# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Hongwei Hou' _publ_contact_author_email houhongw@zzu.edu.cn _publ_section_title ; Crystal structures and magnetism of infinite alternating chains arranged by paddle-wheel dinuclear copper and mononuclear copper units ; _publ_author_name 'Hongwei Hou' # Attachment '- revised cif.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 823529' #TrackingRef '- revised cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H52 Cu3 N6 O32' _chemical_formula_weight 1127.34 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 23.847(5) _cell_length_b 11.390(2) _cell_length_c 8.9114(18) _cell_angle_alpha 90.00 _cell_angle_beta 93.32(3) _cell_angle_gamma 90.00 _cell_volume 2416.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _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 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1162 _exptl_absorpt_coefficient_mu 1.408 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7223 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11672 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2203 _reflns_number_gt 2081 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.1130P)^2^+16.6854P] 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 2203 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.0842 _refine_ls_wR_factor_ref 0.2197 _refine_ls_wR_factor_gt 0.2147 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.010 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 -0.5000 0.5000 0.0000 0.0429(5) Uani 1 4 d S . . Cu2 Cu 0.03032(4) 0.0000 -0.37223(11) 0.0346(4) Uani 1 2 d S . . O1 O -0.0249(2) 0.1225(6) -0.3226(5) 0.0633(16) Uani 1 1 d . . . O2 O -0.07743(19) 0.1235(4) -0.5390(5) 0.0481(12) Uani 1 1 d . . . O3 O -0.4385(2) 0.5000 -0.1371(7) 0.0428(15) Uani 1 2 d S . . O4 O -0.3773(3) 0.5000 0.0634(8) 0.064(2) Uani 1 2 d S . . O5 O -0.5000 0.6724(7) 0.0000 0.066(2) Uani 1 2 d S . . O6 O -0.1198(4) 0.5000 -0.5283(12) 0.093(3) Uani 1 2 d S . . O7 O -0.2389(2) 0.2982(5) -0.2363(8) 0.0744(17) Uani 1 1 d . . . N1 N -0.2391(3) 0.5000 -0.2304(10) 0.047(2) Uani 1 2 d S . . N2 N -0.1815(2) 0.3951(5) -0.3889(7) 0.0510(15) Uani 1 1 d . . . C1 C -0.3874(4) 0.5000 -0.0743(11) 0.044(2) Uani 1 2 d S . . C2 C -0.3415(4) 0.5000 -0.1879(11) 0.050(3) Uani 1 2 d S . . C3 C -0.2819(4) 0.5000 -0.1125(11) 0.050(2) Uani 1 2 d S . . H3A H -0.2765 0.4311 -0.0493 0.060 Uiso 0.50 1 d PR . . C4 C -0.0667(3) 0.1575(6) -0.4064(8) 0.0427(15) Uani 1 1 d . . . C5 C -0.1042(3) 0.2506(7) -0.3391(9) 0.0556(19) Uani 1 1 d . . . H5A H -0.1167 0.2216 -0.2442 0.067 Uiso 1 1 calc R . . H5B H -0.0821 0.3208 -0.3182 0.067 Uiso 1 1 calc R . . C6 C -0.1562(3) 0.2835(7) -0.4414(10) 0.063(2) Uani 1 1 d . . . H6A H -0.1453 0.2930 -0.5440 0.075 Uiso 1 1 calc R . . H6B H -0.1837 0.2209 -0.4401 0.075 Uiso 1 1 calc R . . C7 C -0.1581(5) 0.5000 -0.4408(14) 0.058(3) Uani 1 2 d S . . C8 C -0.2207(3) 0.3919(6) -0.2817(9) 0.0483(17) Uani 1 1 d . . . H5 H -0.5095 0.6970 0.0798 0.058 Uiso 0.50 1 d PR . . H2A H -0.3456 0.4314 -0.2499 0.058 Uiso 0.50 1 d PR . . O8 O -0.1118(11) 0.5000 -0.085(3) 0.218(9) Uani 1 2 d S . . O9 O -0.3232(5) 0.1300(13) -0.1347(18) 0.200(6) Uani 1 1 d . . . O10 O -0.2227(8) 0.0000 -0.2948(19) 0.175(7) Uani 1 2 d S . . O11 O -0.0635(5) 0.3045(9) -0.8090(13) 0.148(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0285(8) 0.0659(11) 0.0357(9) 0.000 0.0137(6) 0.000 Cu2 0.0272(6) 0.0442(7) 0.0329(6) 0.000 0.0071(4) 0.000 O1 0.045(3) 0.094(4) 0.050(3) -0.014(3) 0.000(2) 0.031(3) O2 0.043(3) 0.054(3) 0.048(3) -0.011(2) 0.002(2) 0.012(2) O3 0.023(3) 0.067(4) 0.039(3) 0.000 0.008(2) 0.000 O4 0.045(4) 0.110(7) 0.037(4) 0.000 0.002(3) 0.000 O5 0.088(6) 0.060(5) 0.054(4) 0.000 0.034(4) 0.000 O6 0.077(6) 0.114(8) 0.093(7) 0.000 0.055(6) 0.000 O7 0.060(3) 0.052(3) 0.114(5) 0.006(3) 0.033(3) -0.003(3) N1 0.026(4) 0.053(5) 0.064(5) 0.000 0.018(4) 0.000 N2 0.036(3) 0.050(3) 0.068(4) -0.006(3) 0.015(3) 0.006(3) C1 0.036(5) 0.054(6) 0.042(5) 0.000 0.008(4) 0.000 C2 0.023(4) 0.086(7) 0.042(5) 0.000 0.017(4) 0.000 C3 0.026(4) 0.074(7) 0.050(6) 0.000 0.006(4) 0.000 C4 0.035(3) 0.048(4) 0.047(4) -0.004(3) 0.015(3) -0.002(3) C5 0.041(4) 0.060(5) 0.067(5) -0.009(4) 0.010(3) 0.015(3) C6 0.046(4) 0.062(5) 0.079(5) -0.023(4) -0.001(4) 0.014(4) C7 0.043(6) 0.063(7) 0.070(7) 0.000 0.013(5) 0.000 C8 0.030(3) 0.042(4) 0.074(5) 0.002(3) 0.008(3) 0.004(3) O8 0.25(3) 0.19(2) 0.21(2) 0.000 -0.025(18) 0.000 O9 0.161(11) 0.187(13) 0.244(15) 0.068(11) -0.051(10) -0.030(10) O10 0.172(16) 0.209(18) 0.140(13) 0.000 -0.033(12) 0.000 O11 0.159(9) 0.119(7) 0.169(9) 0.001(7) 0.045(7) 0.046(7) _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 O3 1.962(6) . ? Cu1 O3 1.962(6) 5_465 ? Cu1 O5 1.964(8) 5_465 ? Cu1 O5 1.964(8) . ? Cu2 O1 1.985(5) . ? Cu2 O1 1.985(5) 6 ? Cu2 O2 1.992(4) 2_554 ? Cu2 O2 1.992(4) 5_554 ? Cu2 O3 2.182(6) 3_545 ? Cu2 Cu2 2.626(2) 5_554 ? O1 C4 1.275(8) . ? O2 C4 1.256(8) . ? O2 Cu2 1.992(4) 5_554 ? O3 C1 1.311(11) . ? O3 Cu2 2.182(6) 3_455 ? O4 C1 1.238(12) . ? O5 H5 0.8085 . ? O6 C7 1.234(13) . ? O7 C8 1.229(9) . ? N1 C8 1.394(8) 6_565 ? N1 C8 1.394(8) . ? N1 C3 1.506(12) . ? N2 C8 1.375(9) . ? N2 C7 1.408(8) . ? N2 C6 1.494(9) . ? C1 C2 1.535(12) . ? C2 C3 1.536(13) . ? C2 H2A 0.9591 . ? C3 H3A 0.9700 . ? C4 C5 1.531(9) . ? C5 C6 1.541(11) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N2 1.408(8) 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 O3 Cu1 O3 180 . 5_465 ? O3 Cu1 O5 90 . 5_465 ? O3 Cu1 O5 90 5_465 5_465 ? O3 Cu1 O5 90 . . ? O3 Cu1 O5 90 5_465 . ? O5 Cu1 O5 180 5_465 . ? O1 Cu2 O1 89.3(4) . 6 ? O1 Cu2 O2 89.3(2) . 2_554 ? O1 Cu2 O2 168.8(2) 6 2_554 ? O1 Cu2 O2 168.8(2) . 5_554 ? O1 Cu2 O2 89.3(2) 6 5_554 ? O2 Cu2 O2 89.8(3) 2_554 5_554 ? O1 Cu2 O3 88.81(18) . 3_545 ? O1 Cu2 O3 88.81(18) 6 3_545 ? O2 Cu2 O3 102.30(17) 2_554 3_545 ? O2 Cu2 O3 102.30(17) 5_554 3_545 ? O1 Cu2 Cu2 81.62(15) . 5_554 ? O1 Cu2 Cu2 81.62(15) 6 5_554 ? O2 Cu2 Cu2 87.17(14) 2_554 5_554 ? O2 Cu2 Cu2 87.17(14) 5_554 5_554 ? O3 Cu2 Cu2 166.50(16) 3_545 5_554 ? C4 O1 Cu2 126.6(4) . . ? C4 O2 Cu2 120.2(4) . 5_554 ? C1 O3 Cu1 116.4(6) . . ? C1 O3 Cu2 131.7(6) . 3_455 ? Cu1 O3 Cu2 111.9(3) . 3_455 ? Cu1 O5 H5 110.2 . . ? C8 N1 C8 124.2(8) 6_565 . ? C8 N1 C3 117.9(4) 6_565 . ? C8 N1 C3 117.9(4) . . ? C8 N2 C7 123.3(6) . . ? C8 N2 C6 119.9(6) . . ? C7 N2 C6 116.3(6) . . ? O4 C1 O3 123.2(8) . . ? O4 C1 C2 123.2(9) . . ? O3 C1 C2 113.6(8) . . ? C1 C2 C3 112.9(8) . . ? C1 C2 H2A 109.1 . . ? C3 C2 H2A 108.3 . . ? N1 C3 C2 109.9(8) . . ? N1 C3 H3A 109.4 . . ? C2 C3 H3A 110.1 . . ? O2 C4 O1 124.3(6) . . ? O2 C4 C5 119.4(6) . . ? O1 C4 C5 116.3(6) . . ? C6 C5 C4 113.9(6) . . ? C6 C5 H5A 108.8 . . ? C4 C5 H5A 108.8 . . ? C6 C5 H5B 108.8 . . ? C4 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N2 C6 C5 110.3(6) . . ? N2 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? N2 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? O6 C7 N2 121.9(4) . . ? O6 C7 N2 121.9(4) . 6_565 ? N2 C7 N2 116.1(9) . 6_565 ? O7 C8 N2 121.3(6) . . ? O7 C8 N1 122.3(7) . . ? N2 C8 N1 116.4(6) . . ? 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 Cu2 O1 C4 -79.3(7) 6 . . . ? O2 Cu2 O1 C4 89.5(6) 2_554 . . . ? O2 Cu2 O1 C4 3.7(16) 5_554 . . . ? O3 Cu2 O1 C4 -168.2(6) 3_545 . . . ? Cu2 Cu2 O1 C4 2.3(6) 5_554 . . . ? O3 Cu1 O3 C1 180 5_465 . . . ? O5 Cu1 O3 C1 -90 5_465 . . . ? O5 Cu1 O3 C1 90 . . . . ? O3 Cu1 O3 Cu2 0(100) 5_465 . . 3_455 ? O5 Cu1 O3 Cu2 90 5_465 . . 3_455 ? O5 Cu1 O3 Cu2 -90. . . . 3_455 ? Cu1 O3 C1 O4 0.0 . . . . ? Cu2 O3 C1 O4 180 3_455 . . . ? Cu1 O3 C1 C2 180 . . . . ? Cu2 O3 C1 C2 0.0 3_455 . . . ? O4 C1 C2 C3 0.0 . . . . ? O3 C1 C2 C3 180 . . . . ? C8 N1 C3 C2 89.9(7) 6_565 . . . ? C8 N1 C3 C2 -89.9(7) . . . . ? C1 C2 C3 N1 180 . . . . ? Cu2 O2 C4 O1 3.7(10) 5_554 . . . ? Cu2 O2 C4 C5 -178.6(5) 5_554 . . . ? Cu2 O1 C4 O2 -4.4(11) . . . . ? Cu2 O1 C4 C5 177.9(5) . . . . ? O2 C4 C5 C6 5.9(10) . . . . ? O1 C4 C5 C6 -176.2(7) . . . . ? C8 N2 C6 C5 -87.6(9) . . . . ? C7 N2 C6 C5 85.0(10) . . . . ? C4 C5 C6 N2 -164.6(6) . . . . ? C8 N2 C7 O6 174.3(10) . . . . ? C6 N2 C7 O6 2.0(15) . . . . ? C8 N2 C7 N2 -6.7(15) . . . 6_565 ? C6 N2 C7 N2 -179.0(7) . . . 6_565 ? C7 N2 C8 O7 -177.9(9) . . . . ? C6 N2 C8 O7 -5.9(11) . . . . ? C7 N2 C8 N1 3.3(12) . . . . ? C6 N2 C8 N1 175.3(7) . . . . ? C8 N1 C8 O7 -178.2(6) 6_565 . . . ? C3 N1 C8 O7 1.5(12) . . . . ? C8 N1 C8 N2 0.5(14) 6_565 . . . ? C3 N1 C8 N2 -179.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.129 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.109 #==end=== data_2 _database_code_depnum_ccdc_archive 'CCDC 823530' #TrackingRef '- revised cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H40 Cu3 N6 O26' _chemical_formula_weight 1019.24 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 23.65(3) _cell_length_b 11.709(16) _cell_length_c 12.626(17) _cell_angle_alpha 90.00 _cell_angle_beta 105.079(17) _cell_angle_gamma 90.00 _cell_volume 3376(8) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1850 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 20.50 _exptl_crystal_description Prism _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 1.003 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1042 _exptl_absorpt_coefficient_mu 0.996 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5657 _exptl_absorpt_correction_T_max 0.8049 _exptl_absorpt_process_details '(North et al., 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15791 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.0809 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 28.36 _reflns_number_total 4383 _reflns_number_gt 2206 _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^)+(0.1283P)^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 4383 _refine_ls_number_parameters 157 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1262 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.2200 _refine_ls_wR_factor_gt 0.1972 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.926 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 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 Cu2 Cu 0.01353(3) 0.0000 0.90544(6) 0.0472(3) Uani 1 2 d S . . Cu1 Cu 0.0000 0.0000 0.5000 0.1043(7) Uani 1 4 d S . . O1 O 0.02711(17) 0.0000 0.7474(4) 0.0615(12) Uani 1 2 d S . . O2 O 0.0718(2) 0.0000 0.6144(4) 0.103(2) Uani 1 2 d S . . O3 O 0.42989(13) 0.3806(3) 1.0258(3) 0.0626(8) Uani 1 1 d . . . O4 O 0.45223(13) 0.3819(3) 0.8666(3) 0.0667(9) Uani 1 1 d . . . O5 O 0.23986(14) 0.1935(3) 0.8338(4) 0.0851(12) Uani 1 1 d . . . O6 O 0.3977(2) 0.0000 1.0276(5) 0.0932(19) Uani 1 2 d S . . O7 O 0.3351(10) 0.0000 0.6867(18) 0.200(9) Uani 0.50 2 d SP . . O8 O 0.2657(8) 0.5000 0.8505(16) 0.181(8) Uani 0.50 2 d SP . . O9 O 0.5090(9) 0.2166(17) 0.7261(15) 0.261(10) Uani 0.50 1 d P . . N1 N 0.23850(18) 0.0000 0.8288(5) 0.0549(14) Uani 1 2 d S . . N2 N 0.31917(14) 0.1000(3) 0.9352(3) 0.0553(10) Uani 1 1 d . . . C1 C 0.0730(3) 0.0000 0.7133(6) 0.0609(17) Uani 1 2 d S . . C2 C 0.1317(2) 0.0000 0.7967(5) 0.0616(18) Uani 1 2 d S . . H2A H 0.1345 0.0670 0.8431 0.074 Uiso 0.50 1 calc PR . . H2B H 0.1345 -0.0670 0.8431 0.074 Uiso 0.50 1 calc PR . . C3 C 0.1819(2) 0.0000 0.7446(5) 0.0595(17) Uani 1 2 d S . . H3A H 0.1795 -0.0670 0.6985 0.071 Uiso 0.50 1 calc PR . . H3B H 0.1795 0.0670 0.6985 0.071 Uiso 0.50 1 calc PR . . C4 C 0.26391(17) 0.1046(4) 0.8636(4) 0.0572(12) Uani 1 1 d . . . C5 C 0.3486(2) 0.0000 0.9709(6) 0.0611(18) Uani 1 2 d S . . C6 C 0.3495(2) 0.2086(4) 0.9713(4) 0.0636(13) Uani 1 1 d . . . H6A H 0.3758 0.1992 1.0438 0.076 Uiso 1 1 calc R . . H6B H 0.3209 0.2667 0.9759 0.076 Uiso 1 1 calc R . . C7 C 0.3837(2) 0.2465(4) 0.8921(4) 0.0672(13) Uani 1 1 d . . . H7A H 0.3562 0.2679 0.8236 0.081 Uiso 1 1 calc R . . H7B H 0.4061 0.1820 0.8770 0.081 Uiso 1 1 calc R . . C8 C 0.42502(17) 0.3451(4) 0.9305(4) 0.0532(11) Uani 1 1 d . . . O10 O 0.0000 0.1627(10) 0.5000 0.350(12) Uani 1 2 d S . . 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 Cu2 0.0306(4) 0.0394(4) 0.0677(5) 0.000 0.0055(3) 0.000 Cu1 0.0525(8) 0.200(2) 0.0499(8) 0.000 -0.0058(6) 0.000 O1 0.034(2) 0.081(3) 0.067(3) 0.000 0.008(2) 0.000 O2 0.051(3) 0.208(7) 0.045(3) 0.000 0.000(2) 0.000 O3 0.0510(18) 0.0514(18) 0.087(2) -0.0092(17) 0.0197(17) -0.0140(14) O4 0.0532(18) 0.070(2) 0.076(2) -0.0116(18) 0.0151(17) -0.0225(16) O5 0.0507(19) 0.0480(19) 0.144(4) 0.014(2) 0.003(2) 0.0100(15) O6 0.039(3) 0.078(3) 0.136(5) 0.000 -0.023(3) 0.000 O7 0.26(2) 0.181(18) 0.21(2) 0.000 0.169(19) 0.000 O8 0.169(17) 0.130(14) 0.20(2) 0.000 -0.021(15) 0.000 O9 0.36(3) 0.208(17) 0.240(17) -0.114(14) 0.125(18) -0.080(17) N1 0.023(2) 0.045(3) 0.089(4) 0.000 0.000(2) 0.000 N2 0.0312(16) 0.0420(19) 0.084(3) -0.0041(18) 0.0006(17) -0.0075(14) C1 0.036(3) 0.075(4) 0.063(5) 0.000 -0.004(3) 0.000 C2 0.032(3) 0.086(5) 0.058(4) 0.000 -0.004(3) 0.000 C3 0.033(3) 0.074(4) 0.065(4) 0.000 0.001(3) 0.000 C4 0.036(2) 0.043(2) 0.089(4) 0.001(2) 0.011(2) 0.0010(18) C5 0.030(3) 0.055(4) 0.091(5) 0.000 0.004(3) 0.000 C6 0.051(2) 0.046(2) 0.091(4) -0.011(2) 0.013(2) -0.011(2) C7 0.055(3) 0.054(3) 0.090(4) -0.017(3) 0.013(3) -0.023(2) C8 0.036(2) 0.043(2) 0.077(3) -0.008(2) 0.007(2) 0.0021(18) O10 0.377(19) 0.133(9) 0.352(19) 0.000 -0.240(16) 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. ; 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 Cu2 O4 1.971(4) 3_445 ? Cu2 O4 1.971(4) 8_455 ? Cu2 O3 1.973(3) 7_557 ? Cu2 O3 1.973(3) 4_547 ? Cu2 O1 2.102(5) . ? Cu2 Cu2 2.628(4) 5_557 ? Cu1 O10 1.905(12) 5_556 ? Cu1 O10 1.905(12) . ? Cu1 O2 1.921(5) 5_556 ? Cu1 O2 1.921(5) . ? O1 C1 1.267(8) . ? O2 C1 1.242(8) . ? O3 C8 1.249(6) . ? O3 Cu2 1.973(3) 7_557 ? O4 C8 1.234(6) . ? O4 Cu2 1.971(4) 3 ? O5 C4 1.199(5) . ? O6 C5 1.195(7) . ? N1 C4 1.385(5) . ? N1 C4 1.385(5) 6 ? N1 C3 1.476(7) . ? N2 C5 1.377(5) . ? N2 C4 1.383(5) . ? N2 C6 1.473(5) . ? C1 C2 1.509(8) . ? C2 C3 1.501(9) . ? C5 N2 1.377(5) 6 ? C6 C7 1.508(7) . ? C7 C8 1.509(6) . ? 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 O4 Cu2 O4 89.1(2) 3_445 8_455 ? O4 Cu2 O3 167.73(14) 3_445 7_557 ? O4 Cu2 O3 89.05(18) 8_455 7_557 ? O4 Cu2 O3 89.05(18) 3_445 4_547 ? O4 Cu2 O3 167.73(14) 8_455 4_547 ? O3 Cu2 O3 90.2(2) 7_557 4_547 ? O4 Cu2 O1 92.75(14) 3_445 . ? O4 Cu2 O1 92.75(14) 8_455 . ? O3 Cu2 O1 99.46(14) 7_557 . ? O3 Cu2 O1 99.46(14) 4_547 . ? O4 Cu2 Cu2 83.62(11) 3_445 5_557 ? O4 Cu2 Cu2 83.62(11) 8_455 5_557 ? O3 Cu2 Cu2 84.12(12) 7_557 5_557 ? O3 Cu2 Cu2 84.12(12) 4_547 5_557 ? O1 Cu2 Cu2 174.88(12) . 5_557 ? O10 Cu1 O10 180 5_556 . ? O10 Cu1 O2 90 5_556 5_556 ? O10 Cu1 O2 90 . 5_556 ? O10 Cu1 O2 90 5_556 . ? O10 Cu1 O2 90 . . ? O2 Cu1 O2 180 5_556 . ? C1 O1 Cu2 132.7(4) . . ? C1 O2 Cu1 122.7(5) . . ? C8 O3 Cu2 122.8(3) . 7_557 ? C8 O4 Cu2 123.9(3) . 3 ? C4 N1 C4 124.4(5) . 6 ? C4 N1 C3 117.8(3) . . ? C4 N1 C3 117.8(3) 6 . ? C5 N2 C4 124.0(4) . . ? C5 N2 C6 118.0(4) . . ? C4 N2 C6 118.0(3) . . ? O2 C1 O1 123.0(6) . . ? O2 C1 C2 118.6(6) . . ? O1 C1 C2 118.4(6) . . ? C3 C2 C1 112.5(6) . . ? N1 C3 C2 110.9(5) . . ? O5 C4 N2 122.0(4) . . ? O5 C4 N1 122.5(4) . . ? N2 C4 N1 115.5(4) . . ? O6 C5 N2 121.7(2) . 6 ? O6 C5 N2 121.7(2) . . ? N2 C5 N2 116.5(5) 6 . ? N2 C6 C7 110.5(4) . . ? C6 C7 C8 115.2(4) . . ? O4 C8 O3 125.5(4) . . ? O4 C8 C7 117.5(5) . . ? O3 C8 C7 117.0(4) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.530 -0.030 0.482 1472 191 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.926 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.099