Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Vadapalli Chandrasekha' _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Kanpur 208016 INDIA ; _publ_contact_author_email VC@IITK.AC.IN _publ_section_title ; A new structural form for a decanuclear copper (II) assembly ; loop_ _publ_author_name 'Vadapalli Chandrasekhar' 'Viswanathan Baskar' 'Kandasamy Gopal' 'Paul Kogerler' 'Loganathan Nagarajan' data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 272462' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H65 Cu5 N6 O18 P3' _chemical_formula_weight 1256.53 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4610(10) _cell_length_b 15.5053(14) _cell_length_c 16.3395(15) _cell_angle_alpha 63.260(2) _cell_angle_beta 82.398(2) _cell_angle_gamma 75.381(2) _cell_volume 2508.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3844 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.31 _exptl_crystal_description block _exptl_crystal_colour dark-blue _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1290 _exptl_absorpt_coefficient_mu 2.253 _exptl_absorpt_correction_type 'Bruker SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 15812 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 28.24 _reflns_number_total 11131 _reflns_number_gt 8311 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1035P)^2^+2.9645P] 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 11131 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1708 _refine_ls_wR_factor_gt 0.1531 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 1.854 _refine_ls_shift/su_mean 0.047 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 0.53639(5) 0.66141(4) -0.04149(4) 0.01861(14) Uani 1 1 d . . . Cu2 Cu 0.56582(6) 0.54026(5) 0.29134(4) 0.02396(16) Uani 1 1 d . . . Cu3 Cu 0.49135(5) 0.37212(4) 0.23950(4) 0.01798(14) Uani 1 1 d . . . Cu4 Cu 0.72168(5) 0.47340(4) 0.14432(4) 0.01772(14) Uani 1 1 d . . . Cu5 Cu 0.75970(5) 0.22510(4) 0.28515(4) 0.01995(15) Uani 1 1 d . . . P1 P 0.66185(10) 0.49651(9) -0.05377(8) 0.0168(2) Uani 1 1 d . . . P2 P 0.63982(12) 0.68943(10) 0.11342(9) 0.0245(3) Uani 1 1 d . . . P3 P 0.55013(11) 0.17067(9) 0.23886(8) 0.0193(3) Uani 1 1 d . . . N1 N 0.5314(4) 0.3372(3) 0.3652(3) 0.0236(9) Uani 1 1 d . . . N2 N 0.5640(4) 0.4080(3) 0.3764(3) 0.0259(9) Uani 1 1 d . . . N3 N 0.6283(4) 0.5342(4) 0.4070(3) 0.0323(10) Uani 1 1 d . . . N4 N 0.8172(4) 0.4129(3) 0.2547(3) 0.0234(9) Uani 1 1 d . . . N5 N 0.8222(4) 0.3155(3) 0.3072(3) 0.0225(9) Uani 1 1 d . . . N6 N 0.8221(4) 0.1377(3) 0.4174(3) 0.0253(9) Uani 1 1 d . . . O1 O 0.5743(3) 0.5889(2) -0.1219(2) 0.0192(7) Uani 1 1 d . . . O2 O 0.6558(3) 0.5309(2) 0.0235(2) 0.0187(7) Uani 1 1 d . . . O3 O 0.6286(3) 0.3999(2) -0.0255(2) 0.0208(7) Uani 1 1 d . . . O4 O 0.5501(3) 0.7156(3) 0.0406(3) 0.0281(8) Uani 1 1 d . . . O5 O 0.5742(3) 0.6722(3) 0.2074(3) 0.0280(8) Uani 1 1 d . . . O6 O 0.7433(3) 0.6015(2) 0.1232(2) 0.0247(7) Uani 1 1 d . . . O7 O 0.4692(3) 0.2382(2) 0.2779(2) 0.0220(7) Uani 1 1 d . . . O8 O 0.6771(3) 0.1344(2) 0.2776(2) 0.0222(7) Uani 1 1 d . . . O9 O 0.5573(3) 0.2202(2) 0.1338(2) 0.0221(7) Uani 1 1 d . . . O10 O 0.5088(4) 0.5055(3) 0.2066(3) 0.0234(8) Uani 1 1 d . . . O11 O 0.6936(3) 0.3435(3) 0.1756(3) 0.0200(7) Uani 1 1 d . . . O51 O 0.9224(3) 0.1596(3) 0.2181(3) 0.0284(8) Uani 1 1 d . . . O52 O 0.7958(4) 0.1684(4) 0.0833(3) 0.0425(10) Uani 1 1 d . . . H104 H 0.7250 0.1801 0.0995 0.064 Uiso 1 1 calc R . . O53 O 0.3925(5) 0.7876(4) 0.2680(3) 0.0594(14) Uani 1 1 d . . . H105 H 0.4453 0.7601 0.2432 0.089 Uiso 1 1 calc R . . O54 O 0.8441(5) 0.9551(4) 0.3107(5) 0.080(2) Uani 1 1 d . . . H106 H 0.8207 1.0148 0.2945 0.120 Uiso 1 1 calc R . . O55 O 0.9791(11) 0.6825(10) 0.4136(8) 0.177(5) Uani 1 1 d . . . C1 C 0.8125(4) 0.4942(4) -0.1052(3) 0.0205(9) Uani 1 1 d . . . C2 C 0.9038(5) 0.4131(4) -0.0343(4) 0.0324(12) Uani 1 1 d . . . H2A H 0.8858 0.3498 -0.0168 0.049 Uiso 1 1 calc R . . H2B H 0.8987 0.4254 0.0187 0.049 Uiso 1 1 calc R . . H2C H 0.9837 0.4134 -0.0607 0.049 Uiso 1 1 calc R . . C3 C 0.8160(5) 0.4717(4) -0.1880(4) 0.0309(12) Uani 1 1 d . . . H3A H 0.8961 0.4682 -0.2143 0.046 Uiso 1 1 calc R . . H3B H 0.7606 0.5233 -0.2329 0.046 Uiso 1 1 calc R . . H3C H 0.7936 0.4096 -0.1685 0.046 Uiso 1 1 calc R . . C4 C 0.8430(5) 0.5953(4) -0.1358(4) 0.0342(13) Uani 1 1 d . . . H4A H 0.8432 0.6077 -0.0832 0.051 Uiso 1 1 calc R . . H4B H 0.7837 0.6461 -0.1779 0.051 Uiso 1 1 calc R . . H4C H 0.9212 0.5955 -0.1653 0.051 Uiso 1 1 calc R . . C5 C 0.7070(5) 0.7951(4) 0.0812(4) 0.0299(12) Uani 1 1 d . . . C6 C 0.7892(6) 0.8075(4) -0.0038(4) 0.0362(13) Uani 1 1 d . . . H6A H 0.8223 0.8648 -0.0225 0.054 Uiso 1 1 calc R . . H6B H 0.7431 0.8156 -0.0527 0.054 Uiso 1 1 calc R . . H6C H 0.8535 0.7499 0.0106 0.054 Uiso 1 1 calc R . . C7 C 0.6066(7) 0.8891(4) 0.0590(5) 0.0490(17) Uani 1 1 d . . . H7A H 0.6420 0.9458 0.0361 0.073 Uiso 1 1 calc R . . H7B H 0.5598 0.8841 0.1136 0.073 Uiso 1 1 calc R . . H7C H 0.5554 0.8962 0.0134 0.073 Uiso 1 1 calc R . . C8 C 0.7829(7) 0.7785(5) 0.1601(5) 0.0514(18) Uani 1 1 d . . . H8A H 0.8451 0.7196 0.1740 0.077 Uiso 1 1 calc R . . H8B H 0.7320 0.7714 0.2134 0.077 Uiso 1 1 calc R . . H8C H 0.8189 0.8342 0.1422 0.077 Uiso 1 1 calc R . . C9 C 0.4844(4) 0.0634(4) 0.2745(3) 0.0232(10) Uani 1 1 d . . . C10 C 0.5515(6) -0.0007(4) 0.2264(4) 0.0384(14) Uani 1 1 d . . . H10A H 0.6353 -0.0213 0.2413 0.058 Uiso 1 1 calc R . . H10B H 0.5434 0.0371 0.1612 0.058 Uiso 1 1 calc R . . H10C H 0.5177 -0.0579 0.2465 0.058 Uiso 1 1 calc R . . C11 C 0.3527(5) 0.1011(4) 0.2459(4) 0.0365(13) Uani 1 1 d . . . H11A H 0.3166 0.0459 0.2620 0.055 Uiso 1 1 calc R . . H11B H 0.3487 0.1411 0.1809 0.055 Uiso 1 1 calc R . . H11C H 0.3099 0.1400 0.2769 0.055 Uiso 1 1 calc R . . C12 C 0.4905(5) 0.0037(4) 0.3780(4) 0.0308(12) Uani 1 1 d . . . H12A H 0.4552 -0.0524 0.3963 0.046 Uiso 1 1 calc R . . H12B H 0.4470 0.0445 0.4071 0.046 Uiso 1 1 calc R . . H12C H 0.5732 -0.0187 0.3961 0.046 Uiso 1 1 calc R . . C13 C 0.5474(5) 0.2555(4) 0.4453(3) 0.0291(11) Uani 1 1 d . . . H13 H 0.5324 0.1952 0.4557 0.035 Uiso 1 1 calc R . . C14 C 0.5895(5) 0.2740(4) 0.5101(4) 0.0316(12) Uani 1 1 d . . . H14 H 0.6067 0.2309 0.5711 0.038 Uiso 1 1 calc R . . C15 C 0.6002(5) 0.3730(4) 0.4625(4) 0.0286(11) Uani 1 1 d . . . C16 C 0.6385(5) 0.4448(4) 0.4807(4) 0.0313(12) Uani 1 1 d . . . C17 C 0.6815(6) 0.4279(5) 0.5626(4) 0.0433(15) Uani 1 1 d . . . H17 H 0.6869 0.3664 0.6127 0.052 Uiso 1 1 calc R . . C18 C 0.7163(7) 0.5024(6) 0.5695(5) 0.0512(18) Uani 1 1 d . . . H18 H 0.7458 0.4917 0.6244 0.061 Uiso 1 1 calc R . . C19 C 0.7077(7) 0.5923(6) 0.4957(5) 0.0508(18) Uani 1 1 d . . . H19 H 0.7318 0.6433 0.4995 0.061 Uiso 1 1 calc R . . C20 C 0.6622(6) 0.6066(5) 0.4143(5) 0.0401(14) Uani 1 1 d . . . H20 H 0.6554 0.6681 0.3639 0.048 Uiso 1 1 calc R . . C21 C 0.8673(5) 0.4456(4) 0.3024(4) 0.0289(11) Uani 1 1 d . . . H21 H 0.8753 0.5104 0.2819 0.035 Uiso 1 1 calc R . . C22 C 0.9050(5) 0.3685(4) 0.3865(4) 0.0334(12) Uani 1 1 d . . . H22 H 0.9427 0.3706 0.4324 0.040 Uiso 1 1 calc R . . C23 C 0.8741(4) 0.2880(4) 0.3866(3) 0.0254(11) Uani 1 1 d . . . C24 C 0.8744(4) 0.1845(4) 0.4512(4) 0.0274(11) Uani 1 1 d . . . C25 C 0.9188(5) 0.1384(4) 0.5385(4) 0.0340(13) Uani 1 1 d . . . H25 H 0.9541 0.1717 0.5603 0.041 Uiso 1 1 calc R . . C26 C 0.9097(5) 0.0410(4) 0.5933(4) 0.0378(14) Uani 1 1 d . . . H26 H 0.9410 0.0074 0.6519 0.045 Uiso 1 1 calc R . . C27 C 0.8538(5) -0.0052(4) 0.5598(4) 0.0358(13) Uani 1 1 d . . . H27 H 0.8444 -0.0695 0.5963 0.043 Uiso 1 1 calc R . . C28 C 0.8120(5) 0.0455(4) 0.4711(4) 0.0292(11) Uani 1 1 d . . . H28 H 0.7755 0.0137 0.4484 0.035 Uiso 1 1 calc R . . C51 C 1.0249(5) 0.2004(5) 0.1946(4) 0.0372(13) Uani 1 1 d . . . H51A H 1.0093 0.2624 0.1409 0.056 Uiso 1 1 calc R . . H51B H 1.0917 0.1558 0.1823 0.056 Uiso 1 1 calc R . . H51C H 1.0439 0.2110 0.2444 0.056 Uiso 1 1 calc R . . C52 C 0.8014(8) 0.1698(6) -0.0043(5) 0.059(2) Uani 1 1 d . . . H52A H 0.7450 0.2266 -0.0437 0.089 Uiso 1 1 calc R . . H52B H 0.7817 0.1107 0.0013 0.089 Uiso 1 1 calc R . . H52C H 0.8814 0.1729 -0.0299 0.089 Uiso 1 1 calc R . . C53 C 0.2990(8) 0.8474(8) 0.2069(6) 0.077(3) Uani 1 1 d . . . H53A H 0.2349 0.8763 0.2371 0.116 Uiso 1 1 calc R . . H53B H 0.2692 0.8080 0.1864 0.116 Uiso 1 1 calc R . . H53C H 0.3286 0.8990 0.1551 0.116 Uiso 1 1 calc R . . C54 C 0.9201(10) 0.9378(6) 0.2390(8) 0.094(4) Uani 1 1 d . . . H54A H 0.9819 0.9752 0.2215 0.141 Uiso 1 1 calc R . . H54B H 0.8721 0.9582 0.1869 0.141 Uiso 1 1 calc R . . H54C H 0.9568 0.8686 0.2612 0.141 Uiso 1 1 calc R . . C55 C 0.9903(13) 0.6225(15) 0.3682(11) 0.155(7) Uani 1 1 d . . . H101 H 0.517(8) 0.531(6) 0.165(6) 0.06(3) Uiso 1 1 d . . . H102 H 0.681(5) 0.332(4) 0.146(4) 0.013(16) Uiso 1 1 d . . . H103 H 0.887(5) 0.169(4) 0.172(4) 0.021(15) Uiso 1 1 d . . . C56 C 0.2492(13) 0.1936(9) 0.6026(10) 0.125(5) Uani 1 1 d . . . O56 O 0.1850(10) 0.2226(8) 0.5109(13) 0.236(8) Uani 1 1 d . . . O57 O 0.2535(15) 0.2229(9) 0.4173(6) 0.234(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0219(3) 0.0158(3) 0.0157(3) -0.0053(2) -0.0071(2) 0.0003(2) Cu2 0.0288(3) 0.0262(3) 0.0198(3) -0.0119(3) -0.0013(3) -0.0067(3) Cu3 0.0202(3) 0.0175(3) 0.0130(3) -0.0045(2) -0.0049(2) -0.0006(2) Cu4 0.0195(3) 0.0168(3) 0.0141(3) -0.0042(2) -0.0063(2) -0.0011(2) Cu5 0.0192(3) 0.0174(3) 0.0174(3) -0.0028(2) -0.0067(2) -0.0003(2) P1 0.0175(6) 0.0167(6) 0.0137(5) -0.0050(5) -0.0044(4) -0.0007(4) P2 0.0322(7) 0.0196(6) 0.0222(6) -0.0088(5) -0.0098(5) -0.0026(5) P3 0.0213(6) 0.0157(6) 0.0162(6) -0.0028(5) -0.0050(5) -0.0016(5) N1 0.028(2) 0.023(2) 0.017(2) -0.0076(17) -0.0028(17) -0.0027(18) N2 0.032(2) 0.029(2) 0.015(2) -0.0076(18) -0.0030(18) -0.0064(19) N3 0.034(2) 0.039(3) 0.033(3) -0.023(2) -0.001(2) -0.008(2) N4 0.024(2) 0.024(2) 0.021(2) -0.0080(17) -0.0062(17) -0.0029(17) N5 0.023(2) 0.021(2) 0.019(2) -0.0023(17) -0.0073(17) -0.0045(17) N6 0.020(2) 0.024(2) 0.023(2) -0.0034(18) -0.0081(17) 0.0013(17) O1 0.0237(16) 0.0175(16) 0.0143(16) -0.0058(13) -0.0066(13) 0.0004(13) O2 0.0201(16) 0.0179(16) 0.0160(16) -0.0070(13) -0.0054(13) 0.0010(13) O3 0.0221(16) 0.0214(17) 0.0180(17) -0.0084(14) -0.0043(13) -0.0016(14) O4 0.0326(19) 0.0247(18) 0.030(2) -0.0170(16) -0.0115(16) 0.0032(15) O5 0.037(2) 0.0223(18) 0.0244(19) -0.0100(15) -0.0081(16) -0.0027(16) O6 0.0301(18) 0.0181(17) 0.0233(18) -0.0059(14) -0.0093(15) -0.0023(14) O7 0.0273(18) 0.0190(16) 0.0153(16) -0.0042(14) -0.0029(14) -0.0026(14) O8 0.0203(16) 0.0186(16) 0.0225(18) -0.0037(14) -0.0081(14) -0.0020(13) O9 0.0256(17) 0.0185(16) 0.0149(16) -0.0021(13) -0.0052(14) -0.0002(14) O10 0.030(2) 0.0214(18) 0.0169(19) -0.0058(16) -0.0073(16) -0.0041(15) O11 0.0241(18) 0.0186(17) 0.0175(18) -0.0072(15) -0.0078(14) -0.0022(14) O51 0.0257(19) 0.028(2) 0.029(2) -0.0109(17) -0.0022(17) -0.0039(16) O52 0.037(2) 0.059(3) 0.034(2) -0.027(2) -0.0029(19) 0.000(2) O53 0.069(3) 0.063(3) 0.034(3) -0.021(2) 0.001(2) 0.005(3) O54 0.058(3) 0.037(3) 0.143(6) -0.038(4) -0.041(4) 0.008(3) O55 0.192(11) 0.249(14) 0.165(11) -0.140(11) -0.003(9) -0.078(10) C1 0.017(2) 0.023(2) 0.021(2) -0.009(2) -0.0018(18) -0.0026(18) C2 0.022(3) 0.039(3) 0.033(3) -0.017(3) -0.008(2) 0.004(2) C3 0.031(3) 0.042(3) 0.023(3) -0.018(2) 0.007(2) -0.009(2) C4 0.031(3) 0.034(3) 0.039(3) -0.015(3) 0.009(2) -0.016(2) C5 0.043(3) 0.025(3) 0.022(3) -0.008(2) -0.008(2) -0.008(2) C6 0.045(3) 0.033(3) 0.030(3) -0.011(3) -0.007(3) -0.008(3) C7 0.063(4) 0.024(3) 0.060(5) -0.023(3) 0.005(4) -0.005(3) C8 0.081(5) 0.046(4) 0.033(3) -0.007(3) -0.021(3) -0.034(4) C9 0.026(2) 0.022(2) 0.019(2) -0.003(2) -0.008(2) -0.007(2) C10 0.050(4) 0.034(3) 0.039(3) -0.019(3) 0.005(3) -0.018(3) C11 0.034(3) 0.034(3) 0.034(3) -0.002(3) -0.014(3) -0.014(3) C12 0.041(3) 0.024(3) 0.020(3) 0.001(2) -0.006(2) -0.012(2) C13 0.033(3) 0.032(3) 0.015(2) -0.005(2) -0.006(2) 0.000(2) C14 0.041(3) 0.031(3) 0.017(2) -0.007(2) -0.006(2) -0.002(2) C15 0.034(3) 0.035(3) 0.017(2) -0.012(2) -0.005(2) -0.005(2) C16 0.036(3) 0.037(3) 0.021(3) -0.013(2) -0.005(2) -0.005(2) C17 0.049(4) 0.056(4) 0.030(3) -0.022(3) -0.008(3) -0.011(3) C18 0.066(5) 0.064(5) 0.035(4) -0.029(4) -0.013(3) -0.013(4) C19 0.057(4) 0.061(5) 0.058(5) -0.042(4) -0.013(4) -0.014(4) C20 0.050(4) 0.040(3) 0.040(3) -0.022(3) -0.005(3) -0.014(3) C21 0.030(3) 0.035(3) 0.024(3) -0.010(2) -0.008(2) -0.012(2) C22 0.041(3) 0.039(3) 0.018(3) -0.005(2) -0.012(2) -0.013(3) C23 0.021(2) 0.028(3) 0.020(2) -0.003(2) -0.009(2) -0.004(2) C24 0.020(2) 0.031(3) 0.020(2) 0.000(2) -0.009(2) -0.004(2) C25 0.031(3) 0.040(3) 0.021(3) -0.003(2) -0.007(2) -0.007(2) C26 0.032(3) 0.041(3) 0.022(3) 0.003(2) -0.013(2) -0.004(3) C27 0.028(3) 0.029(3) 0.028(3) 0.006(2) -0.001(2) -0.003(2) C28 0.023(2) 0.025(3) 0.024(3) 0.001(2) -0.004(2) 0.000(2) C51 0.025(3) 0.041(3) 0.033(3) -0.005(3) -0.006(2) -0.005(2) C52 0.082(5) 0.053(4) 0.044(4) -0.030(4) 0.002(4) -0.003(4) C53 0.065(5) 0.099(7) 0.054(5) -0.028(5) -0.014(4) 0.000(5) C54 0.117(8) 0.044(5) 0.135(10) -0.047(6) -0.072(8) 0.013(5) C55 0.107(10) 0.26(2) 0.148(14) -0.156(16) -0.029(9) 0.014(11) C56 0.119(10) 0.078(8) 0.118(11) -0.020(7) 0.018(9) 0.024(7) O56 0.129(9) 0.088(7) 0.38(2) 0.009(10) -0.068(12) -0.031(7) O57 0.48(2) 0.277(14) 0.106(7) -0.135(9) 0.155(11) -0.324(16) _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 O9 1.934(3) 2_665 ? Cu1 O1 2.027(3) . ? Cu1 O2 2.037(3) . ? Cu1 O3 2.259(3) 2_665 ? Cu2 N2 1.894(4) . ? Cu2 O5 1.902(4) . ? Cu2 O10 1.929(4) . ? Cu2 N3 2.064(5) . ? Cu3 O1 1.932(3) 2_665 ? Cu3 O10 1.945(4) . ? Cu3 O7 1.954(3) . ? Cu3 N1 1.961(4) . ? Cu3 O11 2.433(4) . ? Cu4 O2 1.932(3) . ? Cu4 O6 1.933(3) . ? Cu4 O11 1.945(4) . ? Cu4 N4 1.953(4) . ? Cu5 N5 1.907(4) . ? Cu5 O8 1.936(3) . ? Cu5 O11 1.962(4) . ? Cu5 N6 2.074(4) . ? Cu5 O51 2.283(4) . ? P1 O3 1.490(3) . ? P1 O1 1.560(3) . ? P1 O2 1.564(3) . ? P1 C1 1.816(5) . ? P2 O4 1.522(4) . ? P2 O6 1.526(4) . ? P2 O5 1.556(4) . ? P2 C5 1.819(5) . ? P3 O7 1.523(3) . ? P3 O8 1.532(3) . ? P3 O9 1.534(3) . ? P3 C9 1.821(5) . ? N1 N2 1.335(6) . ? N1 C13 1.343(7) . ? N2 C15 1.342(6) . ? N3 C20 1.333(7) . ? N3 C16 1.356(7) . ? N4 C21 1.347(6) . ? N4 N5 1.351(6) . ? N5 C23 1.340(6) . ? N6 C28 1.325(7) . ? N6 C24 1.364(7) . ? O1 Cu3 1.932(3) 2_665 ? O3 Cu1 2.259(3) 2_665 ? O9 Cu1 1.934(3) 2_665 ? O51 C51 1.402(7) . ? O52 C52 1.415(8) . ? O53 C53 1.398(10) . ? O54 C54 1.448(13) . ? O55 C55 1.403(16) . ? C1 C4 1.535(7) . ? C1 C3 1.535(7) . ? C1 C2 1.537(7) . ? C5 C6 1.536(8) . ? C5 C7 1.539(8) . ? C5 C8 1.540(8) . ? C9 C12 1.521(7) . ? C9 C11 1.528(7) . ? C9 C10 1.535(7) . ? C13 C14 1.383(8) . ? C14 C15 1.404(8) . ? C15 C16 1.450(8) . ? C16 C17 1.376(8) . ? C17 C18 1.367(9) . ? C18 C19 1.362(10) . ? C19 C20 1.397(9) . ? C21 C22 1.386(8) . ? C22 C23 1.381(8) . ? C23 C24 1.471(7) . ? C24 C25 1.377(7) . ? C25 C26 1.389(8) . ? C26 C27 1.379(9) . ? C27 C28 1.384(8) . ? C56 O56 1.58(2) . ? O56 O57 1.62(2) . ? 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 O9 97.56(15) . 2_665 ? O4 Cu1 O1 163.20(14) . . ? O9 Cu1 O1 93.88(14) 2_665 . ? O4 Cu1 O2 95.99(14) . . ? O9 Cu1 O2 163.52(13) 2_665 . ? O1 Cu1 O2 70.97(13) . . ? O4 Cu1 O3 97.19(14) . 2_665 ? O9 Cu1 O3 92.81(13) 2_665 2_665 ? O1 Cu1 O3 94.48(12) . 2_665 ? O2 Cu1 O3 94.75(12) . 2_665 ? N2 Cu2 O5 177.67(18) . . ? N2 Cu2 O10 84.31(18) . . ? O5 Cu2 O10 97.18(16) . . ? N2 Cu2 N3 78.84(19) . . ? O5 Cu2 N3 99.63(18) . . ? O10 Cu2 N3 163.12(18) . . ? O1 Cu3 O10 92.49(15) 2_665 . ? O1 Cu3 O7 89.20(14) 2_665 . ? O10 Cu3 O7 177.15(16) . . ? O1 Cu3 N1 170.95(16) 2_665 . ? O10 Cu3 N1 87.83(17) . . ? O7 Cu3 N1 90.14(16) . . ? O1 Cu3 O11 89.41(13) 2_665 . ? O10 Cu3 O11 87.13(15) . . ? O7 Cu3 O11 95.18(13) . . ? N1 Cu3 O11 99.64(15) . . ? O2 Cu4 O6 89.90(14) . . ? O2 Cu4 O11 93.36(15) . . ? O6 Cu4 O11 175.11(16) . . ? O2 Cu4 N4 169.37(16) . . ? O6 Cu4 N4 89.33(16) . . ? O11 Cu4 N4 88.13(17) . . ? N5 Cu5 O8 170.87(16) . . ? N5 Cu5 O11 83.72(17) . . ? O8 Cu5 O11 98.25(15) . . ? N5 Cu5 N6 78.61(17) . . ? O8 Cu5 N6 97.73(16) . . ? O11 Cu5 N6 159.79(17) . . ? N5 Cu5 O51 101.63(16) . . ? O8 Cu5 O51 86.93(14) . . ? O11 Cu5 O51 98.69(15) . . ? N6 Cu5 O51 94.43(16) . . ? O3 P1 O1 115.30(19) . . ? O3 P1 O2 115.97(19) . . ? O1 P1 O2 98.07(17) . . ? O3 P1 C1 110.2(2) . . ? O1 P1 C1 108.1(2) . . ? O2 P1 C1 108.3(2) . . ? O4 P2 O6 113.8(2) . . ? O4 P2 O5 110.7(2) . . ? O6 P2 O5 110.7(2) . . ? O4 P2 C5 108.3(2) . . ? O6 P2 C5 106.9(2) . . ? O5 P2 C5 106.1(2) . . ? O7 P3 O8 111.0(2) . . ? O7 P3 O9 112.58(19) . . ? O8 P3 O9 109.9(2) . . ? O7 P3 C9 107.2(2) . . ? O8 P3 C9 108.1(2) . . ? O9 P3 C9 107.8(2) . . ? N2 N1 C13 107.5(4) . . ? N2 N1 Cu3 115.1(3) . . ? C13 N1 Cu3 137.0(4) . . ? N1 N2 C15 109.9(4) . . ? N1 N2 Cu2 129.8(3) . . ? C15 N2 Cu2 120.3(4) . . ? C20 N3 C16 118.9(5) . . ? C20 N3 Cu2 126.8(4) . . ? C16 N3 Cu2 114.3(4) . . ? C21 N4 N5 107.2(4) . . ? C21 N4 Cu4 136.1(4) . . ? N5 N4 Cu4 115.8(3) . . ? C23 N5 N4 109.0(4) . . ? C23 N5 Cu5 121.3(3) . . ? N4 N5 Cu5 129.5(3) . . ? C28 N6 C24 118.7(5) . . ? C28 N6 Cu5 127.1(4) . . ? C24 N6 Cu5 114.1(3) . . ? P1 O1 Cu3 135.76(19) . 2_665 ? P1 O1 Cu1 95.72(16) . . ? Cu3 O1 Cu1 128.43(16) 2_665 . ? P1 O2 Cu4 135.55(19) . . ? P1 O2 Cu1 95.23(16) . . ? Cu4 O2 Cu1 129.05(16) . . ? P1 O3 Cu1 134.31(19) . 2_665 ? P2 O4 Cu1 134.2(2) . . ? P2 O5 Cu2 117.9(2) . . ? P2 O6 Cu4 124.1(2) . . ? P3 O7 Cu3 120.7(2) . . ? P3 O8 Cu5 120.8(2) . . ? P3 O9 Cu1 133.2(2) . 2_665 ? Cu2 O10 Cu3 122.5(2) . . ? Cu4 O11 Cu5 122.7(2) . . ? Cu4 O11 Cu3 95.84(14) . . ? Cu5 O11 Cu3 95.91(15) . . ? C51 O51 Cu5 119.2(3) . . ? C4 C1 C3 110.1(4) . . ? C4 C1 C2 109.8(4) . . ? C3 C1 C2 109.5(4) . . ? C4 C1 P1 109.1(3) . . ? C3 C1 P1 109.0(3) . . ? C2 C1 P1 109.4(3) . . ? C6 C5 C7 109.4(5) . . ? C6 C5 C8 108.9(5) . . ? C7 C5 C8 109.8(5) . . ? C6 C5 P2 109.2(4) . . ? C7 C5 P2 109.5(4) . . ? C8 C5 P2 110.1(4) . . ? C12 C9 C11 109.5(5) . . ? C12 C9 C10 110.5(4) . . ? C11 C9 C10 109.2(5) . . ? C12 C9 P3 110.0(3) . . ? C11 C9 P3 107.8(4) . . ? C10 C9 P3 109.8(4) . . ? N1 C13 C14 110.3(5) . . ? C13 C14 C15 104.0(5) . . ? N2 C15 C14 108.2(5) . . ? N2 C15 C16 113.8(5) . . ? C14 C15 C16 138.0(5) . . ? N3 C16 C17 121.5(6) . . ? N3 C16 C15 112.8(5) . . ? C17 C16 C15 125.7(6) . . ? C18 C17 C16 119.3(7) . . ? C19 C18 C17 119.8(6) . . ? C18 C19 C20 119.0(6) . . ? N3 C20 C19 121.5(6) . . ? N4 C21 C22 110.0(5) . . ? C23 C22 C21 104.4(5) . . ? N5 C23 C22 109.4(5) . . ? N5 C23 C24 112.7(5) . . ? C22 C23 C24 137.7(5) . . ? N6 C24 C25 122.1(5) . . ? N6 C24 C23 113.2(4) . . ? C25 C24 C23 124.6(5) . . ? C24 C25 C26 118.4(6) . . ? C27 C26 C25 119.3(5) . . ? C26 C27 C28 119.1(5) . . ? N6 C28 C27 122.3(6) . . ? C56 O56 O57 125.3(11) . . ? _diffrn_measured_fraction_theta_max 0.897 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.897 _refine_diff_density_max 2.163 _refine_diff_density_min -1.713 _refine_diff_density_rms 0.166 #===END