Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Robert P. Doyle' _publ_contact_author_address ; School of Chemistry Trinity College Dublin Dublin 2 Ireland ; _publ_contact_author_phone ' 315 443 3584 ' _publ_contact_author_fax ' 315 442 4070 ' _publ_contact_author_email rpdoyle@syr.edu loop_ _publ_author_name _publ_author_address R.P.Doyle ; Department of Chemistry Syracuse University Syracuse, NY 13244-4100 USA ; P.E.Kruger ; Department of Chemistry College of Science University of Canterbury Christchurch 8020 New Zealand ; M.Nieuwenhuyzen ; Chemistry Department Queen's University Belfast, BT9 5AG UK ; M.Julve ; Department de Quimica Inorganica Facultat de Quimica Universitat de Valencia Dr. Molinar 50, E-46100, Valencia Spain. ; F.Lloret ; Department de Quimica Inorganica Facultat de Quimica Universitat de Valencia Dr. Molinar 50, E-46100, Valencia Spain. ; J.Cano ; Department of Quimica Inorganica Centre de Recerca en Quimica Teorica (CERQT) Universitat de Barcelona 08028 Barcelona Spain ; ; T.H.Bauer ; ; Department of Chemistry Syracuse University Syracuse, NY 13244-4100 USA ; _publ_section_title ; Metamorphosis of a butterfly ; data_1 _database_code_depnum_ccdc_archive 'CCDC 655952' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H66.50 Cu4 N8 O27.50 P2.50' _chemical_formula_weight 1431.10 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 14.250(9) _cell_length_b 18.493(12) _cell_length_c 21.397(14) _cell_angle_alpha 90.00 _cell_angle_beta 99.30(2) _cell_angle_gamma 90.00 _cell_volume 5564(6) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour Blue _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 1.675 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4540 _exptl_absorpt_correction_T_max 0.7095 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 27266 _diffrn_reflns_av_R_equivalents 0.1277 _diffrn_reflns_av_sigmaI/netI 0.1865 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9619 _reflns_number_gt 4225 _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^)+(0.1125P)^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 calc _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9619 _refine_ls_number_parameters 751 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1743 _refine_ls_R_factor_gt 0.0851 _refine_ls_wR_factor_ref 0.2517 _refine_ls_wR_factor_gt 0.2132 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.003 _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 1.67795(9) -0.13413(7) 0.84485(6) 0.0229(4) Uani 1 1 d . . . Cu2 Cu 1.67327(9) -0.36224(7) 0.84381(6) 0.0225(4) Uani 1 1 d . . . Cu3 Cu 1.88745(10) -0.16821(7) 0.94344(7) 0.0286(4) Uani 1 1 d . . . Cu4 Cu 1.86378(10) -0.33878(7) 0.95693(7) 0.0301(4) Uani 1 1 d . . . O1 O 1.9468(5) -0.2564(4) 0.9812(4) 0.035(2) Uani 1 1 d . . . P1 P 1.82149(19) -0.24792(15) 0.81705(13) 0.0209(6) Uani 1 1 d D . . O11 O 1.7241(5) -0.2069(3) 0.7965(3) 0.0232(18) Uani 1 1 d D . . O12 O 1.7988(5) -0.3143(3) 0.8547(3) 0.0241(18) Uani 1 1 d D . . O13 O 1.8970(4) -0.2016(3) 0.8595(3) 0.0232(18) Uani 1 1 d D . . O14 O 1.8591(5) -0.2698(3) 0.7587(3) 0.0278(19) Uani 1 1 d D . . P2 P 1.6749(2) -0.24923(16) 0.94872(14) 0.0234(7) Uani 1 1 d . . . O21 O 1.7238(5) -0.1837(3) 0.9248(3) 0.0217(17) Uani 1 1 d . . . O22 O 1.6179(5) -0.2908(4) 0.8911(3) 0.0245(18) Uani 1 1 d . . . O23 O 1.7566(5) -0.2948(4) 0.9870(3) 0.0261(18) Uani 1 1 d . . . O24 O 1.6027(5) -0.2251(4) 0.9888(4) 0.032(2) Uani 1 1 d . . . O1W O 1.5214(5) -0.1825(4) 0.8193(4) 0.0279(19) Uani 1 1 d . . . O2W O 1.6002(5) -0.3106(4) 0.7495(3) 0.0279(19) Uani 1 1 d . . . N1A N 1.6399(6) -0.0470(5) 0.8877(4) 0.026(2) Uani 1 1 d . . . C2A C 1.6311(8) -0.0417(6) 0.9472(6) 0.035(3) Uani 1 1 d . . . H2A H 1.6421 -0.0834 0.9733 0.042 Uiso 1 1 calc R . . C3A C 1.6069(8) 0.0211(6) 0.9732(6) 0.041(3) Uani 1 1 d . . . H3A H 1.5999 0.0236 1.0166 0.049 Uiso 1 1 calc R . . C4A C 1.5928(8) 0.0810(7) 0.9347(7) 0.041(3) Uani 1 1 d . . . H4A H 1.5778 0.1260 0.9522 0.049 Uiso 1 1 calc R . . C5A C 1.5999(8) 0.0775(6) 0.8726(7) 0.039(3) Uani 1 1 d . . . H5A H 1.5887 0.1186 0.8458 0.047 Uiso 1 1 calc R . . C6A C 1.6245(8) 0.0102(6) 0.8493(6) 0.030(3) Uani 1 1 d . . . C7A C 1.6377(8) 0.0009(6) 0.7849(6) 0.029(3) Uani 1 1 d . . . C8A C 1.6267(8) 0.0516(6) 0.7376(6) 0.031(3) Uani 1 1 d . . . H8A H 1.6064 0.0991 0.7459 0.037 Uiso 1 1 calc R . . C9A C 1.6440(8) 0.0348(6) 0.6799(7) 0.039(3) Uani 1 1 d . . . H9A H 1.6389 0.0710 0.6480 0.047 Uiso 1 1 calc R . . C10A C 1.6691(8) -0.0345(6) 0.6663(6) 0.037(3) Uani 1 1 d . . . H10A H 1.6794 -0.0479 0.6251 0.045 Uiso 1 1 calc R . . C11A C 1.6788(8) -0.0832(6) 0.7151(6) 0.030(3) Uani 1 1 d . . . H11A H 1.6971 -0.1313 0.7071 0.036 Uiso 1 1 calc R . . N12A N 1.6637(6) -0.0667(5) 0.7726(4) 0.023(2) Uani 1 1 d . . . N1B N 1.8816(7) -0.1216(6) 1.0257(5) 0.036(3) Uani 1 1 d . . . C2B C 1.8798(8) -0.1554(8) 1.0780(6) 0.049(4) Uani 1 1 d . . . H2B H 1.8799 -0.2068 1.0784 0.059 Uiso 1 1 calc R . . C3B C 1.8776(10) -0.1173(9) 1.1346(7) 0.058(4) Uani 1 1 d . . . H3B H 1.8773 -0.1432 1.1729 0.069 Uiso 1 1 calc R . . C4B C 1.8758(9) -0.0454(9) 1.1351(7) 0.058(4) Uani 1 1 d . . . H4B H 1.8754 -0.0194 1.1733 0.070 Uiso 1 1 calc R . . C5B C 1.8747(8) -0.0099(8) 1.0787(6) 0.049(4) Uani 1 1 d . . . H5B H 1.8712 0.0414 1.0769 0.059 Uiso 1 1 calc R . . C6B C 1.8788(8) -0.0496(7) 1.0251(6) 0.036(3) Uani 1 1 d . . . C7B C 1.8757(7) -0.0186(6) 0.9641(6) 0.027(3) Uani 1 1 d . . . C8B C 1.8675(8) 0.0553(6) 0.9510(6) 0.038(3) Uani 1 1 d . . . H8B H 1.8621 0.0887 0.9840 0.046 Uiso 1 1 calc R . . C9B C 1.8674(8) 0.0796(6) 0.8906(6) 0.040(3) Uani 1 1 d . . . H9B H 1.8608 0.1297 0.8812 0.048 Uiso 1 1 calc R . . C10B C 1.8768(8) 0.0308(6) 0.8438(6) 0.037(3) Uani 1 1 d . . . H10B H 1.8783 0.0466 0.8018 0.044 Uiso 1 1 calc R . . C11B C 1.8839(7) -0.0411(6) 0.8588(6) 0.029(3) Uani 1 1 d . . . H11B H 1.8904 -0.0750 0.8264 0.034 Uiso 1 1 calc R . . N12B N 1.8822(7) -0.0647(5) 0.9164(5) 0.033(2) Uani 1 1 d . . . N1C N 1.5641(7) -0.4303(5) 0.8501(4) 0.027(2) Uani 1 1 d . . . C2C C 1.4836(7) -0.4147(6) 0.8723(5) 0.029(3) Uani 1 1 d . . . H2C H 1.4746 -0.3664 0.8852 0.034 Uiso 1 1 calc R . . C3C C 1.4125(9) -0.4646(7) 0.8778(6) 0.041(3) Uani 1 1 d . . . H3C H 1.3566 -0.4514 0.8939 0.049 Uiso 1 1 calc R . . C4C C 1.4271(9) -0.5330(8) 0.8589(6) 0.045(4) Uani 1 1 d . . . H4C H 1.3815 -0.5697 0.8622 0.053 Uiso 1 1 calc R . . C5C C 1.5098(9) -0.5491(6) 0.8347(6) 0.041(3) Uani 1 1 d . . . H5C H 1.5205 -0.5970 0.8216 0.049 Uiso 1 1 calc R . . C6C C 1.5753(8) -0.4966(7) 0.8297(5) 0.034(3) Uani 1 1 d . . . C7C C 1.6676(8) -0.5064(6) 0.8063(5) 0.028(3) Uani 1 1 d . . . C8C C 1.6957(9) -0.5728(6) 0.7865(5) 0.039(3) Uani 1 1 d . . . H8C H 1.6561 -0.6141 0.7866 0.046 Uiso 1 1 calc R . . C9C C 1.7856(10) -0.5777(7) 0.7660(6) 0.045(4) Uani 1 1 d . . . H9C H 1.8077 -0.6229 0.7532 0.054 Uiso 1 1 calc R . . C10C C 1.8402(9) -0.5170(7) 0.7649(6) 0.040(3) Uani 1 1 d . . . H10C H 1.8996 -0.5194 0.7502 0.049 Uiso 1 1 calc R . . C11C C 1.8072(8) -0.4516(6) 0.7855(5) 0.028(3) Uani 1 1 d . . . H11C H 1.8448 -0.4093 0.7848 0.034 Uiso 1 1 calc R . . N12C N 1.7233(6) -0.4472(5) 0.8066(4) 0.026(2) Uani 1 1 d . . . N1D N 1.8029(6) -0.4361(5) 0.9632(4) 0.025(2) Uani 1 1 d . . . C2D C 1.7174(8) -0.4503(6) 0.9802(5) 0.031(3) Uani 1 1 d . . . H2D H 1.6818 -0.4110 0.9928 0.037 Uiso 1 1 calc R . . C3D C 1.6794(9) -0.5181(6) 0.9802(5) 0.035(3) Uani 1 1 d . . . H3D H 1.6190 -0.5256 0.9925 0.042 Uiso 1 1 calc R . . C4D C 1.7299(9) -0.5746(7) 0.9624(6) 0.043(3) Uani 1 1 d . . . H4D H 1.7054 -0.6225 0.9617 0.052 Uiso 1 1 calc R . . C5D C 1.8216(10) -0.5605(7) 0.9447(6) 0.046(4) Uani 1 1 d . . . H5D H 1.8581 -0.5995 0.9325 0.056 Uiso 1 1 calc R . . C6D C 1.8565(9) -0.4922(6) 0.9453(5) 0.032(3) Uani 1 1 d . . . C7D C 1.9505(8) -0.4706(6) 0.9275(5) 0.031(3) Uani 1 1 d . . . C8D C 2.0139(9) -0.5174(8) 0.9084(6) 0.047(4) Uani 1 1 d . . . H8D H 2.0012 -0.5679 0.9078 0.057 Uiso 1 1 calc R . . C9D C 2.0953(11) -0.4929(8) 0.8902(6) 0.055(4) Uani 1 1 d . . . H9D H 2.1396 -0.5261 0.8777 0.066 Uiso 1 1 calc R . . C10D C 2.1125(10) -0.4225(9) 0.8901(6) 0.060(5) Uani 1 1 d . . . H10D H 2.1681 -0.4043 0.8764 0.072 Uiso 1 1 calc R . . C11D C 2.0464(8) -0.3757(8) 0.9107(6) 0.048(4) Uani 1 1 d . . . H11D H 2.0590 -0.3252 0.9108 0.058 Uiso 1 1 calc R . . N12D N 1.9678(6) -0.3975(5) 0.9299(4) 0.033(2) Uani 1 1 d . . . O3W O 1.0772(6) -0.1818(4) 0.8260(4) 0.046(2) Uani 1 1 d . . . O4W O 1.2788(7) -0.3188(5) 0.8392(4) 0.061(3) Uani 1 1 d . . . O5W O 1.3171(8) -0.7395(7) 0.4567(7) 0.119(5) Uani 1 1 d . . . O6W O 1.2265(7) -0.3399(5) 0.3872(4) 0.063(3) Uani 1 1 d . . . O7W O 1.5166(8) -0.3307(6) 0.4751(5) 0.089(4) Uani 1 1 d . . . O8W O 1.4379(8) -0.1618(6) 0.9256(5) 0.088(4) Uani 1 1 d . . . O9W O 1.0000 -0.3719(5) 0.7500 0.035(3) Uani 1 2 d S . . O10W O 1.0388(12) -0.3477(8) 0.3175(6) 0.142(6) Uani 1 1 d . . . O11W O 1.2638(10) -0.2423(8) 0.2889(8) 0.157(8) Uani 1 1 d . . . O12W O 2.0000 -0.0643(6) 0.7500 0.089(6) Uani 1 2 d S . . O13W O 1.9309(8) -0.7170(6) 0.9022(5) 0.082(3) Uani 1 1 d . . . O14W O 1.0908(11) -0.2058(9) 0.2178(7) 0.150(6) Uani 1 1 d . . . O15W O 1.3912(11) -0.8179(8) 0.8976(7) 0.054(4) Uiso 0.67 1 d P A 2 O16W O 1.8724(8) 0.2012(7) 1.0494(6) 0.046(3) Uiso 0.67 1 d P B 2 O17W O 1.2543(14) 0.2514(10) 0.6078(11) 0.102(6) Uiso 0.67 1 d P C 2 O15' O 1.3420(19) -0.8063(13) 0.8813(12) 0.036(7) Uiso 0.33 1 d P D 1 O16' O 1.7715(18) 0.1494(14) 1.0620(13) 0.055(8) Uiso 0.33 1 d P E 1 O17' O 1.243(3) 0.243(2) 0.561(2) 0.099(13) Uiso 0.33 1 d P F 1 P3 P 1.4776(5) 0.2531(3) 0.7123(3) 0.0316(15) Uani 0.25 1 d PD . 2 O31 O 1.3688(12) 0.2358(16) 0.7025(15) 0.046(9) Uiso 0.25 1 d PD G 2 O32 O 1.496(2) 0.2746(17) 0.6471(9) 0.037(9) Uiso 0.25 1 d PD H 2 O33 O 1.5000 0.3198(8) 0.7500 0.030(6) Uiso 0.50 2 d SPD . 2 O34 O 1.539(2) 0.1921(12) 0.7388(15) 0.059(11) Uiso 0.25 1 d PD . 2 P3' P 1.4776(5) 0.2531(3) 0.7123(3) 0.0316(15) Uani 0.25 1 d PD . 1 O31' O 1.3777(15) 0.2819(19) 0.7159(17) 0.069(12) Uiso 0.25 1 d PD . 1 O32' O 1.490(3) 0.238(2) 0.6455(9) 0.073(15) Uiso 0.25 1 d PD I 1 O33' O 1.5534(16) 0.3046(13) 0.7435(13) 0.042(9) Uiso 0.25 1 d PD . 1 O34' O 1.5000 0.1832(7) 0.7500 0.020(5) Uiso 0.50 2 d SPD . 1 O18W O 1.4416(14) 0.2667(10) 0.6230(10) 0.053(5) Uiso 0.50 1 d P J 3 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 0.0268(8) 0.0213(7) 0.0203(8) 0.0008(6) 0.0025(6) 0.0012(6) Cu2 0.0252(8) 0.0211(7) 0.0208(8) 0.0012(6) 0.0021(6) -0.0022(6) Cu3 0.0354(9) 0.0287(8) 0.0211(9) -0.0004(6) 0.0023(7) -0.0032(7) Cu4 0.0336(9) 0.0303(8) 0.0249(9) 0.0053(7) -0.0001(7) 0.0016(7) O1 0.028(4) 0.035(5) 0.039(5) 0.003(4) 0.001(4) -0.001(4) P1 0.0200(15) 0.0242(15) 0.0184(16) 0.0032(13) 0.0033(12) 0.0014(14) O11 0.035(5) 0.015(4) 0.019(5) 0.000(3) 0.004(4) 0.002(3) O12 0.036(5) 0.024(4) 0.014(4) 0.003(3) 0.009(4) 0.006(3) O13 0.018(4) 0.024(4) 0.027(5) 0.001(3) 0.003(3) -0.002(3) O14 0.034(5) 0.023(4) 0.028(5) -0.001(3) 0.009(4) 0.001(3) P2 0.0287(17) 0.0231(15) 0.0183(16) -0.0008(14) 0.0040(13) -0.0017(14) O21 0.032(4) 0.026(4) 0.008(4) 0.001(3) 0.005(3) 0.007(3) O22 0.033(5) 0.024(4) 0.017(4) -0.003(3) 0.006(4) -0.008(3) O23 0.035(5) 0.026(4) 0.018(5) 0.001(3) 0.004(4) 0.004(4) O24 0.034(5) 0.031(4) 0.033(5) 0.001(4) 0.014(4) 0.004(4) O1W 0.025(4) 0.025(4) 0.033(5) -0.004(4) 0.004(4) -0.002(3) O2W 0.031(5) 0.025(4) 0.027(5) 0.008(3) 0.001(4) 0.001(3) N1A 0.029(6) 0.036(6) 0.015(6) -0.005(5) 0.006(4) -0.005(5) C2A 0.046(8) 0.020(6) 0.038(9) -0.005(6) 0.003(6) 0.011(6) C3A 0.048(8) 0.032(8) 0.043(9) -0.008(7) 0.004(7) 0.003(6) C4A 0.040(8) 0.032(7) 0.050(10) -0.028(7) 0.005(7) 0.000(6) C5A 0.034(8) 0.029(7) 0.052(10) -0.002(6) -0.001(7) 0.006(6) C6A 0.024(7) 0.035(7) 0.029(8) -0.008(6) -0.002(6) 0.005(6) C7A 0.028(7) 0.024(7) 0.035(8) 0.007(5) 0.002(6) -0.001(5) C8A 0.034(7) 0.020(6) 0.039(9) 0.004(6) 0.004(6) 0.004(5) C9A 0.031(7) 0.023(7) 0.062(11) 0.010(6) 0.005(7) -0.002(6) C10A 0.051(8) 0.040(8) 0.021(8) 0.005(6) 0.004(6) -0.004(6) C11A 0.032(7) 0.021(6) 0.033(8) -0.001(6) -0.001(6) -0.009(5) N12A 0.032(6) 0.022(5) 0.016(6) -0.004(4) 0.003(4) 0.002(4) N1B 0.034(6) 0.051(7) 0.023(7) -0.003(5) 0.003(5) -0.013(5) C2B 0.038(8) 0.073(10) 0.032(9) -0.003(8) -0.004(7) -0.025(7) C3B 0.062(10) 0.090(12) 0.023(9) -0.011(8) 0.017(8) -0.008(9) C4B 0.038(9) 0.089(12) 0.045(11) -0.043(9) 0.002(7) 0.002(8) C5B 0.047(9) 0.082(11) 0.020(8) -0.014(8) 0.006(7) 0.010(8) C6B 0.028(7) 0.051(9) 0.030(8) -0.021(7) 0.006(6) -0.010(6) C7B 0.014(6) 0.042(8) 0.026(7) -0.009(6) 0.009(5) -0.002(5) C8B 0.028(7) 0.038(8) 0.045(10) -0.017(7) -0.004(6) 0.011(6) C9B 0.048(8) 0.024(7) 0.048(10) 0.001(6) 0.006(7) 0.011(6) C10B 0.046(8) 0.021(7) 0.045(9) 0.016(6) 0.014(7) 0.002(6) C11B 0.030(7) 0.027(6) 0.033(8) -0.010(6) 0.017(6) -0.012(5) N12B 0.041(6) 0.022(5) 0.037(7) -0.005(5) 0.011(5) 0.000(5) N1C 0.040(6) 0.023(5) 0.015(6) 0.005(4) -0.003(5) -0.008(5) C2C 0.023(7) 0.036(7) 0.026(7) 0.010(6) -0.002(6) 0.001(6) C3C 0.033(8) 0.051(9) 0.039(9) 0.012(7) 0.007(6) -0.007(7) C4C 0.039(8) 0.062(10) 0.029(8) 0.012(7) -0.005(7) -0.020(7) C5C 0.059(9) 0.028(7) 0.037(9) 0.005(6) 0.007(7) -0.018(6) C6C 0.042(8) 0.040(8) 0.018(7) 0.013(6) 0.000(6) -0.009(6) C7C 0.046(8) 0.019(6) 0.017(7) 0.000(5) -0.005(6) -0.010(6) C8C 0.063(9) 0.024(7) 0.026(8) -0.002(6) 0.000(7) -0.006(6) C9C 0.067(10) 0.031(7) 0.037(9) -0.004(6) 0.008(7) 0.017(7) C10C 0.050(9) 0.040(8) 0.030(8) -0.004(6) 0.004(7) 0.010(7) C11C 0.032(7) 0.019(6) 0.031(8) -0.004(5) 0.001(6) 0.000(5) N12C 0.033(6) 0.030(5) 0.016(6) 0.003(4) 0.006(5) -0.001(5) N1D 0.031(6) 0.032(6) 0.012(5) 0.012(4) 0.003(4) 0.005(5) C2D 0.036(7) 0.031(7) 0.026(8) 0.010(6) 0.002(6) -0.001(6) C3D 0.041(8) 0.037(8) 0.026(8) 0.007(6) -0.001(6) -0.007(6) C4D 0.060(9) 0.033(8) 0.033(9) 0.012(6) -0.003(7) -0.005(7) C5D 0.081(11) 0.033(8) 0.024(8) -0.005(6) 0.005(7) 0.008(7) C6D 0.054(8) 0.026(7) 0.013(7) -0.007(5) -0.007(6) 0.006(6) C7D 0.037(7) 0.040(8) 0.014(7) 0.008(6) -0.001(6) 0.012(6) C8D 0.047(9) 0.066(10) 0.028(8) -0.005(7) 0.004(7) 0.022(8) C9D 0.065(11) 0.066(11) 0.031(9) 0.016(8) -0.004(8) 0.032(9) C10D 0.041(9) 0.107(14) 0.034(9) 0.037(9) 0.013(7) 0.008(9) C11D 0.025(7) 0.077(10) 0.044(9) 0.017(8) 0.008(7) 0.004(7) N12D 0.031(6) 0.043(6) 0.024(6) 0.010(5) -0.002(5) -0.003(5) O3W 0.048(5) 0.041(5) 0.052(6) -0.016(4) 0.021(5) -0.014(4) O4W 0.086(7) 0.068(7) 0.035(6) 0.022(5) 0.030(5) 0.022(6) O5W 0.072(9) 0.163(13) 0.126(13) -0.007(10) 0.028(8) -0.001(9) O6W 0.084(7) 0.063(6) 0.038(6) -0.008(5) 0.003(5) -0.011(6) O7W 0.086(8) 0.098(9) 0.078(9) -0.038(7) -0.005(7) 0.047(7) O8W 0.098(8) 0.121(9) 0.051(7) 0.040(7) 0.033(6) 0.078(8) O9W 0.041(7) 0.023(6) 0.044(8) 0.000 0.015(6) 0.000 O10W 0.203(16) 0.149(13) 0.067(10) -0.016(9) 0.000(10) 0.045(12) O11W 0.126(12) 0.161(14) 0.205(18) -0.113(13) 0.086(12) -0.088(11) O12W 0.174(16) 0.030(8) 0.087(13) 0.000 0.095(12) 0.000 O13W 0.103(9) 0.080(8) 0.058(8) 0.010(6) -0.007(7) 0.008(7) O14W 0.152(14) 0.195(16) 0.096(12) -0.014(12) -0.003(10) 0.049(13) P3 0.051(4) 0.020(3) 0.021(4) 0.000(3) 0.001(3) 0.000(3) P3' 0.051(4) 0.020(3) 0.021(4) 0.000(3) 0.001(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O11 1.879(6) . ? Cu1 O21 1.959(7) . ? Cu1 N12A 1.971(9) . ? Cu1 N1A 1.972(9) . ? Cu1 O1W 2.384(7) . ? Cu2 O22 1.911(7) . ? Cu2 N12C 1.947(9) . ? Cu2 O12 1.976(7) . ? Cu2 N1C 2.022(9) . ? Cu2 O2W 2.321(7) . ? Cu3 O13 1.925(7) . ? Cu3 O1 1.951(8) . ? Cu3 N1B 1.973(10) . ? Cu3 N12B 1.997(9) . ? Cu3 O21 2.319(7) . ? Cu4 O23 1.930(7) . ? Cu4 O1 1.948(8) . ? Cu4 N12D 1.996(9) . ? Cu4 N1D 2.011(9) . ? Cu4 O12 2.279(7) . ? P1 O14 1.491(7) . ? P1 O12 1.532(7) . ? P1 O13 1.549(7) . ? P1 O11 1.581(7) . ? P2 O24 1.510(7) . ? P2 O21 1.526(7) . ? P2 O23 1.558(8) . ? P2 O22 1.565(8) . ? N1A C2A 1.303(13) . ? N1A C6A 1.336(14) . ? C2A C3A 1.356(15) . ? C3A C4A 1.377(17) . ? C4A C5A 1.351(17) . ? C5A C6A 1.405(15) . ? C6A C7A 1.430(15) . ? C7A N12A 1.341(13) . ? C7A C8A 1.370(15) . ? C8A C9A 1.334(15) . ? C9A C10A 1.375(15) . ? C10A C11A 1.370(15) . ? C11A N12A 1.319(13) . ? N1B C2B 1.287(15) . ? N1B C6B 1.331(15) . ? C2B C3B 1.405(18) . ? C3B C4B 1.330(19) . ? C4B C5B 1.370(19) . ? C5B C6B 1.372(16) . ? C6B C7B 1.420(16) . ? C7B N12B 1.346(13) . ? C7B C8B 1.396(16) . ? C8B C9B 1.368(16) . ? C9B C10B 1.371(16) . ? C10B C11B 1.366(14) . ? C11B N12B 1.312(14) . ? N1C C6C 1.319(14) . ? N1C C2C 1.343(13) . ? C2C C3C 1.389(14) . ? C3C C4C 1.354(17) . ? C4C C5C 1.393(16) . ? C5C C6C 1.364(15) . ? C6C C7C 1.492(15) . ? C7C N12C 1.352(12) . ? C7C C8C 1.380(15) . ? C8C C9C 1.423(16) . ? C9C C10C 1.368(16) . ? C10C C11C 1.395(15) . ? C11C N12C 1.347(13) . ? N1D C2D 1.354(13) . ? N1D C6D 1.379(13) . ? C2D C3D 1.365(15) . ? C3D C4D 1.358(16) . ? C4D C5D 1.442(17) . ? C5D C6D 1.356(16) . ? C6D C7D 1.504(16) . ? C7D C8D 1.362(15) . ? C7D N12D 1.374(14) . ? C8D C9D 1.359(17) . ? C9D C10D 1.32(2) . ? C10D C11D 1.403(18) . ? C11D N12D 1.316(13) . ? P3 O33 1.479(12) . ? P3 O34 1.483(15) . ? P3 O32 1.514(16) . ? P3 O31 1.563(16) . ? P3 O34 1.58(3) 2_856 ? P3 P3 1.635(12) 2_856 ? O33 P3 1.479(12) 2_856 ? O34 O34 1.28(6) 2_856 ? O34 P3 1.58(3) 2_856 ? O31' O33' 1.27(4) 2_856 ? O33' O31' 1.27(4) 2_856 ? O33' P3' 1.46(3) 2_856 ? O33' O33' 1.59(5) 2_856 ? O34' P3' 1.530(12) 2_856 ? 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 O11 Cu1 O21 92.8(3) . . ? O11 Cu1 N12A 91.3(3) . . ? O21 Cu1 N12A 163.6(3) . . ? O11 Cu1 N1A 170.9(3) . . ? O21 Cu1 N1A 93.1(3) . . ? N12A Cu1 N1A 81.1(4) . . ? O11 Cu1 O1W 90.2(3) . . ? O21 Cu1 O1W 101.1(3) . . ? N12A Cu1 O1W 94.8(3) . . ? N1A Cu1 O1W 95.5(3) . . ? O22 Cu2 N12C 169.8(3) . . ? O22 Cu2 O12 94.1(3) . . ? N12C Cu2 O12 91.5(3) . . ? O22 Cu2 N1C 90.4(3) . . ? N12C Cu2 N1C 82.0(4) . . ? O12 Cu2 N1C 164.3(3) . . ? O22 Cu2 O2W 90.6(3) . . ? N12C Cu2 O2W 96.8(3) . . ? O12 Cu2 O2W 100.8(3) . . ? N1C Cu2 O2W 94.1(3) . . ? O13 Cu3 O1 91.5(3) . . ? O13 Cu3 N1B 172.7(4) . . ? O1 Cu3 N1B 94.2(4) . . ? O13 Cu3 N12B 92.4(3) . . ? O1 Cu3 N12B 156.1(4) . . ? N1B Cu3 N12B 80.5(4) . . ? O13 Cu3 O21 91.2(3) . . ? O1 Cu3 O21 108.9(3) . . ? N1B Cu3 O21 91.2(3) . . ? N12B Cu3 O21 94.6(3) . . ? O23 Cu4 O1 93.5(3) . . ? O23 Cu4 N12D 171.9(3) . . ? O1 Cu4 N12D 93.2(4) . . ? O23 Cu4 N1D 89.0(3) . . ? O1 Cu4 N1D 158.8(3) . . ? N12D Cu4 N1D 83.2(4) . . ? O23 Cu4 O12 90.9(3) . . ? O1 Cu4 O12 103.7(3) . . ? N12D Cu4 O12 92.0(3) . . ? N1D Cu4 O12 97.4(3) . . ? Cu4 O1 Cu3 109.8(4) . . ? O14 P1 O12 110.9(4) . . ? O14 P1 O13 109.3(4) . . ? O12 P1 O13 108.7(4) . . ? O14 P1 O11 108.4(4) . . ? O12 P1 O11 106.3(4) . . ? O13 P1 O11 113.2(4) . . ? P1 O11 Cu1 124.1(4) . . ? P1 O12 Cu2 124.2(4) . . ? P1 O12 Cu4 125.2(4) . . ? Cu2 O12 Cu4 104.1(3) . . ? P1 O13 Cu3 125.3(4) . . ? O24 P2 O21 110.2(4) . . ? O24 P2 O23 112.4(4) . . ? O21 P2 O23 105.2(4) . . ? O24 P2 O22 106.1(4) . . ? O21 P2 O22 109.5(4) . . ? O23 P2 O22 113.4(4) . . ? P2 O21 Cu1 123.9(4) . . ? P2 O21 Cu3 122.8(4) . . ? Cu1 O21 Cu3 106.0(3) . . ? P2 O22 Cu2 123.4(4) . . ? P2 O23 Cu4 128.1(4) . . ? C2A N1A C6A 120.6(10) . . ? C2A N1A Cu1 126.3(8) . . ? C6A N1A Cu1 113.1(7) . . ? N1A C2A C3A 122.5(12) . . ? C2A C3A C4A 117.7(12) . . ? C5A C4A C3A 121.5(11) . . ? C4A C5A C6A 117.1(12) . . ? N1A C6A C5A 120.5(11) . . ? N1A C6A C7A 117.5(10) . . ? C5A C6A C7A 121.9(12) . . ? N12A C7A C8A 119.6(11) . . ? N12A C7A C6A 112.7(10) . . ? C8A C7A C6A 127.7(11) . . ? C9A C8A C7A 120.5(11) . . ? C8A C9A C10A 120.4(12) . . ? C11A C10A C9A 116.7(12) . . ? N12A C11A C10A 123.2(11) . . ? C11A N12A C7A 119.5(10) . . ? C11A N12A Cu1 124.9(7) . . ? C7A N12A Cu1 115.6(7) . . ? C2B N1B C6B 119.3(12) . . ? C2B N1B Cu3 125.0(10) . . ? C6B N1B Cu3 115.7(8) . . ? N1B C2B C3B 120.8(14) . . ? C4B C3B C2B 120.8(15) . . ? C3B C4B C5B 118.0(14) . . ? C4B C5B C6B 118.9(15) . . ? N1B C6B C5B 122.2(13) . . ? N1B C6B C7B 114.2(11) . . ? C5B C6B C7B 123.6(13) . . ? N12B C7B C8B 118.8(11) . . ? N12B C7B C6B 116.5(11) . . ? C8B C7B C6B 124.7(11) . . ? C9B C8B C7B 119.9(11) . . ? C8B C9B C10B 119.2(11) . . ? C11B C10B C9B 118.8(12) . . ? N12B C11B C10B 122.2(11) . . ? C11B N12B C7B 121.1(10) . . ? C11B N12B Cu3 125.9(8) . . ? C7B N12B Cu3 113.0(8) . . ? C6C N1C C2C 118.2(10) . . ? C6C N1C Cu2 114.9(8) . . ? C2C N1C Cu2 126.9(8) . . ? N1C C2C C3C 124.3(11) . . ? C4C C3C C2C 116.5(12) . . ? C3C C4C C5C 119.3(12) . . ? C6C C5C C4C 120.5(12) . . ? N1C C6C C5C 121.0(11) . . ? N1C C6C C7C 112.6(10) . . ? C5C C6C C7C 126.3(12) . . ? N12C C7C C8C 121.6(11) . . ? N12C C7C C6C 116.7(10) . . ? C8C C7C C6C 121.7(10) . . ? C7C C8C C9C 118.1(11) . . ? C10C C9C C8C 119.8(11) . . ? C9C C10C C11C 118.9(11) . . ? N12C C11C C10C 121.5(11) . . ? C11C N12C C7C 120.1(9) . . ? C11C N12C Cu2 126.1(7) . . ? C7C N12C Cu2 113.7(7) . . ? C2D N1D C6D 119.4(10) . . ? C2D N1D Cu4 127.5(8) . . ? C6D N1D Cu4 113.0(7) . . ? N1D C2D C3D 123.6(11) . . ? C4D C3D C2D 118.6(11) . . ? C3D C4D C5D 118.5(12) . . ? C6D C5D C4D 120.9(12) . . ? C5D C6D N1D 119.0(11) . . ? C5D C6D C7D 125.9(11) . . ? N1D C6D C7D 115.2(10) . . ? C8D C7D N12D 120.9(11) . . ? C8D C7D C6D 124.6(12) . . ? N12D C7D C6D 114.5(10) . . ? C9D C8D C7D 120.8(14) . . ? C10D C9D C8D 119.7(14) . . ? C9D C10D C11D 118.2(13) . . ? N12D C11D C10D 123.9(14) . . ? C11D N12D C7D 116.5(11) . . ? C11D N12D Cu4 129.2(9) . . ? C7D N12D Cu4 114.1(7) . . ? O33 P3 O34 111.3(13) . . ? O33 P3 O32 103.2(13) . . ? O34 P3 O32 111.9(16) . . ? O33 P3 O31 111.5(12) . . ? O34 P3 O31 114.0(16) . . ? O32 P3 O31 104.2(15) . . ? O33 P3 O34 106.0(10) . 2_856 ? O34 P3 O34 49(2) . 2_856 ? O32 P3 O34 149.7(17) . 2_856 ? O31 P3 O34 72.0(16) . 2_856 ? O33 P3 P3 56.4(4) . 2_856 ? O34 P3 P3 60.7(13) . 2_856 ? O32 P3 P3 144.1(13) . 2_856 ? O31 P3 P3 110.7(13) . 2_856 ? O34 P3 P3 54.9(8) 2_856 2_856 ? P3 O33 P3 67.1(8) . 2_856 ? O34 O34 P3 69.3(17) 2_856 . ? O34 O34 P3 61.3(17) 2_856 2_856 ? P3 O34 P3 64.4(10) . 2_856 ? O31' O33' P3' 67.8(17) 2_856 2_856 ? O31' O33' O33' 122(3) 2_856 2_856 ? P3' O33' O33' 59.3(14) 2_856 2_856 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.078 _refine_diff_density_min -0.886 _refine_diff_density_rms 0.174