# 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_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Qingming Wang' 'Liping Lu' 'Miaoli Zhu' 'Caixia Yuan' _publ_contact_author_name 'Prof Dr Miaoli Zhu' _publ_contact_author_email miaoli@sxu.edu.cn data_826911 _database_code_depnum_ccdc_archive 'CCDC 826911' #TrackingRef '- CCDC826911.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H56 Cu2 N4 O16 P4, 2(C H4 O), H2 O ' _chemical_formula_sum 'C42 H66 Cu2 N4 O19 P4' _chemical_formula_weight 1181.95 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.708(2) _cell_length_b 11.614(3) _cell_length_c 14.477(4) _cell_angle_alpha 99.471(4) _cell_angle_beta 104.719(4) _cell_angle_gamma 102.425(3) _cell_volume 1499.6(6) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1366 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 20.73 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 0.882 _exptl_absorpt_correction_T_min 0.8434 _exptl_absorpt_correction_T_max 0.9170 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS; Sheldrick, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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, Bruker' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9442 _diffrn_reflns_av_R_equivalents 0.0825 _diffrn_reflns_av_sigmaI/netI 0.1329 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5202 _reflns_number_gt 2654 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker,2000)' _computing_cell_refinement 'SAINT (Bruker,2000)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1999)' _computing_publication_material SHELXTL/PC _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^)+(0.1237P)^2^] 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 5202 _refine_ls_number_parameters 340 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.1551 _refine_ls_R_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.2503 _refine_ls_wR_factor_gt 0.2002 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.026 _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 0.40687(10) 0.26657(8) 0.42505(6) 0.0614(4) Uani 1 1 d . . . N1 N 0.4161(7) 0.2798(6) 0.5693(4) 0.0709(17) Uani 1 1 d . . . H1A H 0.4578 0.2209 0.5878 0.085 Uiso 1 1 calc R . . N2 N 0.2003(7) 0.1511(5) 0.3965(4) 0.0668(17) Uani 1 1 d . A . H2A H 0.1362 0.1918 0.3694 0.080 Uiso 1 1 calc R . . O1 O 0.6116(6) 0.3767(5) 0.4681(4) 0.0744(14) Uani 1 1 d . . . O2 O 0.7126(6) 0.5847(4) 0.5979(4) 0.0807(16) Uani 1 1 d . . . O3 O 0.8132(7) 0.4031(5) 0.6290(5) 0.0896(18) Uani 1 1 d . . . O4 O 0.6246(8) 0.2043(5) 0.7232(4) 0.0863(17) Uani 1 1 d . . . H4A H 0.6483 0.1559 0.7553 0.129 Uiso 1 1 calc R . . O5 O 0.4060(6) 0.1903(5) 0.2887(4) 0.0716(14) Uani 1 1 d . . . O6 O 0.3071(7) -0.0308(5) 0.1842(4) 0.0879(17) Uani 1 1 d . . . O7 O 0.1663(9) 0.1242(8) 0.1500(6) 0.130(3) Uani 1 1 d DU . . O8 O -0.0998(7) 0.1331(6) 0.2771(6) 0.102(2) Uani 1 1 d . A . H8 H -0.1779 0.1491 0.2541 0.153 Uiso 1 1 calc R . . P1 P 0.6722(2) 0.44764(17) 0.57757(15) 0.0623(6) Uani 1 1 d . . . P2 P 0.2719(2) 0.08174(17) 0.22887(14) 0.0605(6) Uani 1 1 d . A . C1 C 0.6311(8) 0.3114(7) 0.7867(5) 0.0630(19) Uani 1 1 d . . . C2 C 0.6875(9) 0.3289(7) 0.8903(6) 0.074(2) Uani 1 1 d . . . H2 H 0.7272 0.2713 0.9168 0.089 Uiso 1 1 calc R . . C3 C 0.6830(12) 0.4342(9) 0.9524(7) 0.099(3) Uani 1 1 d . . . H3 H 0.7186 0.4457 1.0202 0.119 Uiso 1 1 calc R . . C4 C 0.6246(15) 0.5218(9) 0.9116(8) 0.117(4) Uani 1 1 d . . . H4 H 0.6221 0.5912 0.9530 0.140 Uiso 1 1 calc R . . C5 C 0.5712(12) 0.5066(8) 0.8119(8) 0.096(3) Uani 1 1 d . . . H5A H 0.5323 0.5655 0.7869 0.115 Uiso 1 1 calc R . . C6 C 0.5742(9) 0.4011(7) 0.7447(5) 0.071(2) Uani 1 1 d . . . C7 C 0.5179(9) 0.3959(7) 0.6336(6) 0.071(2) Uani 1 1 d . . . H7 H 0.4603 0.4555 0.6284 0.086 Uiso 1 1 calc R . . C8 C 0.9383(14) 0.4844(12) 0.7113(11) 0.134(4) Uani 1 1 d DU . . H8A H 0.9134 0.5586 0.7334 0.161 Uiso 1 1 calc R . . H8B H 0.9569 0.4454 0.7658 0.161 Uiso 1 1 calc R . . C9 C 1.0666(19) 0.5122(18) 0.6811(14) 0.211(8) Uani 1 1 d DU . . H9A H 1.0921 0.4388 0.6604 0.316 Uiso 1 1 calc R . . H9B H 1.1469 0.5653 0.7350 0.316 Uiso 1 1 calc R . . H9C H 1.0482 0.5514 0.6275 0.316 Uiso 1 1 calc R . . C10 C 0.2612(9) 0.2435(8) 0.5742(6) 0.077(2) Uani 1 1 d . . . H10A H 0.2179 0.3111 0.5701 0.092 Uiso 1 1 calc R . . H10B H 0.2623 0.2230 0.6367 0.092 Uiso 1 1 calc R . . C11 C 0.1691(9) 0.1369(8) 0.4921(6) 0.082(3) Uani 1 1 d . . . H11A H 0.0652 0.1294 0.4846 0.099 Uiso 1 1 calc R . . H11B H 0.1907 0.0634 0.5079 0.099 Uiso 1 1 calc R . . C12 C 0.1698(10) 0.0394(7) 0.3206(6) 0.077(2) Uani 1 1 d . . . H12 H 0.2209 -0.0134 0.3539 0.092 Uiso 1 1 calc R A . C13 C 0.0078(9) -0.0395(8) 0.2690(6) 0.071(2) Uani 1 1 d . A . C14 C -0.1187(10) 0.0073(8) 0.2475(6) 0.079(2) Uani 1 1 d . . . C15 C -0.2652(10) -0.0749(9) 0.1950(6) 0.086(3) Uani 1 1 d . A . H15 H -0.3485 -0.0459 0.1816 0.104 Uiso 1 1 calc R . . C16 C -0.2767(12) -0.1987(9) 0.1655(6) 0.085(3) Uani 1 1 d . . . H16 H -0.3691 -0.2519 0.1315 0.102 Uiso 1 1 calc R A . C17 C -0.1559(11) -0.2432(9) 0.1852(6) 0.084(3) Uani 1 1 d . A . H17 H -0.1670 -0.3254 0.1625 0.101 Uiso 1 1 calc R . . C18 C -0.0157(10) -0.1670(8) 0.2389(6) 0.084(2) Uani 1 1 d . . . H18 H 0.0636 -0.2004 0.2554 0.100 Uiso 1 1 calc R A . C19A C 0.067(2) 0.1117(17) 0.0570(11) 0.120(10) Uani 0.51(2) 1 d PDU A 1 H19A H 0.0018 0.0312 0.0254 0.120 Uiso 0.51(2) 1 d PR A 1 H19B H 0.1348 0.1288 0.0189 0.120 Uiso 0.51(2) 1 d PR A 1 C19B C 0.138(2) 0.2276(14) 0.1208(18) 0.136(12) Uani 0.49(2) 1 d PDU A 2 H19C H 0.2202 0.2756 0.1051 0.136 Uiso 0.49(2) 1 d PR A 2 H19D H 0.1285 0.2748 0.1796 0.136 Uiso 0.49(2) 1 d PR A 2 C20 C -0.0003(15) 0.2094(13) 0.0480(10) 0.143(5) Uani 1 1 d DU . . H20A H -0.0973 0.1715 0.0501 0.215 Uiso 1 1 d R A . H20B H -0.0076 0.2326 -0.0133 0.215 Uiso 1 1 d R . . H20C H 0.0444 0.2800 0.1011 0.215 Uiso 1 1 d R . . C21 C 0.5690(15) 0.1797(13) 0.1018(10) 0.139(5) Uani 1 1 d . . . H21A H 0.4778 0.2023 0.0925 0.209 Uiso 1 1 calc R . . H21B H 0.5484 0.0946 0.0742 0.209 Uiso 1 1 calc R . . H21C H 0.6297 0.2248 0.0698 0.209 Uiso 1 1 calc R . . O9 O 0.6472(8) 0.2065(8) 0.2072(6) 0.118(2) Uani 1 1 d . . . H9 H 0.5876 0.2074 0.2384 0.177 Uiso 1 1 calc R . . O10 O 0.744(3) 0.142(2) 0.4652(19) 0.202(9) Uani 0.50 1 d PU . . H10C H 0.7017 0.1832 0.4294 0.303 Uiso 0.50 1 d PR . . H10D H 0.7918 0.1890 0.5210 0.303 Uiso 0.50 1 d PR . . 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 0.0578(6) 0.0533(6) 0.0610(6) 0.0038(4) 0.0150(4) 0.0006(4) N1 0.063(4) 0.064(4) 0.069(4) -0.004(3) 0.012(3) 0.008(3) N2 0.079(4) 0.056(3) 0.046(3) 0.002(3) 0.011(3) -0.005(3) O1 0.063(4) 0.074(3) 0.078(4) 0.011(3) 0.019(3) 0.010(3) O2 0.071(4) 0.042(3) 0.121(5) 0.012(3) 0.025(3) 0.008(2) O3 0.071(4) 0.070(4) 0.110(5) 0.018(3) -0.001(3) 0.018(3) O4 0.108(5) 0.073(4) 0.080(4) 0.012(3) 0.034(4) 0.025(3) O5 0.069(4) 0.063(3) 0.075(3) 0.000(2) 0.029(3) 0.005(3) O6 0.102(5) 0.056(3) 0.107(4) 0.006(3) 0.047(4) 0.017(3) O7 0.119(5) 0.154(6) 0.130(5) 0.071(5) 0.031(4) 0.046(5) O8 0.079(4) 0.073(4) 0.137(6) 0.011(4) 0.020(4) 0.011(3) P1 0.0586(13) 0.0460(10) 0.0722(13) 0.0127(9) 0.0094(10) 0.0061(9) P2 0.0597(13) 0.0551(11) 0.0579(11) 0.0041(8) 0.0137(10) 0.0085(9) C1 0.065(5) 0.058(4) 0.056(4) 0.004(3) 0.014(4) 0.007(4) C2 0.075(6) 0.061(5) 0.078(5) 0.017(4) 0.014(4) 0.012(4) C3 0.125(9) 0.094(7) 0.060(5) -0.002(5) 0.009(5) 0.027(6) C4 0.182(12) 0.077(6) 0.088(7) -0.008(5) 0.037(7) 0.054(8) C5 0.112(8) 0.076(6) 0.097(7) 0.017(5) 0.017(6) 0.038(6) C6 0.068(5) 0.068(5) 0.060(5) 0.013(4) 0.008(4) 0.000(4) C7 0.075(6) 0.053(4) 0.069(5) 0.006(4) 0.010(4) 0.003(4) C8 0.107(7) 0.126(8) 0.164(8) 0.030(6) 0.015(6) 0.054(6) C9 0.200(11) 0.210(11) 0.223(11) 0.039(8) 0.075(9) 0.051(9) C10 0.068(6) 0.080(6) 0.070(5) 0.011(4) 0.023(4) -0.004(4) C11 0.068(6) 0.088(6) 0.070(5) -0.006(4) 0.025(4) -0.011(4) C12 0.081(6) 0.068(5) 0.079(5) 0.014(4) 0.032(5) 0.010(4) C13 0.045(5) 0.087(6) 0.070(5) 0.009(4) 0.016(4) 0.000(4) C14 0.082(7) 0.079(6) 0.064(5) 0.010(4) 0.023(5) 0.000(5) C15 0.059(6) 0.098(7) 0.087(6) 0.021(5) 0.016(5) -0.005(5) C16 0.082(7) 0.080(6) 0.065(5) 0.006(4) 0.018(5) -0.022(5) C17 0.068(6) 0.081(6) 0.086(6) 0.005(5) 0.021(5) -0.003(5) C18 0.078(6) 0.077(6) 0.088(6) 0.004(4) 0.027(5) 0.014(5) C19A 0.130(13) 0.113(13) 0.109(12) 0.015(8) 0.034(9) 0.030(9) C19B 0.134(14) 0.115(14) 0.144(14) 0.026(9) 0.021(9) 0.034(9) C20 0.145(8) 0.150(8) 0.135(8) 0.047(7) 0.009(6) 0.066(7) C21 0.147(12) 0.169(13) 0.141(11) 0.070(10) 0.080(10) 0.056(10) O9 0.101(5) 0.118(6) 0.140(7) 0.033(5) 0.046(5) 0.022(5) O10 0.218(12) 0.179(11) 0.228(12) 0.047(9) 0.062(9) 0.098(9) _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 O1 1.997(5) . ? Cu1 O5 2.024(5) . ? Cu1 N1 2.046(6) . ? Cu1 N2 2.057(6) . ? Cu1 O2 2.301(5) 2_666 ? N1 C7 1.486(9) . ? N1 C10 1.495(10) . ? N1 H1A 0.9100 . ? N2 C12 1.476(9) . ? N2 C11 1.517(9) . ? N2 H2A 0.9100 . ? O1 P1 1.557(6) . ? O2 P1 1.514(5) . ? O2 Cu1 2.301(5) 2_666 ? O3 C8 1.480(13) . ? O3 P1 1.615(6) . ? O4 C1 1.398(8) . ? O4 H4A 0.8200 . ? O5 P2 1.547(5) . ? O6 P2 1.507(6) . ? O7 C19B 1.395(10) . ? O7 C19A 1.406(9) . ? O7 P2 1.551(8) . ? O8 C14 1.411(10) . ? O8 H8 0.8200 . ? P1 C7 1.912(8) . ? P2 C12 1.914(8) . ? C1 C2 1.423(10) . ? C1 C6 1.430(11) . ? C2 C3 1.409(12) . ? C2 H2 0.9300 . ? C3 C4 1.408(14) . ? C3 H3 0.9300 . ? C4 C5 1.371(13) . ? C4 H4 0.9300 . ? C5 C6 1.444(12) . ? C5 H5A 0.9300 . ? C6 C7 1.548(10) . ? C7 H7 0.9800 . ? C8 C9 1.413(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.499(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.558(11) . ? C12 H12 0.9800 . ? C13 C18 1.424(12) . ? C13 C14 1.431(12) . ? C14 C15 1.462(11) . ? C15 C16 1.403(13) . ? C15 H15 0.9300 . ? C16 C17 1.365(13) . ? C16 H16 0.9300 . ? C17 C18 1.399(11) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19A C20 1.434(10) . ? C19A H19A 0.9700 . ? C19A H19B 0.9700 . ? C19B C20 1.430(10) . ? C19B H19C 0.9700 . ? C19B H19D 0.9700 . ? C19B H20C 1.2002 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 O9 1.468(13) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? O9 H9 0.8200 . ? O10 H10C 0.8500 . ? O10 H10D 0.8500 . ? 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 Cu1 O5 97.0(2) . . ? O1 Cu1 N1 89.1(2) . . ? O5 Cu1 N1 158.0(3) . . ? O1 Cu1 N2 173.7(2) . . ? O5 Cu1 N2 88.1(2) . . ? N1 Cu1 N2 84.7(2) . . ? O1 Cu1 O2 96.0(2) . 2_666 ? O5 Cu1 O2 104.3(2) . 2_666 ? N1 Cu1 O2 95.9(3) . 2_666 ? N2 Cu1 O2 86.2(2) . 2_666 ? C7 N1 C10 118.9(6) . . ? C7 N1 Cu1 112.2(5) . . ? C10 N1 Cu1 108.0(5) . . ? C7 N1 H1A 105.5 . . ? C10 N1 H1A 105.5 . . ? Cu1 N1 H1A 105.5 . . ? C12 N2 C11 117.3(6) . . ? C12 N2 Cu1 113.7(5) . . ? C11 N2 Cu1 109.9(4) . . ? C12 N2 H2A 104.9 . . ? C11 N2 H2A 104.9 . . ? Cu1 N2 H2A 104.9 . . ? P1 O1 Cu1 116.5(3) . . ? P1 O2 Cu1 137.6(3) . 2_666 ? C8 O3 P1 121.8(6) . . ? C1 O4 H4A 109.5 . . ? P2 O5 Cu1 116.5(3) . . ? C19B O7 C19A 60.8(11) . . ? C19B O7 P2 142.6(10) . . ? C19A O7 P2 154.9(9) . . ? C14 O8 H8 109.5 . . ? O2 P1 O1 117.3(3) . . ? O2 P1 O3 110.1(3) . . ? O1 P1 O3 107.4(3) . . ? O2 P1 C7 108.0(3) . . ? O1 P1 C7 105.2(3) . . ? O3 P1 C7 108.5(4) . . ? O6 P2 O5 116.3(3) . . ? O6 P2 O7 111.1(4) . . ? O5 P2 O7 109.3(4) . . ? O6 P2 C12 107.0(3) . . ? O5 P2 C12 105.3(3) . . ? O7 P2 C12 107.4(4) . . ? O4 C1 C2 121.1(7) . . ? O4 C1 C6 118.1(6) . . ? C2 C1 C6 120.8(7) . . ? C3 C2 C1 119.6(8) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 119.8(8) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 121.1(9) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 121.4(9) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C1 C6 C5 117.1(7) . . ? C1 C6 C7 125.7(7) . . ? C5 C6 C7 117.2(8) . . ? N1 C7 C6 117.1(6) . . ? N1 C7 P1 108.7(5) . . ? C6 C7 P1 113.7(5) . . ? N1 C7 H7 105.4 . . ? C6 C7 H7 105.4 . . ? P1 C7 H7 105.4 . . ? C9 C8 O3 110.2(14) . . ? C9 C8 H8A 109.6 . . ? O3 C8 H8A 109.6 . . ? C9 C8 H8B 109.6 . . ? O3 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 110.7(7) . . ? N1 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C10 C11 N2 110.9(6) . . ? C10 C11 H11A 109.5 . . ? N2 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 108.0 . . ? N2 C12 C13 120.2(7) . . ? N2 C12 P2 106.8(5) . . ? C13 C12 P2 112.4(5) . . ? N2 C12 H12 105.4 . . ? C13 C12 H12 105.4 . . ? P2 C12 H12 105.4 . . ? C18 C13 C14 117.6(7) . . ? C18 C13 C12 117.7(8) . . ? C14 C13 C12 124.7(8) . . ? O8 C14 C13 119.2(7) . . ? O8 C14 C15 120.8(9) . . ? C13 C14 C15 120.0(8) . . ? C16 C15 C14 118.3(9) . . ? C16 C15 H15 120.9 . . ? C14 C15 H15 120.9 . . ? C17 C16 C15 121.7(8) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 121.0(9) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C17 C18 C13 121.3(9) . . ? C17 C18 H18 119.4 . . ? C13 C18 H18 119.4 . . ? O7 C19A C20 114.9(11) . . ? O7 C19A H19A 116.2 . . ? C20 C19A H19A 115.3 . . ? O7 C19A H19B 101.0 . . ? C20 C19A H19B 99.5 . . ? H19A C19A H19B 106.8 . . ? O7 C19B C20 115.8(12) . . ? O7 C19B H19C 112.9 . . ? C20 C19B H19C 112.4 . . ? O7 C19B H19D 102.9 . . ? C20 C19B H19D 104.3 . . ? H19C C19B H19D 107.3 . . ? O7 C19B H20C 143.9 . . ? H19C C19B H20C 103.1 . . ? H19D C19B H20C 68.6 . . ? C19B C20 C19A 59.4(11) . . ? C19B C20 H20A 127.7 . . ? C19A C20 H20A 100.0 . . ? C19B C20 H20B 122.8 . . ? C19A C20 H20B 113.4 . . ? H20A C20 H20B 109.5 . . ? C19B C20 H20C 56.3 . . ? C19A C20 H20C 114.6 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O9 C21 H21A 109.5 . . ? O9 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O9 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C21 O9 H9 109.5 . . ? H10C O10 H10D 107.7 . . ? 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 Cu1 N1 C7 27.2(6) . . . . ? O5 Cu1 N1 C7 134.0(6) . . . . ? N2 Cu1 N1 C7 -154.4(6) . . . . ? O2 Cu1 N1 C7 -68.7(6) 2_666 . . . ? O1 Cu1 N1 C10 160.3(5) . . . . ? O5 Cu1 N1 C10 -92.9(8) . . . . ? N2 Cu1 N1 C10 -21.3(5) . . . . ? O2 Cu1 N1 C10 64.4(5) 2_666 . . . ? O5 Cu1 N2 C12 24.3(5) . . . . ? N1 Cu1 N2 C12 -134.8(6) . . . . ? O2 Cu1 N2 C12 128.8(5) 2_666 . . . ? O5 Cu1 N2 C11 158.1(6) . . . . ? N1 Cu1 N2 C11 -1.0(5) . . . . ? O2 Cu1 N2 C11 -97.4(6) 2_666 . . . ? O5 Cu1 O1 P1 -173.3(3) . . . . ? N1 Cu1 O1 P1 -14.5(4) . . . . ? O2 Cu1 O1 P1 81.4(4) 2_666 . . . ? O1 Cu1 O5 P2 171.9(3) . . . . ? N1 Cu1 O5 P2 66.5(7) . . . . ? N2 Cu1 O5 P2 -4.5(4) . . . . ? O2 Cu1 O5 P2 -90.1(3) 2_666 . . . ? Cu1 O2 P1 O1 65.2(6) 2_666 . . . ? Cu1 O2 P1 O3 -171.6(5) 2_666 . . . ? Cu1 O2 P1 C7 -53.2(6) 2_666 . . . ? Cu1 O1 P1 O2 -118.7(4) . . . . ? Cu1 O1 P1 O3 116.7(4) . . . . ? Cu1 O1 P1 C7 1.2(4) . . . . ? C8 O3 P1 O2 20.7(9) . . . . ? C8 O3 P1 O1 149.4(8) . . . . ? C8 O3 P1 C7 -97.3(9) . . . . ? Cu1 O5 P2 O6 -129.1(4) . . . . ? Cu1 O5 P2 O7 104.1(4) . . . . ? Cu1 O5 P2 C12 -11.0(5) . . . . ? C19B O7 P2 O6 -141(2) . . . . ? C19A O7 P2 O6 13(3) . . . . ? C19B O7 P2 O5 -11(2) . . . . ? C19A O7 P2 O5 143(3) . . . . ? C19B O7 P2 C12 102(2) . . . . ? C19A O7 P2 C12 -104(3) . . . . ? O4 C1 C2 C3 -175.6(8) . . . . ? C6 C1 C2 C3 2.0(12) . . . . ? C1 C2 C3 C4 -0.8(15) . . . . ? C2 C3 C4 C5 0.2(18) . . . . ? C3 C4 C5 C6 -0.7(18) . . . . ? O4 C1 C6 C5 175.2(7) . . . . ? C2 C1 C6 C5 -2.5(12) . . . . ? O4 C1 C6 C7 -5.8(12) . . . . ? C2 C1 C6 C7 176.4(7) . . . . ? C4 C5 C6 C1 1.8(14) . . . . ? C4 C5 C6 C7 -177.2(10) . . . . ? C10 N1 C7 C6 71.8(10) . . . . ? Cu1 N1 C7 C6 -160.7(6) . . . . ? C10 N1 C7 P1 -157.6(6) . . . . ? Cu1 N1 C7 P1 -30.2(7) . . . . ? C1 C6 C7 N1 46.6(11) . . . . ? C5 C6 C7 N1 -134.4(8) . . . . ? C1 C6 C7 P1 -81.6(8) . . . . ? C5 C6 C7 P1 97.4(8) . . . . ? O2 P1 C7 N1 144.8(5) . . . . ? O1 P1 C7 N1 18.9(6) . . . . ? O3 P1 C7 N1 -95.9(6) . . . . ? O2 P1 C7 C6 -82.8(6) . . . . ? O1 P1 C7 C6 151.3(5) . . . . ? O3 P1 C7 C6 36.5(6) . . . . ? P1 O3 C8 C9 -112.0(12) . . . . ? C7 N1 C10 C11 169.7(7) . . . . ? Cu1 N1 C10 C11 40.3(8) . . . . ? N1 C10 C11 N2 -42.5(10) . . . . ? C12 N2 C11 C10 155.5(8) . . . . ? Cu1 N2 C11 C10 23.5(9) . . . . ? C11 N2 C12 C13 67.1(10) . . . . ? Cu1 N2 C12 C13 -162.6(6) . . . . ? C11 N2 C12 P2 -163.3(6) . . . . ? Cu1 N2 C12 P2 -33.1(7) . . . . ? O6 P2 C12 N2 152.3(5) . . . . ? O5 P2 C12 N2 28.0(7) . . . . ? O7 P2 C12 N2 -88.3(7) . . . . ? O6 P2 C12 C13 -73.8(7) . . . . ? O5 P2 C12 C13 161.9(6) . . . . ? O7 P2 C12 C13 45.6(7) . . . . ? N2 C12 C13 C18 -147.8(8) . . . . ? P2 C12 C13 C18 85.2(8) . . . . ? N2 C12 C13 C14 33.7(11) . . . . ? P2 C12 C13 C14 -93.4(8) . . . . ? C18 C13 C14 O8 179.4(7) . . . . ? C12 C13 C14 O8 -2.1(12) . . . . ? C18 C13 C14 C15 -1.1(11) . . . . ? C12 C13 C14 C15 177.5(7) . . . . ? O8 C14 C15 C16 178.5(8) . . . . ? C13 C14 C15 C16 -1.0(12) . . . . ? C14 C15 C16 C17 0.5(12) . . . . ? C15 C16 C17 C18 2.2(13) . . . . ? C16 C17 C18 C13 -4.5(13) . . . . ? C14 C13 C18 C17 3.8(12) . . . . ? C12 C13 C18 C17 -174.8(7) . . . . ? C19B O7 C19A C20 -23.9(18) . . . . ? P2 O7 C19A C20 173.7(16) . . . . ? C19A O7 C19B C20 24.2(18) . . . . ? P2 O7 C19B C20 -168.0(11) . . . . ? O7 C19B C20 C19A -24.1(18) . . . . ? O7 C19A C20 C19B 23.7(18) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O10 H10C O1 0.85 2.61 3.25(2) 133.2 . O10 H10D O3 0.85 2.65 3.35(2) 140.9 . O9 H9 O5 0.82 2.06 2.863(9) 167.9 . O8 H8 O9 0.82 1.96 2.776(10) 173.5 1_455 O4 H4A O6 0.82 1.89 2.704(9) 173.5 2_656 N2 H2A O8 0.91 2.23 2.929(9) 133.2 . N1 H1A O4 0.91 2.27 2.991(10) 136.0 . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.782 _refine_diff_density_min -0.980 _refine_diff_density_rms 0.091