# 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 _publ_contact_author_name 'Kuirong Ma' _publ_contact_author_address ; Huaian 223300 ; _publ_contact_author_email kuirongma@163.com loop_ _publ_author_name 'Kuirong Ma.' 'Feng Ma.' 'Yu-Lan Zhu.' 'Lin-Juan Yu.' 'Xiao-Min Zhao.' ; Yin Yang ; 'Wei-He Duan.' # Attachment '- 1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 791852' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H40 Cu3 N8 O15 P4' _chemical_formula_sum 'C44 H40 Cu3 N8 O15 P4' _chemical_formula_weight 1235.34 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' 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 -p1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8755(13) _cell_length_b 10.5099(14) _cell_length_c 24.570(3) _cell_angle_alpha 81.129(2) _cell_angle_beta 84.708(2) _cell_angle_gamma 67.205(2) _cell_volume 2321.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5043 _cell_measurement_theta_min 0.84 _cell_measurement_theta_max 25 _exptl_crystal_description sliceblock _exptl_crystal_colour blue _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1254 _exptl_absorpt_coefficient_mu 1.581 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.678 _exptl_absorpt_correction_T_max 0.801 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _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 'SMART APEX II(Bruker, 2005)' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16530 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0818 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8102 _reflns_number_gt 5043 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART APEX II(Bruker, 2005)' _computing_cell_refinement 'SMART APEX II' _computing_data_reduction 'SMART APEX II' _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 ; '(isor 0.01 o2w') (simu 0.01 0.02 3.8 $c) (dfix 0.82 0.01 o2w h2w1 o2w h2w2)' For 1, the O(2W) is disordered and treated by adopting 25% possibility of occupancies at its sites. In additon some C atoms in 1 display the disorders, so restraints are used during the refinements. 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^)+(0.1003P)^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 8102 _refine_ls_number_parameters 687 _refine_ls_number_restraints 896 _refine_ls_R_factor_all 0.1004 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1890 _refine_ls_wR_factor_gt 0.1598 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.030 _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 Cu1 Cu 0.69949(8) 0.44475(8) 0.33936(3) 0.0306(2) Uani 1 1 d . . . Cu2 Cu 0.41912(8) 0.81542(8) 0.21518(3) 0.0340(2) Uani 1 1 d . . . Cu3 Cu 0.06878(8) 0.62685(7) 0.26863(3) 0.0324(2) Uani 1 1 d . . . P1 P 0.37285(17) 0.59929(17) 0.30614(7) 0.0284(4) Uani 1 1 d . . . P2 P 0.14295(18) 0.88097(17) 0.28710(7) 0.0335(4) Uani 1 1 d . . . P3 P 0.97389(18) 0.37338(17) 0.26684(7) 0.0293(4) Uani 1 1 d . . . P4 P -0.25277(17) 0.65808(17) 0.24688(7) 0.0313(4) Uani 1 1 d . . . N1 N 0.7115(6) 0.2773(5) 0.3958(2) 0.0339(13) Uani 1 1 d . . . N2 N 0.7793(7) -0.2665(6) 0.6064(3) 0.0548(17) Uani 1 1 d . . . H2 H 0.7884 -0.3340 0.6324 0.066 Uiso 1 1 calc R . . C19 C 0.5573(9) -0.2112(8) 0.6970(3) 0.0637(19) Uani 1 1 d U . . H19 H 0.6436 -0.2893 0.7029 0.076 Uiso 1 1 calc R . . C21 C 1.0149(8) -0.5376(7) 0.5874(3) 0.0446(15) Uani 1 1 d U . . H21 H 0.9342 -0.5424 0.6090 0.053 Uiso 1 1 calc R . . N5 N 0.4059(6) 0.9758(6) 0.1570(2) 0.0455(15) Uani 1 1 d . . . N6 N 0.3519(8) 1.5214(7) -0.0520(3) 0.0598(18) Uani 1 1 d . . . H6A H 0.3423 1.5904 -0.0773 0.072 Uiso 1 1 calc R . . C43 C 0.0888(11) 1.7739(10) -0.0485(4) 0.085(2) Uani 1 1 d U . . H43 H 0.1583 1.7728 -0.0769 0.102 Uiso 1 1 calc R . . C36 C 0.5860(8) 1.5072(7) -0.1321(3) 0.0462(15) Uani 1 1 d U . . H36 H 0.5150 1.5867 -0.1307 0.055 Uiso 1 1 d R . . O1 O 0.4917(4) 0.5051(4) 0.34541(17) 0.0366(11) Uani 1 1 d . . . O2 O 0.4332(4) 0.6270(4) 0.24808(16) 0.0316(10) Uani 1 1 d . . . O3 O 0.2516(4) 0.5437(4) 0.30759(18) 0.0344(10) Uani 1 1 d . . . O4 O 0.2095(5) 0.8989(4) 0.22970(18) 0.0395(11) Uani 1 1 d . . . O5 O 0.0358(4) 0.8085(4) 0.2904(2) 0.0422(12) Uani 1 1 d . . . O6 O 0.0703(5) 1.0206(4) 0.3103(2) 0.0501(13) Uani 1 1 d . . . O7 O 0.9052(4) 0.3639(4) 0.32472(17) 0.0336(10) Uani 1 1 d . . . O8 O 1.0365(5) 0.2310(4) 0.24562(19) 0.0425(12) Uani 1 1 d . . . O9 O 1.0877(4) 0.4382(4) 0.26194(18) 0.0347(11) Uani 1 1 d . . . O10 O -0.1305(4) 0.7136(4) 0.24304(19) 0.0392(11) Uani 1 1 d . . . O11 O 0.6904(4) 0.6328(4) 0.30571(17) 0.0321(10) Uani 1 1 d . . . O12 O 0.6271(4) 0.7550(5) 0.20803(18) 0.0390(11) Uani 1 1 d . . . O13 O 0.4062(5) 0.8345(5) 0.3180(2) 0.0437(12) Uani 1 1 d . . . H131 H 0.4852 0.7718 0.3297 0.052 Uiso 1 1 d R . . O14 O -0.2883(5) 0.4262(4) 0.2319(2) 0.0434(12) Uani 1 1 d . . . H141 H -0.3687 0.4924 0.2245 0.052 Uiso 1 1 d R . . O1W O 0.8869(12) 0.1139(14) 0.1908(4) 0.073(4) Uani 0.50 1 d P . . H1W1 H 0.9641 0.0426 0.1970 0.109 Uiso 0.50 1 d PR . . H1W2 H 0.8144 0.1633 0.1697 0.109 Uiso 0.50 1 d PR . . O2W' O 0.848(3) 0.9422(18) 0.1792(9) 0.075(9) Uani 0.25 1 d PU . . H2W1 H 0.8388 1.0141 0.1538 0.112 Uiso 0.50 1 d PRD . . H2W2 H 0.8213 0.8669 0.1721 0.112 Uiso 0.50 1 d PRD . . O2W O 0.820(3) 0.941(2) 0.1534(10) 0.080(10) Uani 0.25 1 d PD . . C22 C 1.1364(8) -0.6545(8) 0.5821(3) 0.0539(17) Uani 1 1 d U . . H22 H 1.1345 -0.7382 0.6004 0.065 Uiso 1 1 calc R . . N4 N 1.2585(7) -0.6586(7) 0.5527(3) 0.065(2) Uani 1 1 d . . . C23 C 1.2532(8) -0.5361(8) 0.5264(3) 0.0547(17) Uani 1 1 d U . . H23 H 1.3359 -0.5343 0.5054 0.066 Uiso 1 1 calc R . . C24 C 1.1341(8) -0.4113(7) 0.5280(3) 0.0465(15) Uani 1 1 d U . . H24 H 1.1365 -0.3298 0.5076 0.056 Uiso 1 1 calc R . . C20 C 1.0123(7) -0.4101(7) 0.5601(3) 0.0377(13) Uani 1 1 d U . . C13 C 0.8837(7) -0.2791(7) 0.5630(3) 0.0363(12) Uani 1 1 d U . . C14 C 0.8696(6) -0.1738(6) 0.5240(2) 0.0253(11) Uani 1 1 d U . . H14 H 0.9412 -0.1806 0.4960 0.030 Uiso 1 1 calc R . . C10 C 0.7509(7) -0.0584(7) 0.5256(3) 0.0335(12) Uani 1 1 d U . . C11 C 0.6473(6) -0.0374(6) 0.5648(2) 0.0258(12) Uani 1 1 d U . . H11 H 0.5673 0.0470 0.5639 0.031 Uiso 1 1 calc R . . C12 C 0.6598(7) -0.1400(7) 0.6057(3) 0.0359(12) Uani 1 1 d U . . C15 C 0.5421(7) -0.1153(7) 0.6495(3) 0.0385(14) Uani 1 1 d U . . C16 C 0.4154(8) -0.0004(7) 0.6450(3) 0.0469(16) Uani 1 1 d U . . H16 H 0.4029 0.0653 0.6139 0.056 Uiso 1 1 calc R . . C17 C 0.3056(9) 0.0209(8) 0.6852(3) 0.0574(18) Uani 1 1 d U . . H17 H 0.2217 0.1022 0.6819 0.069 Uiso 1 1 calc R . . N3 N 0.3190(8) -0.0719(8) 0.7277(3) 0.081(2) Uani 1 1 d . . . C18 C 0.4416(10) -0.1874(9) 0.7350(4) 0.076(2) Uani 1 1 d U . . H18 H 0.4484 -0.2520 0.7661 0.091 Uiso 1 1 calc R . . C7 C 0.7359(7) 0.0585(6) 0.4802(3) 0.0327(12) Uani 1 1 d U . . C8 C 0.8484(7) 0.0531(7) 0.4417(3) 0.0402(15) Uani 1 1 d U . . H8 H 0.9352 -0.0255 0.4434 0.048 Uiso 1 1 calc R . . C9 C 0.8338(7) 0.1622(7) 0.4011(3) 0.0390(15) Uani 1 1 d U . . H9 H 0.9122 0.1560 0.3762 0.047 Uiso 1 1 calc R . . C5 C 0.6003(7) 0.2816(7) 0.4334(3) 0.0373(14) Uani 1 1 d U . . H5 H 0.5136 0.3601 0.4304 0.045 Uiso 1 1 calc R . . C6 C 0.6081(7) 0.1789(7) 0.4750(3) 0.0371(14) Uani 1 1 d U . . H6 H 0.5290 0.1883 0.4999 0.045 Uiso 1 1 calc R . . C44 C -0.0382(12) 1.8915(11) -0.0444(5) 0.096(3) Uani 1 1 d U . . H44 H -0.0518 1.9670 -0.0716 0.116 Uiso 1 1 calc R . . N7 N -0.1380(10) 1.9047(10) -0.0062(4) 0.101(3) Uani 1 1 d . . . C40 C -0.1156(11) 1.7928(11) 0.0308(4) 0.087(2) Uani 1 1 d U . . H40 H -0.1857 1.7970 0.0592 0.104 Uiso 1 1 calc R . . C41 C 0.0064(10) 1.6707(10) 0.0294(4) 0.078(2) Uani 1 1 d U . . H41 H 0.0160 1.5956 0.0564 0.093 Uiso 1 1 calc R . . C42 C 0.1097(10) 1.6593(9) -0.0100(3) 0.0581(16) Uani 1 1 d U . . C32 C 0.2447(9) 1.5297(8) -0.0110(3) 0.0545(15) Uani 1 1 d U . . C31 C 0.2571(8) 1.4242(7) 0.0275(3) 0.0396(13) Uani 1 1 d U . . H31 H 0.1834 1.4304 0.0546 0.048 Uiso 1 1 calc R . . C30 C 0.3758(8) 1.3099(8) 0.0268(3) 0.0474(14) Uani 1 1 d U . . C34 C 0.4818(8) 1.2970(7) -0.0124(3) 0.0437(14) Uani 1 1 d U . . H34 H 0.5630 1.2137 -0.0124 0.052 Uiso 1 1 calc R . . C33 C 0.4711(8) 1.4037(8) -0.0517(3) 0.0455(14) Uani 1 1 d U . . C37 C 0.5872(8) 1.3944(7) -0.0945(3) 0.0441(14) Uani 1 1 d U . . C38 C 0.7090(8) 1.2696(8) -0.0990(3) 0.0516(16) Uani 1 1 d U . . H38 H 0.7187 1.1903 -0.0743 0.062 Uiso 1 1 calc R . . C39 C 0.8135(8) 1.2664(8) -0.1403(3) 0.0525(17) Uani 1 1 d U . . H39 H 0.8913 1.1819 -0.1433 0.063 Uiso 1 1 calc R . . N8 N 0.8112(6) 1.3752(6) -0.1763(2) 0.0416(14) Uani 1 1 d . . . C35 C 0.6990(8) 1.4928(7) -0.1716(3) 0.0436(15) Uani 1 1 d U . . H35 H 0.6951 1.5707 -0.1961 0.052 Uiso 1 1 calc R . . C27 C 0.3876(8) 1.1923(7) 0.0724(3) 0.0462(14) Uani 1 1 d U . . C26 C 0.2873(8) 1.2113(8) 0.1158(3) 0.0527(16) Uani 1 1 d U . . H26 H 0.2122 1.2978 0.1179 0.063 Uiso 1 1 calc R . . C25 C 0.2982(8) 1.1016(8) 0.1564(3) 0.0539(18) Uani 1 1 d U . . H25 H 0.2268 1.1159 0.1847 0.065 Uiso 1 1 calc R . . C29 C 0.5037(9) 0.9588(9) 0.1137(3) 0.063(2) Uani 1 1 d U . . H29 H 0.5786 0.8718 0.1124 0.076 Uiso 1 1 calc R . . C28 C 0.4985(9) 1.0627(8) 0.0719(3) 0.0617(18) Uani 1 1 d U . . H28 H 0.5693 1.0460 0.0433 0.074 Uiso 1 1 calc R . . C1 C 0.2956(7) 0.7711(7) 0.3307(3) 0.0349(16) Uani 1 1 d U . . C2 C 0.2516(8) 0.7642(8) 0.3909(3) 0.0511(19) Uani 1 1 d U . . H2A H 0.3347 0.7033 0.4120 0.077 Uiso 1 1 calc R . . H2B H 0.1742 0.7292 0.3973 0.077 Uiso 1 1 calc R . . H2C H 0.2176 0.8556 0.4018 0.077 Uiso 1 1 calc R . . C3 C -0.1777(7) 0.4880(6) 0.2224(3) 0.0311(15) Uani 1 1 d U . . C4 C -0.1253(8) 0.4967(8) 0.1620(3) 0.053(2) Uani 1 1 d U . . H4A H -0.0895 0.4058 0.1505 0.079 Uiso 1 1 calc R . . H4B H -0.0479 0.5316 0.1578 0.079 Uiso 1 1 calc R . . H4C H -0.2058 0.5583 0.1398 0.079 Uiso 1 1 calc R . . 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 0.0207(4) 0.0343(5) 0.0317(5) -0.0001(3) 0.0026(3) -0.0073(4) Cu2 0.0224(4) 0.0352(5) 0.0375(5) 0.0023(4) 0.0027(4) -0.0068(4) Cu3 0.0174(4) 0.0254(4) 0.0503(5) 0.0002(4) 0.0011(4) -0.0059(3) P1 0.0189(9) 0.0291(9) 0.0341(10) -0.0023(7) 0.0027(7) -0.0072(7) P2 0.0269(9) 0.0259(9) 0.0450(11) -0.0084(8) 0.0098(8) -0.0081(8) P3 0.0235(9) 0.0280(9) 0.0339(10) -0.0042(7) 0.0076(7) -0.0088(7) P4 0.0184(9) 0.0295(9) 0.0412(10) 0.0030(8) 0.0002(7) -0.0067(7) N1 0.026(3) 0.035(3) 0.035(3) -0.005(2) 0.008(2) -0.007(3) N2 0.053(4) 0.044(4) 0.060(4) 0.000(3) 0.006(3) -0.016(3) C19 0.052(3) 0.052(3) 0.054(3) 0.005(3) 0.021(3) 0.006(3) C21 0.040(3) 0.040(3) 0.043(3) -0.004(3) 0.004(3) -0.006(3) N5 0.031(3) 0.045(4) 0.049(4) -0.001(3) 0.011(3) -0.006(3) N6 0.070(5) 0.060(4) 0.050(4) 0.008(3) 0.002(4) -0.032(4) C43 0.081(4) 0.077(4) 0.071(4) 0.008(3) 0.002(4) -0.010(3) C36 0.051(3) 0.040(3) 0.042(3) -0.003(3) 0.007(3) -0.014(3) O1 0.023(2) 0.044(3) 0.035(3) 0.007(2) 0.000(2) -0.009(2) O2 0.024(2) 0.034(2) 0.032(2) 0.0002(19) 0.0022(19) -0.008(2) O3 0.023(2) 0.028(2) 0.049(3) -0.002(2) 0.001(2) -0.008(2) O4 0.026(3) 0.039(3) 0.044(3) -0.004(2) 0.005(2) -0.004(2) O5 0.017(2) 0.029(2) 0.076(4) -0.007(2) 0.003(2) -0.005(2) O6 0.053(3) 0.029(3) 0.058(3) -0.012(2) 0.022(3) -0.008(2) O7 0.021(2) 0.038(3) 0.034(3) 0.002(2) 0.0040(19) -0.006(2) O8 0.044(3) 0.030(3) 0.048(3) -0.010(2) 0.008(2) -0.010(2) O9 0.021(2) 0.025(2) 0.054(3) 0.000(2) 0.002(2) -0.0067(19) O10 0.020(2) 0.028(2) 0.064(3) 0.000(2) -0.003(2) -0.005(2) O11 0.022(2) 0.032(2) 0.035(3) 0.002(2) 0.0018(19) -0.006(2) O12 0.021(2) 0.047(3) 0.043(3) 0.009(2) 0.000(2) -0.012(2) O13 0.033(3) 0.041(3) 0.062(3) -0.008(2) -0.002(2) -0.018(2) O14 0.026(3) 0.035(3) 0.070(3) -0.009(2) -0.004(2) -0.010(2) O1W 0.070(8) 0.152(12) 0.031(6) -0.036(7) 0.021(5) -0.076(8) O2W' 0.072(12) 0.051(10) 0.051(11) 0.035(7) 0.025(8) 0.009(8) O2W 0.10(2) 0.079(19) 0.066(19) 0.063(15) -0.037(17) -0.054(17) C22 0.048(3) 0.045(3) 0.054(3) -0.005(3) 0.002(3) -0.004(3) N4 0.051(5) 0.054(4) 0.074(5) -0.021(4) -0.004(4) 0.004(4) C23 0.042(3) 0.054(3) 0.055(4) -0.012(3) 0.009(3) -0.005(3) C24 0.040(3) 0.046(3) 0.047(3) -0.010(3) 0.007(3) -0.010(3) C20 0.032(3) 0.038(3) 0.038(3) -0.007(2) 0.003(2) -0.008(2) C13 0.031(2) 0.039(2) 0.037(3) -0.007(2) 0.005(2) -0.012(2) C14 0.021(2) 0.029(2) 0.026(2) -0.004(2) 0.009(2) -0.012(2) C10 0.028(2) 0.038(2) 0.037(3) -0.008(2) 0.002(2) -0.014(2) C11 0.020(2) 0.025(2) 0.026(2) 0.000(2) 0.010(2) -0.005(2) C12 0.030(2) 0.033(2) 0.041(3) -0.007(2) 0.005(2) -0.009(2) C15 0.033(3) 0.035(3) 0.041(3) -0.006(2) 0.011(2) -0.008(2) C16 0.036(3) 0.042(3) 0.048(3) -0.003(3) 0.009(3) -0.002(3) C17 0.046(3) 0.052(3) 0.054(4) -0.007(3) 0.013(3) 0.000(3) N3 0.066(5) 0.075(5) 0.080(6) -0.018(5) 0.039(4) -0.008(4) C18 0.063(4) 0.066(4) 0.061(4) 0.011(3) 0.022(3) 0.003(3) C7 0.027(2) 0.034(2) 0.035(3) -0.007(2) 0.004(2) -0.009(2) C8 0.025(3) 0.042(3) 0.039(3) -0.003(2) 0.013(2) -0.001(2) C9 0.029(3) 0.036(3) 0.041(3) -0.004(3) 0.014(3) -0.004(3) C5 0.024(3) 0.038(3) 0.041(3) -0.003(3) 0.007(3) -0.004(2) C6 0.025(3) 0.041(3) 0.036(3) -0.004(2) 0.011(2) -0.005(2) C44 0.092(4) 0.081(4) 0.082(4) 0.008(4) -0.002(4) -0.003(4) N7 0.083(7) 0.094(7) 0.109(8) -0.016(6) -0.014(6) -0.011(6) C40 0.078(4) 0.081(4) 0.081(4) -0.003(4) 0.003(4) -0.013(4) C41 0.073(4) 0.074(4) 0.069(4) 0.003(3) 0.003(3) -0.014(3) C42 0.064(3) 0.060(3) 0.049(3) -0.001(3) -0.002(3) -0.024(3) C32 0.056(3) 0.060(3) 0.048(3) -0.001(3) 0.002(3) -0.025(2) C31 0.041(3) 0.046(3) 0.032(3) 0.002(2) 0.007(2) -0.021(2) C30 0.050(3) 0.051(3) 0.039(3) -0.001(2) 0.005(2) -0.020(2) C34 0.044(3) 0.046(3) 0.037(3) 0.001(2) 0.008(2) -0.017(2) C33 0.048(3) 0.047(3) 0.042(3) -0.002(2) -0.002(2) -0.020(2) C37 0.045(3) 0.046(3) 0.040(3) 0.001(3) 0.002(3) -0.018(2) C38 0.054(3) 0.046(3) 0.047(3) 0.002(3) 0.000(3) -0.014(3) C39 0.048(3) 0.051(3) 0.049(3) -0.004(3) -0.001(3) -0.009(3) N8 0.031(3) 0.037(3) 0.052(4) -0.003(3) 0.005(3) -0.010(3) C35 0.046(3) 0.044(3) 0.041(3) -0.002(3) 0.004(3) -0.020(3) C27 0.044(3) 0.046(3) 0.044(3) 0.003(2) 0.008(3) -0.018(2) C26 0.047(3) 0.046(3) 0.049(3) 0.007(3) 0.019(3) -0.009(3) C25 0.050(3) 0.045(3) 0.050(3) 0.002(3) 0.021(3) -0.008(3) C29 0.052(4) 0.054(4) 0.056(4) 0.008(3) 0.015(3) 0.001(3) C28 0.052(3) 0.061(3) 0.046(3) 0.004(3) 0.022(3) -0.003(3) C1 0.029(4) 0.036(4) 0.041(4) -0.009(3) 0.010(3) -0.015(3) C2 0.054(5) 0.052(5) 0.044(4) -0.013(4) 0.006(4) -0.015(4) C3 0.025(3) 0.032(3) 0.033(4) -0.002(3) 0.000(3) -0.008(3) C4 0.055(5) 0.059(5) 0.035(4) -0.001(4) 0.006(4) -0.015(4) _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 O7 1.897(4) . ? Cu1 O1 1.898(4) . ? Cu1 O11 1.992(4) . ? Cu1 N1 2.037(5) . ? Cu1 O14 2.665(5) 1_655 ? Cu2 O12 1.900(4) . ? Cu2 O4 1.933(4) . ? Cu2 O2 1.977(4) . ? Cu2 N5 2.005(6) . ? Cu2 O13 2.554(5) . ? Cu3 O10 1.939(4) . ? Cu3 O3 1.944(4) . ? Cu3 O9 1.950(4) 1_455 ? Cu3 O5 1.960(4) . ? Cu3 N8 2.460(6) 2_675 ? P1 O1 1.517(4) . ? P1 O3 1.518(4) . ? P1 O2 1.524(4) . ? P1 C1 1.842(6) . ? P2 O5 1.515(4) . ? P2 O4 1.516(4) . ? P2 O6 1.536(5) . ? P2 C1 1.823(7) . ? P3 O9 1.511(4) . ? P3 O7 1.524(4) . ? P3 O8 1.535(4) . ? P3 C3 1.839(6) 1_655 ? P4 O10 1.522(4) . ? P4 O11 1.524(4) 1_455 ? P4 O12 1.526(4) 1_455 ? P4 C3 1.824(6) . ? N1 C9 1.337(8) . ? N1 C5 1.360(7) . ? N2 C12 1.393(8) . ? N2 C13 1.398(8) . ? N2 H2 0.8600 . ? C19 C18 1.375(10) . ? C19 C15 1.398(9) . ? C19 H19 0.9300 . ? C21 C22 1.358(10) . ? C21 C20 1.394(9) . ? C21 H21 0.9300 . ? N5 C25 1.336(9) . ? N5 C29 1.354(9) . ? N6 C33 1.336(9) . ? N6 C32 1.379(9) . ? N6 H6A 0.8600 . ? C43 C42 1.372(11) . ? C43 C44 1.387(12) . ? C43 H43 0.9300 . ? C36 C37 1.383(9) . ? C36 C35 1.388(9) . ? C36 H36 0.8601 . ? O9 Cu3 1.950(4) 1_655 ? O11 P4 1.524(4) 1_655 ? O12 P4 1.526(4) 1_655 ? O13 C1 1.474(7) . ? O13 H131 0.8421 . ? O14 C3 1.457(7) . ? O14 H141 0.8415 . ? O1W H1W1 0.8420 . ? O1W H1W2 0.8662 . ? O2W' O2W 0.719(19) . ? O2W' H2W1 0.8841 . ? O2W' H2W2 0.9674 . ? O2W H2W1 0.8592 . ? O2W H2W2 0.8380 . ? C22 N4 1.337(9) . ? C22 H22 0.9300 . ? N4 C23 1.332(10) . ? C23 C24 1.385(9) . ? C23 H23 0.9300 . ? C24 C20 1.373(9) . ? C24 H24 0.9300 . ? C20 C13 1.475(9) . ? C13 C14 1.319(8) . ? C14 C10 1.323(8) . ? C14 H14 0.9300 . ? C10 C11 1.316(8) . ? C10 C7 1.497(8) . ? C11 C12 1.333(8) . ? C11 H11 0.9300 . ? C12 C15 1.482(8) . ? C15 C16 1.360(9) . ? C16 C17 1.373(9) . ? C16 H16 0.9300 . ? C17 N3 1.292(10) . ? C17 H17 0.9300 . ? N3 C18 1.344(10) . ? C18 H18 0.9300 . ? C7 C8 1.381(8) . ? C7 C6 1.398(9) . ? C8 C9 1.370(9) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C5 C6 1.350(9) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C44 N7 1.278(12) . ? C44 H44 0.9300 . ? N7 C40 1.328(12) . ? C40 C41 1.382(12) . ? C40 H40 0.9300 . ? C41 C42 1.323(11) . ? C41 H41 0.9300 . ? C42 C32 1.493(11) . ? C32 C31 1.316(9) . ? C31 C30 1.315(10) . ? C31 H31 0.9300 . ? C30 C34 1.337(9) . ? C30 C27 1.510(9) . ? C34 C33 1.339(9) . ? C34 H34 0.9300 . ? C33 C37 1.467(9) . ? C37 C38 1.406(10) . ? C38 C39 1.373(10) . ? C38 H38 0.9300 . ? C39 N8 1.327(9) . ? C39 H39 0.9300 . ? N8 C35 1.314(8) . ? N8 Cu3 2.460(6) 2_675 ? C35 H35 0.9300 . ? C27 C26 1.370(9) . ? C27 C28 1.379(10) . ? C26 C25 1.380(9) . ? C26 H26 0.9300 . ? C25 H25 0.9300 . ? C29 C28 1.368(10) . ? C29 H29 0.9300 . ? C28 H28 0.9300 . ? C1 C2 1.501(9) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.527(9) . ? C3 P3 1.839(6) 1_455 ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? 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 O7 Cu1 O1 169.99(19) . . ? O7 Cu1 O11 91.99(17) . . ? O1 Cu1 O11 92.41(17) . . ? O7 Cu1 N1 90.23(19) . . ? O1 Cu1 N1 88.39(19) . . ? O11 Cu1 N1 161.83(19) . . ? O1 Cu1 O14 93.87(16) . 1_655 ? O7 Cu1 O14 78.29(16) . 1_655 ? O11 Cu1 O14 77.83(15) . 1_655 ? N1 Cu1 O14 120.24(18) . 1_655 ? O12 Cu2 O4 170.5(2) . . ? O12 Cu2 O2 91.28(17) . . ? O4 Cu2 O2 93.76(17) . . ? O12 Cu2 N5 88.3(2) . . ? O4 Cu2 N5 89.8(2) . . ? O2 Cu2 N5 159.0(2) . . ? O12 Cu2 O13 94.90(17) . . ? O4 Cu2 O13 78.27(17) . . ? O2 Cu2 O13 78.43(15) . . ? N5 Cu2 O13 122.5(2) . . ? O10 Cu3 O3 169.56(18) . . ? O10 Cu3 O9 94.64(17) . 1_455 ? O3 Cu3 O9 87.27(17) . 1_455 ? O10 Cu3 O5 85.69(18) . . ? O3 Cu3 O5 90.42(18) . . ? O9 Cu3 O5 168.53(18) 1_455 . ? O10 Cu3 N8 95.59(19) . 2_675 ? O3 Cu3 N8 94.79(18) . 2_675 ? O9 Cu3 N8 85.67(18) 1_455 2_675 ? O5 Cu3 N8 105.72(19) . 2_675 ? O1 P1 O3 110.2(2) . . ? O1 P1 O2 113.0(2) . . ? O3 P1 O2 113.3(2) . . ? O1 P1 C1 106.9(3) . . ? O3 P1 C1 108.7(3) . . ? O2 P1 C1 104.4(3) . . ? O5 P2 O4 113.5(3) . . ? O5 P2 O6 110.4(3) . . ? O4 P2 O6 111.5(3) . . ? O5 P2 C1 107.5(3) . . ? O4 P2 C1 106.2(3) . . ? O6 P2 C1 107.4(3) . . ? O9 P3 O7 113.5(3) . . ? O9 P3 O8 111.2(2) . . ? O7 P3 O8 111.3(2) . . ? O9 P3 C3 107.5(3) . 1_655 ? O7 P3 C3 105.8(3) . 1_655 ? O8 P3 C3 107.3(3) . 1_655 ? O10 P4 O11 113.4(3) . 1_455 ? O10 P4 O12 108.5(2) . 1_455 ? O11 P4 O12 113.5(2) 1_455 1_455 ? O10 P4 C3 108.1(3) . . ? O11 P4 C3 105.4(3) 1_455 . ? O12 P4 C3 107.6(3) 1_455 . ? C9 N1 C5 116.3(5) . . ? C9 N1 Cu1 121.8(4) . . ? C5 N1 Cu1 121.6(4) . . ? C12 N2 C13 117.1(6) . . ? C12 N2 H2 121.5 . . ? C13 N2 H2 121.5 . . ? C18 C19 C15 118.5(7) . . ? C18 C19 H19 120.8 . . ? C15 C19 H19 120.8 . . ? C22 C21 C20 119.4(7) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C25 N5 C29 115.9(6) . . ? C25 N5 Cu2 123.4(5) . . ? C29 N5 Cu2 120.6(5) . . ? C33 N6 C32 118.6(7) . . ? C33 N6 H6A 120.7 . . ? C32 N6 H6A 120.7 . . ? C42 C43 C44 118.7(9) . . ? C42 C43 H43 120.6 . . ? C44 C43 H43 120.6 . . ? C37 C36 C35 120.2(7) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 120.0 . . ? P1 O1 Cu1 131.6(3) . . ? P1 O2 Cu2 121.8(2) . . ? P1 O3 Cu3 127.9(3) . . ? P2 O4 Cu2 121.1(3) . . ? P2 O5 Cu3 128.4(3) . . ? P3 O7 Cu1 122.5(3) . . ? P3 O9 Cu3 131.0(2) . 1_655 ? P4 O10 Cu3 130.8(3) . . ? P4 O11 Cu1 121.5(2) 1_655 . ? P4 O12 Cu2 131.2(3) 1_655 . ? C1 O13 Cu2 93.6(3) . . ? C1 O13 H131 104.7 . . ? Cu2 O13 H131 103.8 . . ? C3 O14 H141 105.3 . . ? H1W1 O1W H1W2 149.2 . . ? O2W O2W' H2W1 63.9 . . ? O2W O2W' H2W2 57.4 . . ? H2W1 O2W' H2W2 121.2 . . ? O2W' O2W H2W1 67.5 . . ? O2W' O2W H2W2 76.4 . . ? H2W1 O2W H2W2 143.9 . . ? N4 C22 C21 125.0(8) . . ? N4 C22 H22 117.5 . . ? C21 C22 H22 117.5 . . ? C23 N4 C22 114.7(7) . . ? N4 C23 C24 125.1(7) . . ? N4 C23 H23 117.5 . . ? C24 C23 H23 117.5 . . ? C20 C24 C23 118.7(7) . . ? C20 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C24 C20 C21 117.1(6) . . ? C24 C20 C13 120.3(6) . . ? C21 C20 C13 122.6(6) . . ? C14 C13 N2 120.8(6) . . ? C14 C13 C20 118.7(6) . . ? N2 C13 C20 120.6(6) . . ? C13 C14 C10 118.3(6) . . ? C13 C14 H14 120.8 . . ? C10 C14 H14 120.8 . . ? C11 C10 C14 125.0(6) . . ? C11 C10 C7 117.6(6) . . ? C14 C10 C7 117.3(6) . . ? C10 C11 C12 118.3(6) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? C11 C12 N2 120.4(6) . . ? C11 C12 C15 117.8(6) . . ? N2 C12 C15 121.7(6) . . ? C16 C15 C19 117.5(6) . . ? C16 C15 C12 121.8(6) . . ? C19 C15 C12 120.7(6) . . ? C15 C16 C17 121.6(7) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? N3 C17 C16 119.9(7) . . ? N3 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 N3 C18 121.5(7) . . ? N3 C18 C19 120.8(8) . . ? N3 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C8 C7 C6 116.6(6) . . ? C8 C7 C10 121.6(6) . . ? C6 C7 C10 121.8(6) . . ? C9 C8 C7 120.7(6) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? N1 C9 C8 122.8(6) . . ? N1 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? C6 C5 N1 124.0(6) . . ? C6 C5 H5 118.0 . . ? N1 C5 H5 118.0 . . ? C5 C6 C7 119.5(6) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? N7 C44 C43 125.3(10) . . ? N7 C44 H44 117.3 . . ? C43 C44 H44 117.3 . . ? C44 N7 C40 115.1(10) . . ? N7 C40 C41 123.4(10) . . ? N7 C40 H40 118.3 . . ? C41 C40 H40 118.3 . . ? C42 C41 C40 120.8(9) . . ? C42 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C41 C42 C43 116.6(9) . . ? C41 C42 C32 121.4(8) . . ? C43 C42 C32 121.9(8) . . ? C31 C32 N6 121.3(8) . . ? C31 C32 C42 118.4(7) . . ? N6 C32 C42 120.3(7) . . ? C30 C31 C32 118.7(7) . . ? C30 C31 H31 120.7 . . ? C32 C31 H31 120.7 . . ? C31 C30 C34 121.9(7) . . ? C31 C30 C27 117.1(6) . . ? C34 C30 C27 120.9(7) . . ? C30 C34 C33 120.1(7) . . ? C30 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? N6 C33 C34 119.4(7) . . ? N6 C33 C37 119.2(6) . . ? C34 C33 C37 121.5(7) . . ? C36 C37 C38 115.7(6) . . ? C36 C37 C33 122.6(7) . . ? C38 C37 C33 121.7(6) . . ? C39 C38 C37 119.2(7) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? N8 C39 C38 124.6(7) . . ? N8 C39 H39 117.7 . . ? C38 C39 H39 117.7 . . ? C35 N8 C39 116.4(6) . . ? C35 N8 Cu3 112.1(4) . 2_675 ? C39 N8 Cu3 127.5(5) . 2_675 ? N8 C35 C36 123.8(7) . . ? N8 C35 H35 118.1 . . ? C36 C35 H35 118.1 . . ? C26 C27 C28 117.7(7) . . ? C26 C27 C30 120.7(7) . . ? C28 C27 C30 121.7(6) . . ? C27 C26 C25 119.8(7) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? N5 C25 C26 123.4(7) . . ? N5 C25 H25 118.3 . . ? C26 C25 H25 118.3 . . ? N5 C29 C28 123.5(7) . . ? N5 C29 H29 118.2 . . ? C28 C29 H29 118.2 . . ? C29 C28 C27 119.6(7) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? O13 C1 C2 111.5(5) . . ? O13 C1 P2 104.5(4) . . ? C2 C1 P2 112.6(5) . . ? O13 C1 P1 107.3(4) . . ? C2 C1 P1 113.2(5) . . ? P2 C1 P1 107.2(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O14 C3 C4 111.8(5) . . ? O14 C3 P4 108.7(4) . . ? C4 C3 P4 112.1(5) . . ? O14 C3 P3 105.0(4) . 1_455 ? C4 C3 P3 111.0(5) . 1_455 ? P4 C3 P3 107.8(3) . 1_455 ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? 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 O13 H131 O11 0.84 2.08 2.810(6) 144.2 . O14 H141 O2 0.84 2.02 2.781(6) 151.0 1_455 O2W H2W1 O1W 0.86 1.71 2.48(2) 148.2 1_565 O2W H2W2 O10 0.84 2.13 2.912(16) 154.4 1_655 O2W H2W2 O12 0.84 2.64 3.295(19) 136.2 . O1W H1W1 O4 0.84 2.44 3.238(13) 158.7 1_645 N2 H2 O3 0.86 2.60 3.422(7) 160.8 2_656 N3 H3 O1W 0.86 2.05 2.858(1) 157.2 2_656 C5 H5 O1 0.93 2.36 2.873(8) 114.5 . C9 H9 O6 0.93 2.37 3.165(8) 143.7 1_645 C17 H17 O10 0.93 2.72 3.331(9) 124.0 2_566 C17 H17 O5 0.93 2.42 3.196(9) 141.4 2_566 C19 H19 O3 0.93 2.51 3.280(9) 140.2 2_656 C25 H25 O4 0.93 2.44 2.919(8) 112.2 . C25 H25 O8 0.93 2.35 3.238(8) 160.4 1_465 C35 H35 O9 0.93 2.54 3.118(8) 120.2 2_775 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.984 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.115 # Attachment '- 2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 818650' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H52 Cu8 N4 O38 P8 ' _chemical_formula_sum 'C28 H52 Cu8 N4 O38 P8' _chemical_formula_weight 1808.82 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' P P 0.1023 0.0942 '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 -p1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0321(10) _cell_length_b 10.0674(11) _cell_length_c 15.5816(17) _cell_angle_alpha 103.9290(10) _cell_angle_beta 91.1570(10) _cell_angle_gamma 99.5740(10) _cell_volume 1353.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3713 _cell_measurement_theta_min 1.35 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 3.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.347 _exptl_absorpt_correction_T_max 0.487 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _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 'SMART APEX II(Bruker, 2005)' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9610 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4712 _reflns_number_gt 3713 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART APEX II(Bruker, 2005)' _computing_cell_refinement 'SMART APEX II' _computing_data_reduction 'SMART APEX II' _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^)+(0.0603P)^2^+0.5287P] 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 4712 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.1100 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 0.42283(5) 0.98209(5) 0.28823(3) 0.01423(15) Uani 1 1 d . . . Cu2 Cu 0.13454(5) 0.52514(5) 0.06559(3) 0.01647(15) Uani 1 1 d . . . Cu3 Cu 0.92603(5) 1.47329(5) 0.27637(3) 0.01559(15) Uani 1 1 d . . . Cu4 Cu 0.64553(5) 1.03927(5) 0.05976(3) 0.01842(15) Uani 1 1 d . . . P1 P 0.34952(11) 1.14219(10) 0.14091(6) 0.0115(2) Uani 1 1 d . . . P2 P 0.64051(11) 1.23091(10) 0.25187(6) 0.0138(2) Uani 1 1 d . . . P3 P -0.15378(11) 0.64425(10) 0.13718(6) 0.0114(2) Uani 1 1 d . . . P4 P 0.13204(11) 0.73702(10) 0.25234(6) 0.0128(2) Uani 1 1 d . . . N1 N 0.5317(4) 0.9105(3) 0.3788(2) 0.0198(8) Uani 1 1 d . . . N2 N 0.9503(4) 0.6099(3) 0.6485(2) 0.0205(8) Uani 1 1 d . . . O1 O 0.3081(3) 1.0480(3) 0.20290(17) 0.0169(6) Uani 1 1 d . . . O2 O 0.4340(3) 1.0698(3) 0.06124(16) 0.0155(6) Uani 1 1 d . . . O3 O 0.2157(3) 1.1898(3) 0.10795(17) 0.0191(6) Uani 1 1 d . . . O4 O 0.5697(3) 1.1493(3) 0.31563(18) 0.0235(7) Uani 1 1 d . . . O5 O 0.7139(3) 1.1439(3) 0.17655(19) 0.0277(7) Uani 1 1 d . . . O6 O 0.7491(3) 1.3596(3) 0.30236(16) 0.0167(6) Uani 1 1 d . . . O7 O -0.0634(3) 0.5813(3) 0.05777(16) 0.0154(6) Uani 1 1 d . . . O8 O -0.1939(3) 0.5430(3) 0.19517(17) 0.0163(6) Uani 1 1 d . . . O9 O -0.2894(3) 0.6897(3) 0.10356(17) 0.0178(6) Uani 1 1 d . . . O10 O 0.2355(3) 0.8672(3) 0.30571(16) 0.0147(6) Uani 1 1 d . . . O11 O 0.2102(3) 0.6625(3) 0.17315(18) 0.0239(7) Uani 1 1 d . . . O12 O 0.0705(3) 0.6435(3) 0.31124(19) 0.0242(7) Uani 1 1 d . . . O13 O 0.4869(3) 0.8209(3) 0.1694(2) 0.0375(8) Uani 1 1 d . . . H131 H 0.5726 0.8009 0.1495 0.045 Uiso 1 1 d R . . H132 H 0.4231 0.7484 0.1621 0.045 Uiso 1 1 d R . . O14 O 0.3354(3) 0.4802(3) 0.05139(17) 0.0195(6) Uani 1 1 d . . . H141 H 0.3891 0.4645 0.0911 0.023 Uiso 1 1 d R . . H142 H 0.3523 0.4133 0.0042 0.023 Uiso 1 1 d R . . O15 O 0.0153(3) 0.3548(3) 0.13716(18) 0.0232(7) Uani 1 1 d . . . H151 H 0.0805 0.3062 0.1407 0.028 Uiso 1 1 d R . . H152 H -0.0632 0.3067 0.1068 0.028 Uiso 1 1 d R . . O16 O 0.8406(3) 0.9857(3) 0.04714(18) 0.0254(7) Uani 1 1 d . . . H161 H 0.8922 0.9690 0.0897 0.031 Uiso 1 1 d R . . H162 H 0.8585 0.9184 0.0038 0.031 Uiso 1 1 d R . . O17 O 0.5407(3) 1.3694(3) 0.13869(17) 0.0195(6) Uani 1 1 d . . . H17 H 0.6169 1.4253 0.1601 0.029 Uiso 1 1 calc R . . O18 O 0.0211(3) 0.8897(3) 0.15479(19) 0.0233(7) Uani 1 1 d . . . H18 H 0.0989 0.9414 0.1780 0.035 Uiso 1 1 calc R . . O1W O 0.2685(4) 0.7558(3) -0.00440(19) 0.0454(10) Uani 1 1 d . . . H1W1 H 0.2941 0.7873 0.0475 0.055 Uiso 1 1 d R . . H1W2 H 0.3325 0.7182 -0.0337 0.055 Uiso 1 1 d R . . C1 C 0.4852(4) 1.2932(4) 0.2024(2) 0.0147(8) Uani 1 1 d . . . C2 C 0.4109(5) 1.3855(4) 0.2739(3) 0.0252(10) Uani 1 1 d . . . H2A H 0.4808 1.4691 0.3002 0.038 Uiso 1 1 calc R . . H2B H 0.3807 1.3371 0.3185 0.038 Uiso 1 1 calc R . . H2C H 0.3241 1.4087 0.2483 0.038 Uiso 1 1 calc R . . C3 C -0.0290(4) 0.7945(4) 0.2084(2) 0.0137(8) Uani 1 1 d . . . C4 C -0.1220(4) 0.8613(4) 0.2824(3) 0.0225(9) Uani 1 1 d . . . H4A H -0.0571 0.9327 0.3255 0.034 Uiso 1 1 calc R . . H4B H -0.1702 0.7918 0.3103 0.034 Uiso 1 1 calc R . . H4C H -0.1969 0.9014 0.2579 0.034 Uiso 1 1 calc R . . C5 C 0.6502(4) 0.9884(4) 0.4321(3) 0.0189(9) Uani 1 1 d . . . H5 H 0.6784 1.0813 0.4314 0.023 Uiso 1 1 calc R . . C6 C 0.7312(5) 0.9343(4) 0.4879(3) 0.0229(10) Uani 1 1 d . . . H6 H 0.8098 0.9922 0.5252 0.027 Uiso 1 1 calc R . . C7 C 0.6972(5) 0.7961(4) 0.4890(3) 0.0196(9) Uani 1 1 d . . . C8 C 0.5716(5) 0.7167(5) 0.4359(3) 0.0343(12) Uani 1 1 d . . . H8 H 0.5405 0.6241 0.4364 0.041 Uiso 1 1 calc R . . C9 C 0.4940(5) 0.7770(4) 0.3826(3) 0.0333(12) Uani 1 1 d . . . H9 H 0.4112 0.7223 0.3474 0.040 Uiso 1 1 calc R . . C10 C 0.7862(4) 0.7302(4) 0.5431(3) 0.0184(9) Uani 1 1 d . . . C11 C 0.7928(5) 0.5899(4) 0.5187(3) 0.0226(9) Uani 1 1 d . . . H11 H 0.7451 0.5344 0.4656 0.027 Uiso 1 1 calc R . . C12 C 0.8710(5) 0.5325(4) 0.5741(3) 0.0222(9) Uani 1 1 d . . . H12 H 0.8685 0.4370 0.5591 0.027 Uiso 1 1 calc R . . C13 C 0.9486(4) 0.7478(4) 0.6698(3) 0.0213(9) Uani 1 1 d . . . H13 H 1.0054 0.8031 0.7200 0.026 Uiso 1 1 calc R . . C14 C 0.8672(4) 0.8101(4) 0.6209(3) 0.0219(9) Uani 1 1 d . . . H14 H 0.8658 0.9048 0.6394 0.026 Uiso 1 1 calc R . . 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 0.0112(3) 0.0139(3) 0.0184(3) 0.0087(2) -0.00256(19) -0.00187(19) Cu2 0.0117(3) 0.0211(3) 0.0152(3) 0.0001(2) -0.0019(2) 0.0058(2) Cu3 0.0115(3) 0.0152(3) 0.0216(3) 0.0109(2) -0.0031(2) -0.0020(2) Cu4 0.0130(3) 0.0222(3) 0.0181(3) -0.0004(2) -0.0031(2) 0.0059(2) P1 0.0088(5) 0.0115(5) 0.0144(5) 0.0044(4) -0.0005(4) 0.0011(4) P2 0.0123(5) 0.0137(5) 0.0152(5) 0.0059(4) -0.0034(4) -0.0008(4) P3 0.0088(5) 0.0122(5) 0.0135(5) 0.0039(4) 0.0002(4) 0.0020(4) P4 0.0104(5) 0.0122(5) 0.0155(5) 0.0048(4) -0.0034(4) -0.0002(4) N1 0.0192(19) 0.0194(18) 0.0220(18) 0.0076(14) -0.0037(15) 0.0037(15) N2 0.0161(18) 0.0238(19) 0.0248(18) 0.0132(15) -0.0013(14) 0.0023(15) O1 0.0130(14) 0.0163(14) 0.0227(14) 0.0119(12) -0.0020(11) -0.0035(11) O2 0.0113(14) 0.0178(14) 0.0167(14) 0.0031(11) -0.0018(11) 0.0026(11) O3 0.0161(15) 0.0219(15) 0.0208(15) 0.0055(12) 0.0000(12) 0.0079(12) O4 0.0213(16) 0.0229(16) 0.0268(16) 0.0183(13) -0.0099(12) -0.0110(12) O5 0.0223(17) 0.0336(18) 0.0239(15) -0.0052(13) -0.0082(13) 0.0143(14) O6 0.0141(14) 0.0169(14) 0.0176(14) 0.0073(11) -0.0006(11) -0.0053(11) O7 0.0079(13) 0.0213(15) 0.0156(14) 0.0009(11) -0.0008(11) 0.0043(11) O8 0.0118(14) 0.0166(14) 0.0207(14) 0.0089(11) -0.0030(11) -0.0030(11) O9 0.0136(14) 0.0212(15) 0.0193(14) 0.0039(12) -0.0012(11) 0.0073(12) O10 0.0125(14) 0.0144(14) 0.0162(13) 0.0063(11) 0.0014(11) -0.0046(11) O11 0.0142(15) 0.0269(16) 0.0248(15) -0.0054(12) -0.0056(12) 0.0053(12) O12 0.0201(16) 0.0226(16) 0.0307(16) 0.0186(13) -0.0126(13) -0.0094(12) O13 0.0255(18) 0.0324(19) 0.048(2) -0.0066(15) 0.0058(15) 0.0107(14) O14 0.0142(15) 0.0271(16) 0.0187(14) 0.0052(12) -0.0017(11) 0.0088(12) O15 0.0185(15) 0.0199(15) 0.0328(17) 0.0070(13) 0.0008(13) 0.0074(12) O16 0.0210(16) 0.0350(18) 0.0212(15) 0.0037(13) -0.0036(12) 0.0131(13) O17 0.0176(16) 0.0185(15) 0.0212(15) 0.0082(12) -0.0065(12) -0.0043(12) O18 0.0188(16) 0.0206(16) 0.0323(16) 0.0164(13) -0.0100(13) -0.0050(12) O1W 0.070(3) 0.034(2) 0.032(2) 0.0096(17) 0.0056(19) 0.0069(19) C1 0.013(2) 0.0132(19) 0.0161(19) 0.0022(15) -0.0025(16) -0.0002(16) C2 0.020(2) 0.023(2) 0.027(2) -0.0029(18) 0.0006(18) 0.0015(18) C3 0.013(2) 0.0102(19) 0.0175(19) 0.0049(15) 0.0001(16) -0.0008(15) C4 0.013(2) 0.020(2) 0.028(2) -0.0021(18) 0.0040(18) -0.0011(17) C5 0.021(2) 0.016(2) 0.021(2) 0.0074(17) 0.0007(17) 0.0016(17) C6 0.022(2) 0.024(2) 0.021(2) 0.0041(18) -0.0092(18) 0.0028(18) C7 0.022(2) 0.019(2) 0.021(2) 0.0083(17) 0.0004(17) 0.0065(18) C8 0.038(3) 0.026(2) 0.040(3) 0.018(2) -0.017(2) -0.004(2) C9 0.031(3) 0.024(2) 0.044(3) 0.015(2) -0.020(2) -0.007(2) C10 0.016(2) 0.022(2) 0.020(2) 0.0105(17) 0.0027(17) 0.0037(17) C11 0.028(2) 0.022(2) 0.018(2) 0.0038(17) -0.0043(18) 0.0065(18) C12 0.022(2) 0.022(2) 0.022(2) 0.0051(18) -0.0005(18) 0.0052(18) C13 0.018(2) 0.020(2) 0.024(2) 0.0074(17) -0.0025(17) -0.0049(17) C14 0.020(2) 0.020(2) 0.028(2) 0.0103(18) -0.0035(18) 0.0023(18) _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 O4 1.914(3) . ? Cu1 O10 1.948(2) . ? Cu1 O1 1.970(3) . ? Cu1 N1 2.037(3) . ? Cu1 O13 2.304(3) . ? Cu2 O11 1.927(3) . ? Cu2 O14 1.946(3) . ? Cu2 O7 1.973(2) . ? Cu2 O7 1.997(2) 2_565 ? Cu2 O15 2.387(3) . ? Cu2 Cu2 3.0387(9) 2_565 ? Cu3 O6 1.915(2) . ? Cu3 O12 1.927(3) 1_665 ? Cu3 O8 1.973(3) 1_665 ? Cu3 N2 2.012(3) 2_776 ? Cu3 O15 2.434(3) 1_665 ? Cu4 O5 1.902(3) . ? Cu4 O16 1.927(3) . ? Cu4 O2 1.985(3) . ? Cu4 O2 1.990(2) 2_675 ? Cu4 O1W 2.440(3) 2_675 ? P1 O3 1.497(3) . ? P1 O1 1.520(3) . ? P1 O2 1.563(3) . ? P1 C1 1.834(4) . ? P2 O5 1.521(3) . ? P2 O6 1.521(3) . ? P2 O4 1.522(3) . ? P2 C1 1.854(4) . ? P3 O9 1.503(3) . ? P3 O8 1.524(3) . ? P3 O7 1.560(3) . ? P3 C3 1.834(4) . ? P4 O12 1.517(3) . ? P4 O10 1.523(3) . ? P4 O11 1.533(3) . ? P4 C3 1.831(4) . ? N1 C9 1.346(5) . ? N1 C5 1.350(5) . ? N2 C12 1.345(5) . ? N2 C13 1.351(5) . ? N2 Cu3 2.012(3) 2_776 ? O2 Cu4 1.990(2) 2_675 ? O7 Cu2 1.997(2) 2_565 ? O8 Cu3 1.973(3) 1_445 ? O12 Cu3 1.927(3) 1_445 ? O13 H131 0.8760 . ? O13 H132 0.8337 . ? O14 H141 0.8381 . ? O14 H142 0.9042 . ? O15 Cu3 2.434(3) 1_445 ? O15 H151 0.8342 . ? O15 H152 0.8504 . ? O16 H161 0.8677 . ? O16 H162 0.8731 . ? O17 C1 1.443(4) . ? O17 H17 0.8200 . ? O18 C3 1.441(4) . ? O18 H18 0.8200 . ? O1W Cu4 2.440(3) 2_675 ? O1W H1W1 0.8083 . ? O1W H1W2 0.8290 . ? C1 C2 1.515(5) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.530(5) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.386(5) . ? C5 H5 0.9300 . ? C6 C7 1.378(6) . ? C6 H6 0.9300 . ? C7 C8 1.397(6) . ? C7 C10 1.489(6) . ? C8 C9 1.382(6) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.382(5) . ? C10 C14 1.397(5) . ? C11 C12 1.389(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.369(5) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? 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 Cu1 O10 153.29(12) . . ? O4 Cu1 O1 92.54(11) . . ? O10 Cu1 O1 87.64(11) . . ? O4 Cu1 N1 89.51(12) . . ? O10 Cu1 N1 89.65(12) . . ? O1 Cu1 N1 177.16(12) . . ? O4 Cu1 O13 111.23(12) . . ? O10 Cu1 O13 95.46(11) . . ? O1 Cu1 O13 87.54(11) . . ? N1 Cu1 O13 93.54(12) . . ? O11 Cu2 O14 88.85(11) . . ? O11 Cu2 O7 96.37(11) . . ? O14 Cu2 O7 168.71(11) . . ? O11 Cu2 O7 167.33(12) . 2_565 ? O14 Cu2 O7 92.65(10) . 2_565 ? O7 Cu2 O7 80.09(11) . 2_565 ? O11 Cu2 O15 95.67(11) . . ? O14 Cu2 O15 102.48(10) . . ? O7 Cu2 O15 87.00(10) . . ? O7 Cu2 O15 96.29(10) 2_565 . ? O11 Cu2 Cu2 135.49(9) . 2_565 ? O14 Cu2 Cu2 131.84(8) . 2_565 ? O7 Cu2 Cu2 40.33(7) . 2_565 ? O7 Cu2 Cu2 39.76(7) 2_565 2_565 ? O15 Cu2 Cu2 92.18(7) . 2_565 ? O6 Cu3 O12 148.09(12) . 1_665 ? O6 Cu3 O8 90.81(11) . 1_665 ? O12 Cu3 O8 94.03(11) 1_665 1_665 ? O6 Cu3 N2 88.94(12) . 2_776 ? O12 Cu3 N2 88.44(12) 1_665 2_776 ? O8 Cu3 N2 175.70(12) 1_665 2_776 ? O6 Cu3 O15 109.06(10) . 1_665 ? O12 Cu3 O15 102.84(11) 1_665 1_665 ? O8 Cu3 O15 81.60(10) 1_665 1_665 ? N2 Cu3 O15 94.43(12) 2_776 1_665 ? O5 Cu4 O16 87.93(12) . . ? O5 Cu4 O2 98.86(11) . . ? O16 Cu4 O2 172.21(11) . . ? O5 Cu4 O2 177.82(11) . 2_675 ? O16 Cu4 O2 94.16(11) . 2_675 ? O2 Cu4 O2 79.02(11) . 2_675 ? O5 Cu4 O1W 89.60(12) . 2_675 ? O16 Cu4 O1W 91.08(12) . 2_675 ? O2 Cu4 O1W 92.79(11) . 2_675 ? O2 Cu4 O1W 90.98(10) 2_675 2_675 ? O3 P1 O1 112.43(16) . . ? O3 P1 O2 110.27(15) . . ? O1 P1 O2 111.13(15) . . ? O3 P1 C1 109.65(17) . . ? O1 P1 C1 107.54(16) . . ? O2 P1 C1 105.54(16) . . ? O5 P2 O6 111.89(16) . . ? O5 P2 O4 113.52(18) . . ? O6 P2 O4 110.28(15) . . ? O5 P2 C1 107.65(16) . . ? O6 P2 C1 106.71(16) . . ? O4 P2 C1 106.37(17) . . ? O9 P3 O8 112.74(15) . . ? O9 P3 O7 109.90(15) . . ? O8 P3 O7 111.15(15) . . ? O9 P3 C3 109.91(16) . . ? O8 P3 C3 105.27(16) . . ? O7 P3 C3 107.66(16) . . ? O12 P4 O10 111.10(15) . . ? O12 P4 O11 113.27(17) . . ? O10 P4 O11 111.00(15) . . ? O12 P4 C3 106.82(17) . . ? O10 P4 C3 106.80(16) . . ? O11 P4 C3 107.48(16) . . ? C9 N1 C5 117.0(3) . . ? C9 N1 Cu1 120.0(3) . . ? C5 N1 Cu1 122.8(3) . . ? C12 N2 C13 117.4(3) . . ? C12 N2 Cu3 121.9(3) . 2_776 ? C13 N2 Cu3 120.6(3) . 2_776 ? P1 O1 Cu1 134.41(16) . . ? P1 O2 Cu4 128.56(15) . . ? P1 O2 Cu4 129.94(15) . 2_675 ? Cu4 O2 Cu4 100.98(11) . 2_675 ? P2 O4 Cu1 127.83(17) . . ? P2 O5 Cu4 133.85(17) . . ? P2 O6 Cu3 135.92(16) . . ? P3 O7 Cu2 126.36(15) . . ? P3 O7 Cu2 130.29(15) . 2_565 ? Cu2 O7 Cu2 99.91(11) . 2_565 ? P3 O8 Cu3 133.27(16) . 1_445 ? P4 O10 Cu1 136.53(16) . . ? P4 O11 Cu2 132.47(17) . . ? P4 O12 Cu3 126.81(17) . 1_445 ? Cu1 O13 H131 133.8 . . ? Cu1 O13 H132 107.7 . . ? H131 O13 H132 110.2 . . ? Cu2 O14 H141 125.1 . . ? Cu2 O14 H142 119.6 . . ? H141 O14 H142 100.5 . . ? Cu2 O15 Cu3 108.73(10) . 1_445 ? Cu2 O15 H151 104.2 . . ? Cu3 O15 H151 116.5 1_445 . ? Cu2 O15 H152 110.7 . . ? Cu3 O15 H152 105.2 1_445 . ? H151 O15 H152 111.5 . . ? Cu4 O16 H161 123.7 . . ? Cu4 O16 H162 122.4 . . ? H161 O16 H162 98.8 . . ? C1 O17 H17 109.5 . . ? C3 O18 H18 109.5 . . ? Cu4 O1W H1W1 99.6 2_675 . ? Cu4 O1W H1W2 87.8 2_675 . ? H1W1 O1W H1W2 113.8 . . ? O17 C1 C2 109.5(3) . . ? O17 C1 P1 106.4(2) . . ? C2 C1 P1 111.1(3) . . ? O17 C1 P2 110.6(2) . . ? C2 C1 P2 110.3(3) . . ? P1 C1 P2 108.74(19) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O18 C3 C4 110.5(3) . . ? O18 C3 P4 110.2(2) . . ? C4 C3 P4 111.7(3) . . ? O18 C3 P3 107.6(2) . . ? C4 C3 P3 107.2(3) . . ? P4 C3 P3 109.53(19) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C6 122.0(4) . . ? N1 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C7 C6 C5 121.1(4) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C8 116.7(4) . . ? C6 C7 C10 123.5(4) . . ? C8 C7 C10 119.8(4) . . ? C9 C8 C7 119.4(4) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? N1 C9 C8 123.6(4) . . ? N1 C9 H9 118.2 . . ? C8 C9 H9 118.2 . . ? C11 C10 C14 117.8(4) . . ? C11 C10 C7 122.0(4) . . ? C14 C10 C7 120.3(4) . . ? C10 C11 C12 119.5(4) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? N2 C12 C11 122.5(4) . . ? N2 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? N2 C13 C14 123.1(4) . . ? N2 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C13 C14 C10 119.5(4) . . ? C13 C14 H14 120.3 . . ? C10 C14 H14 120.3 . . ? 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 O13 H131 O9 0.88 1.85 2.683(4) 157.4 1_655 O13 H132 O11 0.83 2.00 2.742(4) 147.5 . O14 H141 O17 0.84 2.02 2.802(4) 154.9 1_545 O14 H142 O9 0.90 1.77 2.581(4) 147.4 2_565 O15 H151 O3 0.83 1.83 2.629(4) 160.6 1_545 O15 H152 O1W 0.85 2.32 3.133(4) 159.9 2_565 O16 H161 O18 0.87 1.92 2.757(4) 162.7 1_655 O16 H162 O3 0.87 1.86 2.611(4) 142.8 2_675 O17 H17 O8 0.82 1.90 2.712(4) 172.0 1_665 O18 H18 O1 0.82 1.99 2.791(4) 164.7 . O18 H18 O10 0.82 2.64 3.090(4) 116.2 . O1W H1W1 O13 0.81 2.47 3.187(4) 147.9 . O1W H1W1 O11 0.81 2.63 3.156(4) 124.3 . O1W H1W2 O17 0.83 2.12 2.922(4) 163.7 2_675 C12 H12 O12 0.93 2.44 2.900(5) 110.9 2_666 C14 H14 O10 0.93 2.57 3.461(5) 159.9 2_676 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.511 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.181 # Attachment '- checkcif 1-2.txt'