Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Peter Tasker' 'Andrew Harrison' 'David K. Henderson' 'Paul A. Lovatt' 'Andrew Parkin' 'R. Winpenny' _publ_contact_author_name 'Prof Peter Tasker' _publ_contact_author_address ; School of Chemistry University of Edinburgh West Mains Road Edinburgh EH9 3JJ UNITED KINGDOM ; _publ_contact_author_email P.A.TASKER@ED.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis, Structure and Magnetic Properties of [Cu4(Hmbpp)2(H2NC(O)NH2)2(H2O)8].4H2O. ; data_cud164 _database_code_CSD 217024 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H52 Cu4 N4 O28 P4' _chemical_formula_sum 'C20 H52 Cu4 N4 O28 P4' _chemical_formula_weight 1174.70 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' P P 0.1023 0.0942 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.9478(18) _cell_length_b 14.715(3) _cell_length_c 17.977(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.129(4) _cell_angle_gamma 90.00 _cell_volume 2075.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1020 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.0 _exptl_crystal_description rod _exptl_crystal_colour Orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.879 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 2.275 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 11629 _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 26.38 _reflns_number_total 4219 _reflns_number_gt 3825 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0468P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_reflns 4219 _refine_ls_number_parameters 321 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0249 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0665 _refine_ls_wR_factor_gt 0.0659 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.040 _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 -0.02452(3) 0.013277(14) 0.082817(12) 0.01124(7) Uani 1 1 d . . . O1 O 0.22102(19) -0.03333(10) 0.14604(9) 0.0221(3) Uani 1 1 d D . . H11 H 0.225(3) -0.0399(18) 0.1906(10) 0.037(8) Uiso 1 1 d D . . H12 H 0.311(2) -0.0154(15) 0.1389(13) 0.020(6) Uiso 1 1 d D . . C1 C -0.0998(2) -0.16627(12) 0.00344(9) 0.0127(4) Uani 1 1 d . . . O11 O -0.04870(16) -0.07795(8) 0.00066(7) 0.0142(3) Uani 1 1 d . . . C2 C -0.2657(2) -0.18596(12) 0.01596(10) 0.0145(4) Uani 1 1 d . . . C21 C -0.3814(2) -0.10983(13) 0.03026(10) 0.0163(4) Uani 1 1 d . . . H21A H -0.5016 -0.1295 0.0171 0.020 Uiso 1 1 calc R . . H21B H -0.3636 -0.0572 -0.0019 0.020 Uiso 1 1 calc R . . P2 P -0.33893(6) -0.07677(3) 0.12794(3) 0.01284(11) Uani 1 1 d . . . O21 O -0.14670(15) -0.05845(8) 0.14718(7) 0.0139(3) Uani 1 1 d . . . O22 O -0.38441(16) -0.15791(9) 0.17503(7) 0.0159(3) Uani 1 1 d . . . O23 O -0.44682(16) 0.00521(8) 0.13924(8) 0.0177(3) Uani 1 1 d . . . C3 C -0.3154(3) -0.27615(13) 0.01989(11) 0.0184(4) Uani 1 1 d . . . H3 H -0.4275 -0.2891 0.0290 0.022 Uiso 1 1 calc R . . C4 C -0.2070(3) -0.34793(13) 0.01102(11) 0.0208(4) Uani 1 1 d . . . C41 C -0.2640(3) -0.44536(15) 0.01619(14) 0.0332(5) Uani 1 1 d . . . H41A H -0.1639 -0.4849 0.0265 0.050 Uiso 0.50 1 calc PR . . H41B H -0.3334 -0.4632 -0.0316 0.050 Uiso 0.50 1 calc PR . . H41C H -0.3318 -0.4511 0.0570 0.050 Uiso 0.50 1 calc PR . . H41D H -0.3888 -0.4479 0.0081 0.050 Uiso 0.50 1 calc PR . . H41E H -0.2193 -0.4696 0.0662 0.050 Uiso 0.50 1 calc PR . . H41F H -0.2210 -0.4818 -0.0224 0.050 Uiso 0.50 1 calc PR . . C5 C -0.0445(3) -0.32697(13) -0.00233(10) 0.0195(4) Uani 1 1 d . . . H5 H 0.0314 -0.3751 -0.0089 0.023 Uiso 1 1 calc R . . C6 C 0.0111(2) -0.23746(13) -0.00640(10) 0.0150(4) Uani 1 1 d . . . C61 C 0.1856(2) -0.21710(13) -0.02382(10) 0.0164(4) Uani 1 1 d . . . H61A H 0.2628 -0.2688 -0.0079 0.020 Uiso 1 1 calc R . . H61B H 0.2321 -0.1625 0.0044 0.020 Uiso 1 1 calc R . . P6 P 0.17452(6) -0.19795(3) -0.12356(3) 0.01389(11) Uani 1 1 d . . . O61 O 0.04173(16) -0.12309(8) -0.14499(7) 0.0148(3) Uani 1 1 d . . . O62 O 0.12791(17) -0.28551(8) -0.16436(7) 0.0191(3) Uani 1 1 d . . . O63 O 0.35548(16) -0.16722(9) -0.13714(8) 0.0190(3) Uani 1 1 d . . . H63 H 0.3634 -0.1104 -0.1332 0.029 Uiso 1 1 calc R . . Cu2 Cu -0.27324(3) -0.276721(15) 0.193700(12) 0.01523(8) Uani 1 1 d . . . O2 O -0.3047(2) -0.27743(10) 0.32253(9) 0.0259(3) Uani 1 1 d D . . H21 H -0.393(3) -0.2971(18) 0.3370(15) 0.045(8) Uiso 1 1 d D . . H22 H -0.230(3) -0.3056(18) 0.3482(14) 0.049(9) Uiso 1 1 d D . . O3 O -0.04961(17) -0.21724(9) 0.20385(8) 0.0190(3) Uani 1 1 d D . . H31 H -0.069(3) -0.1616(12) 0.1933(13) 0.032(7) Uiso 1 1 d D . . H32 H -0.007(3) -0.2162(16) 0.2484(10) 0.031(7) Uiso 1 1 d D . . O4 O -0.13575(18) -0.39039(10) 0.20910(8) 0.0213(3) Uani 1 1 d D . . H41 H -0.079(3) -0.392(2) 0.2516(11) 0.053(9) Uiso 1 1 d D . . H42 H -0.186(3) -0.4410(13) 0.2035(14) 0.033(7) Uiso 1 1 d D . . N1U N -0.6958(2) -0.24936(12) 0.16470(10) 0.0238(4) Uani 1 1 d . . . H1U1 H -0.6262 -0.2028 0.1655 0.029 Uiso 1 1 calc R . . H1U2 H -0.8060 -0.2402 0.1623 0.029 Uiso 1 1 calc R . . C2U C -0.6348(2) -0.33351(13) 0.16711(10) 0.0193(4) Uani 1 1 d . . . O2U O -0.47713(16) -0.35074(9) 0.17054(8) 0.0202(3) Uani 1 1 d . . . N3U N -0.7462(2) -0.40232(12) 0.16297(11) 0.0292(4) Uani 1 1 d . . . H3U1 H -0.7100 -0.4588 0.1627 0.035 Uiso 1 1 calc R . . H3U2 H -0.8557 -0.3910 0.1606 0.035 Uiso 1 1 calc R . . O1W O -0.6227(2) -0.58865(11) 0.17649(9) 0.0312(4) Uani 1 1 d D . . H1W1 H -0.615(5) -0.616(2) 0.2182(13) 0.089(13) Uiso 1 1 d D . . H1W2 H -0.664(3) -0.6335(14) 0.1470(13) 0.041(8) Uiso 1 1 d D . . O2W O -0.2734(2) -0.55693(11) 0.19714(9) 0.0268(3) Uani 1 1 d D . . H2W1 H -0.230(4) -0.6096(15) 0.1906(18) 0.067(10) Uiso 1 1 d D . . H2W2 H -0.378(2) -0.570(2) 0.1884(18) 0.067(11) Uiso 1 1 d 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 0.01130(13) 0.01091(12) 0.01223(12) -0.00071(8) 0.00406(9) -0.00113(8) O1 0.0113(7) 0.0335(8) 0.0220(8) 0.0048(6) 0.0037(6) 0.0011(6) C1 0.0149(9) 0.0119(8) 0.0110(8) 0.0004(6) 0.0014(7) -0.0019(7) O11 0.0172(7) 0.0121(6) 0.0144(6) -0.0017(5) 0.0063(5) -0.0040(5) C2 0.0156(9) 0.0159(9) 0.0115(8) 0.0002(7) 0.0011(7) -0.0019(7) C21 0.0106(9) 0.0212(10) 0.0165(9) 0.0012(7) 0.0005(7) -0.0003(7) P2 0.0104(2) 0.0132(2) 0.0156(2) 0.00188(17) 0.00428(18) 0.00041(17) O21 0.0113(6) 0.0155(6) 0.0153(6) 0.0019(5) 0.0030(5) -0.0006(5) O22 0.0141(6) 0.0148(6) 0.0199(7) 0.0030(5) 0.0062(5) 0.0006(5) O23 0.0136(7) 0.0150(7) 0.0262(7) 0.0012(5) 0.0081(6) 0.0010(5) C3 0.0166(10) 0.0220(10) 0.0171(9) -0.0008(7) 0.0040(7) -0.0080(8) C4 0.0273(11) 0.0165(10) 0.0190(9) -0.0009(7) 0.0053(8) -0.0059(8) C41 0.0428(14) 0.0181(11) 0.0407(14) -0.0006(9) 0.0127(11) -0.0083(10) C5 0.0260(11) 0.0129(9) 0.0202(10) -0.0008(7) 0.0056(8) 0.0035(8) C6 0.0150(9) 0.0177(9) 0.0124(8) 0.0002(7) 0.0027(7) -0.0009(7) C61 0.0133(9) 0.0200(10) 0.0159(9) -0.0002(7) 0.0023(7) 0.0015(7) P6 0.0130(2) 0.0134(2) 0.0156(2) -0.00234(17) 0.00323(18) 0.00048(18) O61 0.0158(7) 0.0131(6) 0.0151(6) -0.0021(5) 0.0015(5) 0.0012(5) O62 0.0200(7) 0.0146(7) 0.0223(7) -0.0040(5) 0.0019(6) 0.0015(5) O63 0.0162(7) 0.0142(7) 0.0283(7) -0.0020(6) 0.0084(6) -0.0001(5) Cu2 0.01289(13) 0.01346(13) 0.01959(13) 0.00201(8) 0.00333(9) 0.00051(8) O2 0.0240(9) 0.0292(9) 0.0240(8) 0.0062(6) 0.0027(7) -0.0022(7) O3 0.0155(7) 0.0179(7) 0.0226(8) 0.0053(6) -0.0004(6) -0.0003(6) O4 0.0210(8) 0.0164(7) 0.0256(8) 0.0001(6) 0.0009(6) 0.0011(6) N1U 0.0162(9) 0.0178(8) 0.0388(10) 0.0007(7) 0.0085(7) -0.0001(7) C2U 0.0193(10) 0.0228(10) 0.0161(9) 0.0009(7) 0.0038(7) -0.0025(8) O2U 0.0137(7) 0.0181(7) 0.0291(7) 0.0008(6) 0.0046(5) 0.0003(5) N3U 0.0198(9) 0.0225(9) 0.0447(11) 0.0005(8) 0.0033(8) -0.0023(7) O1W 0.0407(10) 0.0235(8) 0.0295(9) 0.0005(7) 0.0060(7) -0.0024(7) O2W 0.0291(9) 0.0192(8) 0.0318(9) -0.0039(6) 0.0040(7) 0.0036(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 O21 1.9371(13) . ? Cu1 O11 1.9426(13) 3 ? Cu1 O61 1.9819(13) 3 ? Cu1 O11 1.9825(12) . ? Cu1 O1 2.2060(15) . ? O1 H11 0.803(17) . ? O1 H12 0.789(16) . ? C1 O11 1.365(2) . ? C1 C6 1.398(3) . ? C1 C2 1.402(3) . ? O11 Cu1 1.9426(13) 3 ? C2 C3 1.390(3) . ? C2 C21 1.498(3) . ? C21 P2 1.8016(18) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? P2 O23 1.5124(14) . ? P2 O21 1.5359(13) . ? P2 O22 1.5394(13) . ? O22 Cu2 1.9637(13) . ? C3 C4 1.388(3) . ? C3 H3 0.9500 . ? C4 C5 1.385(3) . ? C4 C41 1.511(3) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C41 H41D 0.9800 . ? C41 H41E 0.9800 . ? C41 H41F 0.9800 . ? C5 C6 1.395(3) . ? C5 H5 0.9500 . ? C6 C61 1.500(3) . ? C61 P6 1.8034(19) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? P6 O62 1.4997(13) . ? P6 O61 1.5319(13) . ? P6 O63 1.5633(14) . ? O61 Cu1 1.9819(13) 3 ? O63 H63 0.8400 . ? Cu2 O2U 1.9420(13) . ? Cu2 O3 1.9635(14) . ? Cu2 O4 1.9931(15) . ? Cu2 O2 2.3685(17) . ? O2 H21 0.839(17) . ? O2 H22 0.805(17) . ? O3 H31 0.848(16) . ? O3 H32 0.817(16) . ? O4 H41 0.825(17) . ? O4 H42 0.845(16) . ? N1U C2U 1.328(3) . ? N1U H1U1 0.8800 . ? N1U H1U2 0.8800 . ? C2U O2U 1.270(2) . ? C2U N3U 1.340(3) . ? N3U H3U1 0.8800 . ? N3U H3U2 0.8800 . ? O1W H1W1 0.843(18) . ? O1W H1W2 0.877(17) . ? O2W H2W1 0.864(18) . ? O2W H2W2 0.844(18) . ? 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 O21 Cu1 O11 165.56(5) . 3 ? O21 Cu1 O61 91.22(5) . 3 ? O11 Cu1 O61 95.29(5) 3 3 ? O21 Cu1 O11 94.45(5) . . ? O11 Cu1 O11 76.21(6) 3 . ? O61 Cu1 O11 164.81(5) 3 . ? O21 Cu1 O1 90.53(6) . . ? O11 Cu1 O1 101.62(6) 3 . ? O61 Cu1 O1 95.60(5) 3 . ? O11 Cu1 O1 98.43(6) . . ? Cu1 O1 H11 116.3(18) . . ? Cu1 O1 H12 124.1(17) . . ? H11 O1 H12 108(2) . . ? O11 C1 C6 120.75(16) . . ? O11 C1 C2 119.71(16) . . ? C6 C1 C2 119.54(16) . . ? C1 O11 Cu1 128.47(11) . 3 ? C1 O11 Cu1 127.71(11) . . ? Cu1 O11 Cu1 103.79(6) 3 . ? C3 C2 C1 119.21(17) . . ? C3 C2 C21 121.19(17) . . ? C1 C2 C21 119.45(16) . . ? C2 C21 P2 110.13(12) . . ? C2 C21 H21A 109.6 . . ? P2 C21 H21A 109.6 . . ? C2 C21 H21B 109.6 . . ? P2 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? O23 P2 O21 113.24(7) . . ? O23 P2 O22 110.92(8) . . ? O21 P2 O22 108.92(7) . . ? O23 P2 C21 108.89(8) . . ? O21 P2 C21 107.03(8) . . ? O22 P2 C21 107.61(8) . . ? P2 O21 Cu1 122.42(7) . . ? P2 O22 Cu2 130.23(8) . . ? C4 C3 C2 122.26(18) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C5 C4 C3 117.60(18) . . ? C5 C4 C41 121.25(19) . . ? C3 C4 C41 121.16(19) . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C4 C41 H41D 109.5 . . ? H41A C41 H41D 141.1 . . ? H41B C41 H41D 56.3 . . ? H41C C41 H41D 56.3 . . ? C4 C41 H41E 109.5 . . ? H41A C41 H41E 56.3 . . ? H41B C41 H41E 141.1 . . ? H41C C41 H41E 56.3 . . ? H41D C41 H41E 109.5 . . ? C4 C41 H41F 109.5 . . ? H41A C41 H41F 56.3 . . ? H41B C41 H41F 56.3 . . ? H41C C41 H41F 141.1 . . ? H41D C41 H41F 109.5 . . ? H41E C41 H41F 109.5 . . ? C4 C5 C6 122.08(18) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 119.30(17) . . ? C5 C6 C61 120.72(17) . . ? C1 C6 C61 119.95(16) . . ? C6 C61 P6 109.75(12) . . ? C6 C61 H61A 109.7 . . ? P6 C61 H61A 109.7 . . ? C6 C61 H61B 109.7 . . ? P6 C61 H61B 109.7 . . ? H61A C61 H61B 108.2 . . ? O62 P6 O61 112.83(7) . . ? O62 P6 O63 109.52(8) . . ? O61 P6 O63 111.53(7) . . ? O62 P6 C61 108.74(8) . . ? O61 P6 C61 106.59(8) . . ? O63 P6 C61 107.42(8) . . ? P6 O61 Cu1 123.43(7) . 3 ? P6 O63 H63 109.5 . . ? O2U Cu2 O3 169.16(6) . . ? O2U Cu2 O22 97.19(6) . . ? O3 Cu2 O22 89.72(6) . . ? O2U Cu2 O4 88.83(6) . . ? O3 Cu2 O4 83.85(6) . . ? O22 Cu2 O4 173.14(6) . . ? O2U Cu2 O2 89.61(6) . . ? O3 Cu2 O2 98.36(6) . . ? O22 Cu2 O2 93.25(5) . . ? O4 Cu2 O2 90.06(6) . . ? Cu2 O2 H21 121.9(19) . . ? Cu2 O2 H22 112(2) . . ? H21 O2 H22 103(3) . . ? Cu2 O3 H31 106.5(16) . . ? Cu2 O3 H32 109.0(18) . . ? H31 O3 H32 103(2) . . ? Cu2 O4 H41 111(2) . . ? Cu2 O4 H42 118.8(17) . . ? H41 O4 H42 106(3) . . ? C2U N1U H1U1 120.0 . . ? C2U N1U H1U2 120.0 . . ? H1U1 N1U H1U2 120.0 . . ? O2U C2U N1U 122.69(18) . . ? O2U C2U N3U 119.36(18) . . ? N1U C2U N3U 117.90(18) . . ? C2U O2U Cu2 132.97(13) . . ? C2U N3U H3U1 120.0 . . ? C2U N3U H3U2 120.0 . . ? H3U1 N3U H3U2 120.0 . . ? H1W1 O1W H1W2 99(3) . . ? H2W1 O2W H2W2 100(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.479 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.073