2050 0.9038 0.5705 0.043 Uiso 1 1 calc R . . C14 C 0.1375(2) 0.8328(4) 0.4831(2) 0.0292(9) Uani 1 1 d . . . H14 H 0.1358 0.9174 0.4580 0.035 Uiso 1 1 calc R . . C15 C 0.0379(2) 0.3014(3) 0.2071(2) 0.0193(8) Uani 1 1 d . . . H15 H 0.0655 0.3495 0.1756 0.023 Uiso 1 1 calc R . . C16 C 0.0382(2) 0.1580(3) 0.2071(2) 0.0192(8) Uani 1 1 d . . . H16 H 0.0662 0.1103 0.1757 0.023 Uiso 1 1 calc R . . Cu1 Cu 0.0000 0.86259(6) 0.2500 0.01650(19) Uani 1 2 d SU . . Cu2 Cu 0.0000 0.59529(6) 0.2500 0.01612(19) Uani 1 2 d SU . . N1 N 0.0000 0.3729(4) 0.2500 0.0163(9) Uani 1 2 d SU . . N2 N 0.0000 0.0859(4) 0.2500 0.0181(9) Uani 1 2 d SU . . O1 O 0.09927(15) 0.8482(2) 0.21633(14) 0.0208(6) Uani 1 1 d . . . O2 O 0.10779(15) 0.6197(2) 0.23241(15) 0.0212(6) Uani 1 1 d . . . O3 O 0.03399(16) 0.6098(2) 0.35099(14) 0.0210(6) Uani 1 1 d . . . O4 O 0.05340(15) 0.8382(2) 0.34741(14) 0.0216(6) 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 C1 0.0181(18) 0.0078(16) 0.027(2) 0.0001(13) 0.0047(15) 0.0020(13) C2 0.0171(18) 0.0100(17) 0.029(2) -0.0003(14) 0.0049(15) 0.0018(13) C3 0.021(2) 0.0141(19) 0.044(3) 0.0058(16) 0.0127(17) 0.0053(14) C4 0.024(2) 0.026(2) 0.048(3) 0.0086(19) 0.0116(19) -0.0027(17) C5 0.017(2) 0.034(2) 0.043(3) -0.0042(19) 0.0099(18) 0.0034(17) C6 0.018(2) 0.020(2) 0.044(3) -0.0087(17) 0.0028(17) 0.0079(15) C7 0.0186(19) 0.0098(18) 0.036(2) -0.0027(15) 0.0027(16) 0.0043(13) C8 0.0186(18) 0.0104(17) 0.030(2) -0.0028(14) 0.0115(15) -0.0014(13) C9 0.0187(18) 0.0148(18) 0.029(2) -0.0025(15) 0.0091(15) -0.0016(14) C10 0.024(2) 0.018(2) 0.032(2) 0.0007(15) 0.0089(17) 0.0003(15) C11 0.030(2) 0.029(2) 0.034(2) 0.0036(18) 0.0051(18) 0.0042(18) C12 0.027(2) 0.045(3) 0.031(2) -0.0027(19) 0.0048(18) -0.0008(19) C13 0.034(3) 0.038(3) 0.037(3) -0.011(2) 0.008(2) -0.015(2) C14 0.035(2) 0.020(2) 0.034(2) -0.0046(17) 0.0111(18) -0.0057(17) C15 0.0181(18) 0.0066(18) 0.035(2) 0.0020(14) 0.0100(15) 0.0007(13) C16 0.0177(18) 0.0077(18) 0.034(2) -0.0022(14) 0.0094(15) -0.0007(13) Cu1 0.0171(3) 0.0024(3) 0.0317(4) 0.000 0.0092(2) 0.000 Cu2 0.0188(3) 0.0022(3) 0.0282(4) 0.000 0.0061(2) 0.000 N1 0.019(2) 0.0028(18) 0.028(2) 0.000 0.0058(17) 0.000 N2 0.017(2) 0.008(2) 0.030(2) 0.000 0.0046(17) 0.000 O1 0.0204(14) 0.0059(12) 0.0389(16) 0.0031(10) 0.0137(11) 0.0025(9) O2 0.0196(14) 0.0060(12) 0.0393(17) 0.0011(10) 0.0084(12) 0.0009(10) O3 0.0288(15) 0.0074(12) 0.0271(15) 0.0000(10) 0.0050(11) -0.0013(10) O4 0.0256(14) 0.0057(13) 0.0339(16) 0.0002(10) 0.0061(11) -0.0025(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.258(4) . ? C1 O1 1.266(4) . ? C1 C2 1.483(5) . ? C2 C3 1.388(5) . ? C2 C7 1.394(5) . ? C3 C4 1.386(5) . ? C4 C5 1.384(6) . ? C5 C6 1.380(6) . ? C6 C7 1.378(5) . ? C8 O4 1.265(4) . ? C8 O3 1.265(4) . ? C8 C9 1.476(5) . ? C9 C10 1.394(5) . ? C9 C14 1.397(5) . ? C10 C11 1.370(6) . ? C11 C12 1.386(6) . ? C12 C13 1.375(7) . ? C13 C14 1.379(6) . ? C15 N1 1.326(4) . ? C15 C16 1.389(5) . ? C16 N2 1.332(4) . ? Cu1 O1 1.944(2) . ? Cu1 O1 1.944(2) 2 ? Cu1 O4 1.979(3) 2 ? Cu1 O4 1.979(3) . ? Cu1 N2 2.164(4) 1_565 ? Cu1 Cu2 2.5895(9) . ? Cu2 O3 1.949(3) 2 ? Cu2 O3 1.949(3) . ? Cu2 O2 1.977(3) . ? Cu2 O2 1.977(3) 2 ? Cu2 N1 2.155(4) . ? N1 C15 1.326(4) 2 ? N2 C16 1.332(4) 2 ? N2 Cu1 2.164(4) 1_545 ? 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 C1 O1 124.9(3) . . ? O2 C1 C2 117.9(3) . . ? O1 C1 C2 117.2(3) . . ? C3 C2 C7 118.9(4) . . ? C3 C2 C1 120.6(3) . . ? C7 C2 C1 120.5(3) . . ? C4 C3 C2 120.6(3) . . ? C5 C4 C3 119.6(4) . . ? C6 C5 C4 120.3(4) . . ? C7 C6 C5 120.0(3) . . ? C6 C7 C2 120.5(4) . . ? O4 C8 O3 124.8(4) . . ? O4 C8 C9 118.2(3) . . ? O3 C8 C9 117.0(3) . . ? C10 C9 C14 118.0(4) . . ? C10 C9 C8 121.0(3) . . ? C14 C9 C8 121.0(3) . . ? C11 C10 C9 121.1(4) . . ? C10 C11 C12 120.1(4) . . ? C13 C12 C11 119.7(4) . . ? C12 C13 C14 120.3(4) . . ? C13 C14 C9 120.7(4) . . ? N1 C15 C16 121.6(3) . . ? N2 C16 C15 121.5(3) . . ? O1 Cu1 O1 171.78(14) . 2 ? O1 Cu1 O4 89.84(11) . 2 ? O1 Cu1 O4 89.18(11) 2 2 ? O1 Cu1 O4 89.18(11) . . ? O1 Cu1 O4 89.84(11) 2 . ? O4 Cu1 O4 166.29(14) 2 . ? O1 Cu1 N2 94.11(7) . 1_565 ? O1 Cu1 N2 94.11(7) 2 1_565 ? O4 Cu1 N2 96.85(7) 2 1_565 ? O4 Cu1 N2 96.85(7) . 1_565 ? O1 Cu1 Cu2 85.89(7) . . ? O1 Cu1 Cu2 85.89(7) 2 . ? O4 Cu1 Cu2 83.15(7) 2 . ? O4 Cu1 Cu2 83.15(7) . . ? N2 Cu1 Cu2 180.000(1) 1_565 . ? O3 Cu2 O3 171.75(14) 2 . ? O3 Cu2 O2 88.88(11) 2 . ? O3 Cu2 O2 90.14(11) . . ? O3 Cu2 O2 90.14(11) 2 2 ? O3 Cu2 O2 88.88(11) . 2 ? O2 Cu2 O2 166.29(14) . 2 ? O3 Cu2 N1 94.13(7) 2 . ? O3 Cu2 N1 94.13(7) . . ? O2 Cu2 N1 96.86(7) . . ? O2 Cu2 N1 96.86(7) 2 . ? O3 Cu2 Cu1 85.87(7) 2 . ? O3 Cu2 Cu1 85.87(7) . . ? O2 Cu2 Cu1 83.14(7) . . ? O2 Cu2 Cu1 83.14(7) 2 . ? N1 Cu2 Cu1 180.0 . . ? C15 N1 C15 117.1(4) . 2 ? C15 N1 Cu2 121.5(2) . . ? C15 N1 Cu2 121.5(2) 2 . ? C16 N2 C16 116.8(4) . 2 ? C16 N2 Cu1 121.6(2) . 1_545 ? C16 N2 Cu1 121.6(2) 2 1_545 ? C1 O1 Cu1 121.4(2) . . ? C1 O2 Cu2 122.8(2) . . ? C8 O3 Cu2 121.0(2) . . ? C8 O4 Cu1 123.0(2) . . ? 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 O2 C1 C2 C3 175.4(4) . . . . ? O1 C1 C2 C3 -2.6(6) . . . . ? O2 C1 C2 C7 -2.8(6) . . . . ? O1 C1 C2 C7 179.2(4) . . . . ? C7 C2 C3 C4 2.8(6) . . . . ? C1 C2 C3 C4 -175.3(4) . . . . ? C2 C3 C4 C5 0.0(7) . . . . ? C3 C4 C5 C6 -2.5(7) . . . . ? C4 C5 C6 C7 2.0(7) . . . . ? C5 C6 C7 C2 1.0(6) . . . . ? C3 C2 C7 C6 -3.4(6) . . . . ? C1 C2 C7 C6 174.8(4) . . . . ? O4 C8 C9 C10 174.8(3) . . . . ? O3 C8 C9 C10 -6.5(5) . . . . ? O4 C8 C9 C14 -8.0(5) . . . . ? O3 C8 C9 C14 170.7(4) . . . . ? C14 C9 C10 C11 -0.6(6) . . . . ? C8 C9 C10 C11 176.7(4) . . . . ? C9 C10 C11 C12 -0.9(6) . . . . ? C10 C11 C12 C13 1.6(7) . . . . ? C11 C12 C13 C14 -1.0(7) . . . . ? C12 C13 C14 C9 -0.5(7) . . . . ? C10 C9 C14 C13 1.3(6) . . . . ? C8 C9 C14 C13 -176.0(4) . . . . ? N1 C15 C16 N2 0.3(5) . . . . ? O1 Cu1 Cu2 O3 -79.90(11) . . . 2 ? O1 Cu1 Cu2 O3 100.10(11) 2 . . 2 ? O4 Cu1 Cu2 O3 10.43(10) 2 . . 2 ? O4 Cu1 Cu2 O3 -169.57(10) . . . 2 ? N2 Cu1 Cu2 O3 165(66) 1_565 . . 2 ? O1 Cu1 Cu2 O3 100.10(11) . . . . ? O1 Cu1 Cu2 O3 -79.90(11) 2 . . . ? O4 Cu1 Cu2 O3 -169.57(10) 2 . . . ? O4 Cu1 Cu2 O3 10.43(10) . . . . ? N2 Cu1 Cu2 O3 -15(27) 1_565 . . . ? O1 Cu1 Cu2 O2 9.46(11) . . . . ? O1 Cu1 Cu2 O2 -170.54(11) 2 . . . ? O4 Cu1 Cu2 O2 99.79(11) 2 . . . ? O4 Cu1 Cu2 O2 -80.21(11) . . . . ? N2 Cu1 Cu2 O2 -106(71) 1_565 . . . ? O1 Cu1 Cu2 O2 -170.54(11) . . . 2 ? O1 Cu1 Cu2 O2 9.46(11) 2 . . 2 ? O4 Cu1 Cu2 O2 -80.21(11) 2 . . 2 ? O4 Cu1 Cu2 O2 99.79(11) . . . 2 ? N2 Cu1 Cu2 O2 74(27) 1_565 . . 2 ? O1 Cu1 Cu2 N1 -161(100) . . . . ? O1 Cu1 Cu2 N1 19(100) 2 . . . ? O4 Cu1 Cu2 N1 -70(100) 2 . . . ? O4 Cu1 Cu2 N1 110(100) . . . . ? N2 Cu1 Cu2 N1 0(41) 1_565 . . . ? C16 C15 N1 C15 -0.2(2) . . . 2 ? C16 C15 N1 Cu2 179.8(2) . . . . ? O3 Cu2 N1 C15 53.0(2) 2 . . . ? O3 Cu2 N1 C15 -127.0(2) . . . . ? O2 Cu2 N1 C15 -36.4(2) . . . . ? O2 Cu2 N1 C15 143.6(2) 2 . . . ? Cu1 Cu2 N1 C15 134(100) . . . . ? O3 Cu2 N1 C15 -127.0(2) 2 . . 2 ? O3 Cu2 N1 C15 53.0(2) . . . 2 ? O2 Cu2 N1 C15 143.6(2) . . . 2 ? O2 Cu2 N1 C15 -36.4(2) 2 . . 2 ? Cu1 Cu2 N1 C15 -46(100) . . . 2 ? C15 C16 N2 C16 -0.2(2) . . . 2 ? C15 C16 N2 Cu1 179.8(2) . . . 1_545 ? O2 C1 O1 Cu1 3.0(5) . . . . ? C2 C1 O1 Cu1 -179.2(2) . . . . ? O1 Cu1 O1 C1 -9.7(3) 2 . . . ? O4 Cu1 O1 C1 -92.8(3) 2 . . . ? O4 Cu1 O1 C1 73.5(3) . . . . ? N2 Cu1 O1 C1 170.3(3) 1_565 . . . ? Cu2 Cu1 O1 C1 -9.7(3) . . . . ? O1 C1 O2 Cu2 10.0(5) . . . . ? C2 C1 O2 Cu2 -167.8(2) . . . . ? O3 Cu2 O2 C1 73.1(3) 2 . . . ? O3 Cu2 O2 C1 -98.7(3) . . . . ? O2 Cu2 O2 C1 -12.9(3) 2 . . . ? N1 Cu2 O2 C1 167.1(3) . . . . ? Cu1 Cu2 O2 C1 -12.9(3) . . . . ? O4 C8 O3 Cu2 11.3(5) . . . . ? C9 C8 O3 Cu2 -167.3(2) . . . . ? O3 Cu2 O3 C8 -14.4(3) 2 . . . ? O2 Cu2 O3 C8 68.7(3) . . . . ? O2 Cu2 O3 C8 -97.6(3) 2 . . . ? N1 Cu2 O3 C8 165.6(3) . . . . ? Cu1 Cu2 O3 C8 -14.4(3) . . . . ? O3 C8 O4 Cu1 2.8(5) . . . . ? C9 C8 O4 Cu1 -178.6(2) . . . . ? O1 Cu1 O4 C8 -96.3(3) . . . . ? O1 Cu1 O4 C8 75.5(3) 2 . . . ? O4 Cu1 O4 C8 -10.4(3) 2 . . . ? N2 Cu1 O4 C8 169.6(3) 1_565 . . . ? Cu2 Cu1 O4 C8 -10.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.035 _refine_diff_density_min -1.702 _refine_diff_density_rms 0.135