# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Damir Safin' _publ_contact_author_email damir.safin@ksu.ru _publ_section_title ; Homoleptic polynuclear CuI and AgI complexes of N-thiophosphorylated thioureas o-RO(O)CC6H4NHC(S)NHP(S)(OiPr)2 (R = Me, Et) ; _publ_author_name D.Safin # Attachment '- [Cu3LI3].cif' data_safin66 _database_code_depnum_ccdc_archive 'CCDC 805255' #TrackingRef '- [Cu3LI3].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H66 Cu3 N6 O12 P3 S6' _chemical_formula_sum 'C45 H66 Cu3 N6 O12 P3 S6' _chemical_formula_weight 1358.93 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 17.6497(2) _cell_length_b 17.6497(2) _cell_length_c 34.4980(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 9306.8(2) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8105 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 31.9 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4212 _exptl_absorpt_coefficient_mu 1.356 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7027 _exptl_absorpt_correction_T_max 0.7732 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(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 'Siemens CCD three-circle diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 25686 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 30.51 _reflns_number_total 6312 _reflns_number_gt 4817 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP (Sheldrick, 2008)' _computing_publication_material SHELXL97 _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^)+(0.0578P)^2^+0.6940P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6312 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0960 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 0.335146(12) 0.546487(13) 0.419743(6) 0.02597(7) Uani 1 1 d . . . P1 P 0.46974(3) 0.49042(3) 0.415558(13) 0.02446(10) Uani 1 1 d . . . S1 S 0.36196(3) 0.44811(3) 0.446992(14) 0.03080(11) Uani 1 1 d . . . S2 S 0.45661(2) 0.67017(2) 0.402825(14) 0.02523(10) Uani 1 1 d . . . N1 N 0.54731(8) 0.58916(8) 0.42360(4) 0.0257(3) Uani 1 1 d . . . N2 N 0.61781(8) 0.73941(9) 0.42991(4) 0.0252(3) Uani 1 1 d . . . H2 H 0.6176(13) 0.7828(13) 0.4224(6) 0.029(5) Uiso 1 1 d . . . O1 O 0.45424(8) 0.48177(8) 0.37070(4) 0.0316(3) Uani 1 1 d . . . O2 O 0.51055(8) 0.43043(8) 0.42281(4) 0.0304(3) Uani 1 1 d . . . O3 O 0.71015(9) 0.89821(9) 0.39769(4) 0.0417(3) Uani 1 1 d . . . O4 O 0.85463(8) 0.95591(9) 0.39445(4) 0.0408(3) Uani 1 1 d . . . C1 C 0.54620(10) 0.66186(10) 0.42057(5) 0.0226(3) Uani 1 1 d . . . C2 C 0.39166(15) 0.39599(13) 0.35342(6) 0.0432(5) Uani 1 1 d . . . H2A H 0.3602 0.3531 0.3747 0.052 Uiso 1 1 calc R . . C3 C 0.4445(3) 0.3661(2) 0.33047(11) 0.1009(13) Uani 1 1 d . . . H3A H 0.4846 0.3593 0.3478 0.151 Uiso 1 1 calc R . . H3B H 0.4782 0.4096 0.3105 0.151 Uiso 1 1 calc R . . H3C H 0.4051 0.3099 0.3181 0.151 Uiso 1 1 calc R . . C4 C 0.32725(16) 0.40824(16) 0.33035(7) 0.0551(6) Uani 1 1 d . . . H4A H 0.2957 0.4273 0.3475 0.083 Uiso 1 1 calc R . . H4B H 0.2856 0.3528 0.3180 0.083 Uiso 1 1 calc R . . H4C H 0.3581 0.4527 0.3104 0.083 Uiso 1 1 calc R . . C5 C 0.52154(13) 0.40384(13) 0.46147(6) 0.0374(4) Uani 1 1 d . . . H5 H 0.5096 0.4377 0.4814 0.045 Uiso 1 1 calc R . . C6 C 0.45624(17) 0.30778(15) 0.46571(8) 0.0575(6) Uani 1 1 d . . . H6A H 0.3968 0.2985 0.4634 0.086 Uiso 1 1 calc R . . H6B H 0.4634 0.2874 0.4912 0.086 Uiso 1 1 calc R . . H6C H 0.4661 0.2750 0.4453 0.086 Uiso 1 1 calc R . . C7 C 0.61508(16) 0.42529(17) 0.46457(8) 0.0578(7) Uani 1 1 d . . . H7A H 0.6539 0.4885 0.4616 0.087 Uiso 1 1 calc R . . H7B H 0.6276 0.3945 0.4441 0.087 Uiso 1 1 calc R . . H7C H 0.6248 0.4068 0.4900 0.087 Uiso 1 1 calc R . . C11 C 0.69981(10) 0.75334(10) 0.44293(5) 0.0237(3) Uani 1 1 d . . . C12 C 0.77714(10) 0.83026(10) 0.43261(5) 0.0251(3) Uani 1 1 d . . . C13 C 0.85752(11) 0.84352(12) 0.44644(5) 0.0313(4) Uani 1 1 d . . . H13 H 0.9098 0.8952 0.4394 0.038 Uiso 1 1 calc R . . C14 C 0.86229(12) 0.78325(13) 0.47007(5) 0.0356(4) Uani 1 1 d . . . H14 H 0.9173 0.7929 0.4790 0.043 Uiso 1 1 calc R . . C15 C 0.78594(12) 0.70830(12) 0.48065(6) 0.0351(4) Uani 1 1 d . . . H15 H 0.7888 0.6667 0.4971 0.042 Uiso 1 1 calc R . . C16 C 0.70521(11) 0.69323(11) 0.46753(5) 0.0303(4) Uani 1 1 d . . . H16 H 0.6534 0.6418 0.4753 0.036 Uiso 1 1 calc R . . C17 C 0.77524(11) 0.89681(11) 0.40698(5) 0.0286(3) Uani 1 1 d . . . C18 C 0.85731(15) 1.02257(15) 0.36889(7) 0.0517(6) Uani 1 1 d . . . H18A H 0.8181 0.9945 0.3468 0.078 Uiso 1 1 calc R . . H18B H 0.9172 1.0599 0.3595 0.078 Uiso 1 1 calc R . . H18C H 0.8384 1.0583 0.3831 0.078 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 0.01927(10) 0.02441(11) 0.03504(13) -0.00050(8) 0.00005(8) 0.01152(8) P1 0.02123(19) 0.01953(18) 0.0330(2) -0.00046(16) -0.00111(16) 0.01049(15) S1 0.02299(19) 0.0276(2) 0.0415(3) 0.00871(17) 0.00324(17) 0.01243(16) S2 0.01947(17) 0.01955(17) 0.0374(2) -0.00102(15) -0.00265(15) 0.01031(14) N1 0.0183(6) 0.0215(6) 0.0378(8) -0.0021(6) -0.0015(5) 0.0103(5) N2 0.0174(6) 0.0191(6) 0.0375(8) 0.0011(6) -0.0005(5) 0.0081(5) O1 0.0333(6) 0.0250(6) 0.0336(7) -0.0022(5) -0.0034(5) 0.0126(5) O2 0.0321(6) 0.0252(6) 0.0397(7) -0.0003(5) -0.0001(5) 0.0187(5) O3 0.0302(7) 0.0332(7) 0.0602(9) 0.0154(6) 0.0065(6) 0.0147(6) O4 0.0272(6) 0.0340(7) 0.0419(8) 0.0077(6) 0.0014(5) 0.0008(5) C1 0.0189(7) 0.0214(7) 0.0264(8) 0.0001(6) 0.0016(6) 0.0094(6) C2 0.0506(12) 0.0277(9) 0.0443(12) -0.0085(8) -0.0166(9) 0.0143(9) C3 0.103(3) 0.100(3) 0.118(3) -0.074(2) -0.033(2) 0.064(2) C4 0.0533(13) 0.0489(13) 0.0459(13) 0.0041(10) -0.0178(10) 0.0128(11) C5 0.0415(10) 0.0397(10) 0.0436(11) -0.0020(8) -0.0061(8) 0.0297(9) C6 0.0642(15) 0.0432(12) 0.0774(17) 0.0217(12) 0.0188(13) 0.0360(12) C7 0.0476(13) 0.0647(15) 0.0790(18) -0.0239(13) -0.0241(12) 0.0416(12) C11 0.0194(7) 0.0238(7) 0.0278(8) -0.0038(6) -0.0005(6) 0.0107(6) C12 0.0205(7) 0.0257(7) 0.0255(8) -0.0041(6) 0.0015(6) 0.0088(6) C13 0.0210(7) 0.0350(9) 0.0315(9) -0.0058(7) 0.0005(6) 0.0093(7) C14 0.0241(8) 0.0484(11) 0.0355(10) -0.0065(8) -0.0058(7) 0.0190(8) C15 0.0312(9) 0.0376(10) 0.0386(10) -0.0006(8) -0.0058(7) 0.0187(8) C16 0.0244(8) 0.0279(8) 0.0366(10) 0.0015(7) -0.0021(7) 0.0116(6) C17 0.0244(7) 0.0247(8) 0.0292(9) -0.0031(6) 0.0022(6) 0.0065(6) C18 0.0457(12) 0.0397(11) 0.0437(12) 0.0135(9) 0.0008(10) 0.0018(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 S2 2.1981(4) 3_565 ? Cu1 S1 2.2236(5) . ? Cu1 S2 2.2410(4) . ? P1 O1 1.5656(13) . ? P1 O2 1.5699(12) . ? P1 N1 1.6132(14) . ? P1 S1 1.9829(6) . ? S2 C1 1.7687(16) . ? S2 Cu1 2.1981(4) 2_665 ? N1 C1 1.2972(19) . ? N2 C1 1.3582(19) . ? N2 C11 1.415(2) . ? N2 H2 0.81(2) . ? O1 C2 1.482(2) . ? O2 C5 1.459(2) . ? O3 C17 1.205(2) . ? O4 C17 1.333(2) . ? O4 C18 1.452(3) . ? C2 C4 1.489(3) . ? C2 C3 1.506(4) . ? C2 H2A 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.502(3) . ? C5 C6 1.507(3) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C11 C16 1.398(2) . ? C11 C12 1.407(2) . ? C12 C13 1.401(2) . ? C12 C17 1.484(2) . ? C13 C14 1.376(3) . ? C13 H13 0.9500 . ? C14 C15 1.384(3) . ? C14 H14 0.9500 . ? C15 C16 1.388(2) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? 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 S2 Cu1 S1 132.780(17) 3_565 . ? S2 Cu1 S2 113.68(2) 3_565 . ? S1 Cu1 S2 113.407(17) . . ? O1 P1 O2 102.04(7) . . ? O1 P1 N1 106.72(7) . . ? O2 P1 N1 105.87(7) . . ? O1 P1 S1 114.57(5) . . ? O2 P1 S1 109.64(5) . . ? N1 P1 S1 116.68(6) . . ? P1 S1 Cu1 90.77(2) . . ? C1 S2 Cu1 115.82(5) . 2_665 ? C1 S2 Cu1 106.77(5) . . ? Cu1 S2 Cu1 113.007(19) 2_665 . ? C1 N1 P1 129.08(12) . . ? C1 N2 C11 127.31(14) . . ? C1 N2 H2 115.7(14) . . ? C11 N2 H2 115.2(15) . . ? C2 O1 P1 120.13(12) . . ? C5 O2 P1 122.85(11) . . ? C17 O4 C18 115.26(16) . . ? N1 C1 N2 120.73(14) . . ? N1 C1 S2 124.48(12) . . ? N2 C1 S2 114.74(11) . . ? O1 C2 C4 107.45(16) . . ? O1 C2 C3 107.1(2) . . ? C4 C2 C3 114.9(2) . . ? O1 C2 H2A 109.1 . . ? C4 C2 H2A 109.1 . . ? C3 C2 H2A 109.1 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2 C5 C7 106.87(18) . . ? O2 C5 C6 107.52(17) . . ? C7 C5 C6 113.75(18) . . ? O2 C5 H5 109.5 . . ? C7 C5 H5 109.5 . . ? C6 C5 H5 109.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C16 C11 C12 118.97(15) . . ? C16 C11 N2 120.85(14) . . ? C12 C11 N2 120.12(14) . . ? C13 C12 C11 119.19(16) . . ? C13 C12 C17 119.50(15) . . ? C11 C12 C17 121.31(15) . . ? C14 C13 C12 121.39(17) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 119.23(17) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C14 C15 C16 120.84(17) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C11 120.35(16) . . ? C15 C16 H16 119.8 . . ? C11 C16 H16 119.8 . . ? O3 C17 O4 122.53(17) . . ? O3 C17 C12 125.02(15) . . ? O4 C17 C12 112.44(15) . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 P1 S1 Cu1 -60.89(5) . . . . ? O2 P1 S1 Cu1 -174.89(5) . . . . ? N1 P1 S1 Cu1 64.83(6) . . . . ? S2 Cu1 S1 P1 144.29(2) 3_565 . . . ? S2 Cu1 S1 P1 -31.19(3) . . . . ? S2 Cu1 S2 C1 177.64(5) 3_565 . . . ? S1 Cu1 S2 C1 -5.98(6) . . . . ? S2 Cu1 S2 Cu1 49.16(4) 3_565 . . 2_665 ? S1 Cu1 S2 Cu1 -134.47(2) . . . 2_665 ? O1 P1 N1 C1 70.11(17) . . . . ? O2 P1 N1 C1 178.28(15) . . . . ? S1 P1 N1 C1 -59.45(17) . . . . ? O2 P1 O1 C2 64.02(15) . . . . ? N1 P1 O1 C2 174.87(13) . . . . ? S1 P1 O1 C2 -54.37(15) . . . . ? O1 P1 O2 C5 -168.14(13) . . . . ? N1 P1 O2 C5 80.36(14) . . . . ? S1 P1 O2 C5 -46.30(14) . . . . ? P1 N1 C1 N2 177.75(13) . . . . ? P1 N1 C1 S2 -4.7(2) . . . . ? C11 N2 C1 N1 1.0(3) . . . . ? C11 N2 C1 S2 -176.76(13) . . . . ? Cu1 S2 C1 N1 159.05(12) 2_665 . . . ? Cu1 S2 C1 N1 32.22(15) . . . . ? Cu1 S2 C1 N2 -23.29(14) 2_665 . . . ? Cu1 S2 C1 N2 -150.12(11) . . . . ? P1 O1 C2 C4 124.93(17) . . . . ? P1 O1 C2 C3 -111.1(2) . . . . ? P1 O2 C5 C7 -128.56(14) . . . . ? P1 O2 C5 C6 108.96(16) . . . . ? C1 N2 C11 C16 -36.4(3) . . . . ? C1 N2 C11 C12 146.39(17) . . . . ? C16 C11 C12 C13 1.6(2) . . . . ? N2 C11 C12 C13 178.78(15) . . . . ? C16 C11 C12 C17 -179.28(15) . . . . ? N2 C11 C12 C17 -2.1(2) . . . . ? C11 C12 C13 C14 -0.4(3) . . . . ? C17 C12 C13 C14 -179.60(16) . . . . ? C12 C13 C14 C15 -0.6(3) . . . . ? C13 C14 C15 C16 0.4(3) . . . . ? C14 C15 C16 C11 0.7(3) . . . . ? C12 C11 C16 C15 -1.7(3) . . . . ? N2 C11 C16 C15 -178.92(16) . . . . ? C18 O4 C17 O3 0.3(3) . . . . ? C18 O4 C17 C12 179.44(16) . . . . ? C13 C12 C17 O3 -169.50(18) . . . . ? C11 C12 C17 O3 11.4(3) . . . . ? C13 C12 C17 O4 11.4(2) . . . . ? C11 C12 C17 O4 -167.78(15) . . . . ? 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 N2 H2 O3 0.81(2) 2.05(2) 2.6794(19) 133.8(19) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.489 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.077 # Attachment '- [Ag4LI4].cif' data_safin81 _database_code_depnum_ccdc_archive 'CCDC 813939' #TrackingRef '- [Ag4LI4].cif' # start Validation Reply Form _vrf_PLAT220_I ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.03 Ratio RESPONSE: The isopropyl group is disordered. ; _vrf_PLAT242_I ; PROBLEM: Check Low Ueq as Compared to Neighbors for C5 RESPONSE: The isopropyl group is disordered. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H88 Ag4 N8 O16 P4 S8' _chemical_formula_sum 'C60 H88 Ag4 N8 O16 P4 S8' _chemical_formula_weight 1989.22 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' Ag Ag -0.8971 1.1015 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I41/a _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x, y+1/2, -z' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 27.4538(9) _cell_length_b 27.4538(9) _cell_length_c 10.7505(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8102.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4032 _exptl_absorpt_coefficient_mu 1.301 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7368 _exptl_absorpt_correction_T_max 0.7901 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The bond lengths and angles of the following atoms are restrained to be equal. SAME O2 > C7 SAME O2' > C7' O1 5 0.566377 0.656348 0.477186 11.00000 0.05570 0.06473 = 0.06157 0.00857 0.00812 -0.01514 C2 1 0.520949 0.630062 0.466553 11.00000 0.06611 0.08742 = 0.06770 0.00759 0.01536 -0.03337 AFIX 13 H2A 2 0.512695 0.626213 0.376489 11.00000 -1.20000 AFIX 0 C3 1 0.524982 0.581113 0.524080 11.00000 0.13533 0.08188 = 0.16842 0.02564 0.07401 -0.02688 AFIX 33 H3A 2 0.550029 0.562211 0.480624 11.00000 -1.50000 H3B 2 0.493616 0.564253 0.517751 11.00000 -1.50000 H3C 2 0.533965 0.584539 0.611870 11.00000 -1.50000 AFIX 0 C4 1 0.483303 0.661789 0.527021 11.00000 0.06093 0.13095 = 0.08383 0.02428 0.01394 -0.00089 AFIX 33 H4A 2 0.482122 0.693326 0.484423 11.00000 -1.50000 H4B 2 0.491821 0.666784 0.614623 11.00000 -1.50000 H4C 2 0.451366 0.645988 0.521528 11.00000 -1.50000 AFIX 0 PART 1 O2 5 0.645584 0.624178 0.517892 31.00000 0.06875 C5 1 0.698504 0.619364 0.506694 31.00000 0.08169 AFIX 13 H5 2 0.710775 0.639082 0.435034 31.00000 -1.20000 AFIX 0 C6 1 0.710261 0.566882 0.488391 31.00000 0.22518 AFIX 33 H6A 2 0.699412 0.556577 0.405628 31.00000 -1.50000 H6B 2 0.693584 0.547449 0.551898 31.00000 -1.50000 H6C 2 0.745522 0.562094 0.495604 31.00000 -1.50000 AFIX 0 C7 1 0.718136 0.639160 0.627718 31.00000 0.12083 AFIX 33 H7A 2 0.711179 0.674110 0.633050 31.00000 -1.50000 H7B 2 0.753423 0.633950 0.631201 31.00000 -1.50000 H7C 2 0.702550 0.622273 0.697474 31.00000 -1.50000 AFIX 0 PART 2 O2' 5 0.648017 0.610207 0.458717 -31.00000 0.04501 C5' 1 0.670234 0.623283 0.576100 -31.00000 0.06329 AFIX 13 H5' 2 0.666597 0.659274 0.586996 -31.00000 -1.20000 AFIX 0 C6' 1 0.643866 0.599047 0.680031 -31.00000 0.09639 AFIX 33 H6'1 2 0.609302 0.607876 0.676748 -31.00000 -1.50000 H6'2 2 0.657709 0.609665 0.759560 -31.00000 -1.50000 H6'3 2 0.647224 0.563640 0.672218 -31.00000 -1.50000 AFIX 0 C7' 1 0.723441 0.612226 0.567817 -31.00000 0.11633 AFIX 33 H7'1 2 0.737385 0.629024 0.495694 -31.00000 -1.50000 H7'2 2 0.728079 0.577017 0.558592 -31.00000 -1.50000 H7'3 2 0.739747 0.623388 0.643735 -31.00000 -1.50000 AFIX 0 PART 0 ; _diffrn_ambient_temperature 173(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 'Siemens CCD three-circle diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 75564 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 26.36 _reflns_number_total 4145 _reflns_number_gt 3086 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP (Sheldrick, 2008)' _computing_publication_material SHELXL97 _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^)+(0.0411P)^2^+81.4871P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4145 _refine_ls_number_parameters 220 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1374 _refine_ls_wR_factor_gt 0.1237 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.048 _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 C1 C 0.62708(18) 0.74056(19) 0.3431(5) 0.0372(11) Uani 1 1 d . . . Ag1 Ag 0.555372(17) 0.678061(18) 0.14567(5) 0.05450(18) Uani 1 1 d . . . P1 P 0.61384(6) 0.64871(6) 0.39990(19) 0.0579(5) Uani 1 1 d . . . S1 S 0.60559(7) 0.61365(6) 0.2435(2) 0.0720(6) Uani 1 1 d . A . S2 S 0.56837(5) 0.75136(5) 0.28178(15) 0.0442(3) Uani 1 1 d . . . N1 N 0.64136(16) 0.70070(17) 0.3936(5) 0.0453(11) Uani 1 1 d . A . N2 N 0.65711(15) 0.77981(15) 0.3384(4) 0.0412(11) Uani 1 1 d . . . H2 H 0.6437 0.8066 0.3095 0.049 Uiso 1 1 calc R . . O1 O 0.56638(15) 0.65635(16) 0.4772(4) 0.0607(12) Uani 1 1 d D A . C2 C 0.5209(3) 0.6301(3) 0.4666(7) 0.074(2) Uani 1 1 d D . . H2A H 0.5127 0.6263 0.3765 0.088 Uiso 1 1 calc R A . C3 C 0.5250(4) 0.5811(3) 0.5239(12) 0.129(4) Uani 1 1 d D A . H3A H 0.5500 0.5622 0.4804 0.193 Uiso 1 1 calc R . . H3B H 0.4936 0.5643 0.5175 0.193 Uiso 1 1 calc R . . H3C H 0.5339 0.5845 0.6117 0.193 Uiso 1 1 calc R . . C4 C 0.4833(3) 0.6618(3) 0.5270(8) 0.092(3) Uani 1 1 d D A . H4A H 0.4821 0.6933 0.4844 0.138 Uiso 1 1 calc R . . H4B H 0.4918 0.6668 0.6146 0.138 Uiso 1 1 calc R . . H4C H 0.4514 0.6460 0.5215 0.138 Uiso 1 1 calc R . . O2 O 0.6456(3) 0.6242(4) 0.5179(12) 0.069(3) Uiso 0.499(11) 1 d PD A 1 C5 C 0.6985(5) 0.6194(6) 0.5067(15) 0.082(5) Uiso 0.499(11) 1 d PD A 1 H5 H 0.7108 0.6391 0.4351 0.098 Uiso 0.499(11) 1 calc PR A 1 C6 C 0.7103(12) 0.5669(9) 0.488(3) 0.225(18) Uiso 0.499(11) 1 d PD A 1 H6A H 0.6994 0.5566 0.4056 0.338 Uiso 0.499(11) 1 calc PR A 1 H6B H 0.6936 0.5475 0.5519 0.338 Uiso 0.499(11) 1 calc PR A 1 H6C H 0.7456 0.5621 0.4956 0.338 Uiso 0.499(11) 1 calc PR A 1 C7 C 0.7182(8) 0.6391(8) 0.6277(19) 0.121(8) Uiso 0.499(11) 1 d PD A 1 H7A H 0.7112 0.6741 0.6331 0.181 Uiso 0.499(11) 1 calc PR A 1 H7B H 0.7534 0.6339 0.6311 0.181 Uiso 0.499(11) 1 calc PR A 1 H7C H 0.7026 0.6222 0.6975 0.181 Uiso 0.499(11) 1 calc PR A 1 O2' O 0.6480(3) 0.6102(3) 0.4587(8) 0.045(2) Uiso 0.501(11) 1 d PD A 2 C5' C 0.6703(5) 0.6233(5) 0.5761(11) 0.063(4) Uiso 0.501(11) 1 d PD A 2 H5' H 0.6666 0.6593 0.5870 0.076 Uiso 0.501(11) 1 calc PR A 2 C6' C 0.6439(6) 0.5990(7) 0.6801(15) 0.097(6) Uiso 0.501(11) 1 d PD A 2 H6'1 H 0.6093 0.6078 0.6768 0.145 Uiso 0.501(11) 1 calc PR A 2 H6'2 H 0.6578 0.6096 0.7596 0.145 Uiso 0.501(11) 1 calc PR A 2 H6'3 H 0.6473 0.5636 0.6723 0.145 Uiso 0.501(11) 1 calc PR A 2 C7' C 0.7234(6) 0.6122(9) 0.568(2) 0.116(7) Uiso 0.501(11) 1 d PD A 2 H7'1 H 0.7374 0.6290 0.4958 0.174 Uiso 0.501(11) 1 calc PR A 2 H7'2 H 0.7281 0.5770 0.5587 0.174 Uiso 0.501(11) 1 calc PR A 2 H7'3 H 0.7397 0.6233 0.6439 0.174 Uiso 0.501(11) 1 calc PR A 2 C11 C 0.7061(2) 0.7841(2) 0.3726(5) 0.0433(13) Uani 1 1 d . B . C12 C 0.7291(3) 0.8292(3) 0.3571(7) 0.069(2) Uani 1 1 d . . . C13 C 0.7788(3) 0.8333(4) 0.3846(8) 0.088(3) Uani 1 1 d . B . H13 H 0.7950 0.8633 0.3692 0.106 Uiso 1 1 calc R . . C14 C 0.8044(3) 0.7956(4) 0.4325(8) 0.082(2) Uani 1 1 d . . . H14 H 0.8376 0.7998 0.4555 0.098 Uiso 1 1 calc R B . C15 C 0.7823(2) 0.7517(3) 0.4473(8) 0.074(2) Uani 1 1 d . B . H15 H 0.8002 0.7249 0.4795 0.089 Uiso 1 1 calc R . . C16 C 0.7334(2) 0.7457(2) 0.4158(7) 0.0594(18) Uani 1 1 d . . . H16 H 0.7187 0.7145 0.4242 0.071 Uiso 1 1 calc R B . O3 O 0.6509(3) 0.8758(3) 0.3189(9) 0.053(2) Uiso 0.529(10) 1 d P B 1 O4 O 0.7220(4) 0.9167(4) 0.3230(11) 0.081(3) Uiso 0.529(10) 1 d P B 1 C17 C 0.6932(5) 0.8763(5) 0.3344(14) 0.056(3) Uiso 0.529(10) 1 d P B 1 C18 C 0.6928(7) 0.9604(7) 0.289(2) 0.111(7) Uiso 0.529(10) 1 d P B 1 H18A H 0.7077 0.9895 0.3258 0.166 Uiso 0.529(10) 1 calc PR B 1 H18B H 0.6595 0.9567 0.3213 0.166 Uiso 0.529(10) 1 calc PR B 1 H18C H 0.6918 0.9637 0.1986 0.166 Uiso 0.529(10) 1 calc PR B 1 O3' O 0.6684(3) 0.8732(3) 0.2652(9) 0.044(2) Uiso 0.471(10) 1 d P B 2 O4' O 0.7451(4) 0.8992(4) 0.2537(12) 0.081(4) Uiso 0.471(10) 1 d P B 2 C17' C 0.7109(5) 0.8660(5) 0.2916(13) 0.045(3) Uiso 0.471(10) 1 d P B 2 C18' C 0.7225(8) 0.9430(7) 0.199(2) 0.101(7) Uiso 0.471(10) 1 d P B 2 H18D H 0.7468 0.9606 0.1491 0.152 Uiso 0.471(10) 1 calc PR B 2 H18E H 0.7105 0.9642 0.2652 0.152 Uiso 0.471(10) 1 calc PR B 2 H18F H 0.6953 0.9333 0.1451 0.152 Uiso 0.471(10) 1 calc PR B 2 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 C1 0.034(3) 0.041(3) 0.036(3) -0.005(2) 0.001(2) -0.001(2) Ag1 0.0490(3) 0.0631(3) 0.0514(3) -0.0134(2) 0.0063(2) -0.0214(2) P1 0.0456(9) 0.0469(9) 0.0812(13) 0.0278(9) 0.0078(8) -0.0025(7) S1 0.0695(11) 0.0356(8) 0.1108(16) -0.0009(9) 0.0361(11) -0.0024(7) S2 0.0349(7) 0.0405(7) 0.0572(9) -0.0065(6) -0.0097(6) 0.0037(6) N1 0.039(2) 0.044(3) 0.052(3) 0.019(2) -0.002(2) -0.003(2) N2 0.038(2) 0.030(2) 0.055(3) -0.001(2) -0.008(2) -0.0016(18) O1 0.056(3) 0.065(3) 0.061(3) 0.009(2) 0.008(2) -0.015(2) C2 0.066(4) 0.087(5) 0.068(5) 0.008(4) 0.015(4) -0.033(4) C3 0.136(9) 0.082(6) 0.169(11) 0.026(7) 0.074(8) -0.027(6) C4 0.061(5) 0.131(8) 0.084(6) 0.024(6) 0.014(4) -0.001(5) C11 0.038(3) 0.050(3) 0.041(3) -0.004(3) -0.006(2) -0.006(2) C12 0.068(4) 0.071(4) 0.069(5) 0.015(4) -0.023(4) -0.033(4) C13 0.069(5) 0.109(7) 0.087(6) 0.020(5) -0.021(4) -0.048(5) C14 0.039(4) 0.122(7) 0.084(6) -0.016(5) -0.003(4) -0.020(4) C15 0.037(3) 0.087(5) 0.098(6) -0.028(5) -0.008(4) 0.010(3) C16 0.037(3) 0.056(4) 0.085(5) -0.018(3) -0.011(3) 0.009(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 C1 N1 1.283(7) . ? C1 N2 1.358(6) . ? C1 S2 1.766(5) . ? Ag1 S2 2.4183(16) 14_565 ? Ag1 S1 2.477(2) . ? Ag1 S2 2.5135(15) . ? P1 O2' 1.549(8) . ? P1 O1 1.560(5) . ? P1 N1 1.616(5) . ? P1 O2 1.680(11) . ? P1 S1 1.951(3) . ? S2 Ag1 2.4183(16) 12_766 ? N2 C11 1.401(7) . ? N2 H2 0.8800 . ? O1 C2 1.445(7) . ? C2 C3 1.483(11) . ? C2 C4 1.499(10) . ? C2 H2A 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? O2 C5 1.464(13) . ? C5 C6 1.489(18) . ? C5 C7 1.509(16) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? O2' C5' 1.447(13) . ? C5' C6' 1.489(15) . ? C5' C7' 1.494(15) . ? C5' H5' 1.0000 . ? C6' H6'1 0.9800 . ? C6' H6'2 0.9800 . ? C6' H6'3 0.9800 . ? C7' H7'1 0.9800 . ? C7' H7'2 0.9800 . ? C7' H7'3 0.9800 . ? C11 C16 1.375(8) . ? C11 C12 1.398(8) . ? C12 C17' 1.330(14) . ? C12 C13 1.402(10) . ? C12 C17 1.643(16) . ? C13 C14 1.350(12) . ? C13 H13 0.9500 . ? C14 C15 1.361(11) . ? C14 H14 0.9500 . ? C15 C16 1.393(8) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? O3 C17 1.173(15) . ? O4 C17 1.369(16) . ? O4 C18 1.49(2) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O3' C17' 1.217(15) . ? O4' C17' 1.370(17) . ? O4' C18' 1.48(2) . ? C18' H18D 0.9800 . ? C18' H18E 0.9800 . ? C18' H18F 0.9800 . ? 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 N1 C1 N2 120.5(5) . . ? N1 C1 S2 125.4(4) . . ? N2 C1 S2 114.0(4) . . ? S2 Ag1 S1 134.85(6) 14_565 . ? S2 Ag1 S2 120.92(6) 14_565 . ? S1 Ag1 S2 104.21(6) . . ? O2' P1 O1 112.4(4) . . ? O2' P1 N1 109.7(3) . . ? O1 P1 N1 107.1(3) . . ? O2' P1 O2 26.3(4) . . ? O1 P1 O2 94.9(4) . . ? N1 P1 O2 98.2(4) . . ? O2' P1 S1 94.9(4) . . ? O1 P1 S1 115.4(2) . . ? N1 P1 S1 117.0(2) . . ? O2 P1 S1 120.9(4) . . ? P1 S1 Ag1 94.49(8) . . ? C1 S2 Ag1 111.13(19) . 12_766 ? C1 S2 Ag1 102.27(18) . . ? Ag1 S2 Ag1 92.14(5) 12_766 . ? C1 N1 P1 128.9(4) . . ? C1 N2 C11 129.9(5) . . ? C1 N2 H2 115.1 . . ? C11 N2 H2 115.1 . . ? C2 O1 P1 127.7(5) . . ? O1 C2 C3 110.8(7) . . ? O1 C2 C4 105.7(6) . . ? C3 C2 C4 113.4(7) . . ? O1 C2 H2A 108.9 . . ? C3 C2 H2A 108.9 . . ? C4 C2 H2A 108.9 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C5 O2 P1 119.3(10) . . ? O2 C5 C6 108.3(16) . . ? O2 C5 C7 104.6(13) . . ? C6 C5 C7 112.6(17) . . ? O2 C5 H5 110.4 . . ? C6 C5 H5 110.4 . . ? C7 C5 H5 110.4 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5' O2' P1 116.3(8) . . ? O2' C5' C6' 109.8(11) . . ? O2' C5' C7' 108.1(12) . . ? C6' C5' C7' 115.3(13) . . ? O2' C5' H5' 107.8 . . ? C6' C5' H5' 107.8 . . ? C7' C5' H5' 107.8 . . ? C5' C6' H6'1 109.5 . . ? C5' C6' H6'2 109.5 . . ? H6'1 C6' H6'2 109.5 . . ? C5' C6' H6'3 109.5 . . ? H6'1 C6' H6'3 109.5 . . ? H6'2 C6' H6'3 109.5 . . ? C5' C7' H7'1 109.5 . . ? C5' C7' H7'2 109.5 . . ? H7'1 C7' H7'2 109.5 . . ? C5' C7' H7'3 109.5 . . ? H7'1 C7' H7'3 109.5 . . ? H7'2 C7' H7'3 109.5 . . ? C16 C11 C12 118.3(6) . . ? C16 C11 N2 123.1(5) . . ? C12 C11 N2 118.5(5) . . ? C17' C12 C11 124.5(8) . . ? C17' C12 C13 114.7(8) . . ? C11 C12 C13 119.0(7) . . ? C17' C12 C17 25.6(7) . . ? C11 C12 C17 116.3(7) . . ? C13 C12 C17 123.6(8) . . ? C14 C13 C12 121.8(7) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 119.3(7) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C14 C15 C16 120.5(7) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C11 C16 C15 121.0(6) . . ? C11 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C17 O4 C18 111.3(13) . . ? O3 C17 O4 124.6(12) . . ? O3 C17 C12 127.4(11) . . ? O4 C17 C12 107.7(10) . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17' O4' C18' 112.0(13) . . ? O3' C17' C12 127.3(11) . . ? O3' C17' O4' 118.7(12) . . ? C12 C17' O4' 114.0(11) . . ? O4' C18' H18D 109.5 . . ? O4' C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? O4' C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2' P1 S1 Ag1 -176.5(3) . . . . ? O1 P1 S1 Ag1 65.9(2) . . . . ? N1 P1 S1 Ag1 -61.5(2) . . . . ? O2 P1 S1 Ag1 179.0(4) . . . . ? S2 Ag1 S1 P1 -163.02(7) 14_565 . . . ? S2 Ag1 S1 P1 15.21(9) . . . . ? N1 C1 S2 Ag1 -146.7(5) . . . 12_766 ? N2 C1 S2 Ag1 36.2(4) . . . 12_766 ? N1 C1 S2 Ag1 -49.6(5) . . . . ? N2 C1 S2 Ag1 133.4(4) . . . . ? S2 Ag1 S2 C1 -153.72(19) 14_565 . . . ? S1 Ag1 S2 C1 27.7(2) . . . . ? S2 Ag1 S2 Ag1 -41.55(5) 14_565 . . 12_766 ? S1 Ag1 S2 Ag1 139.90(5) . . . 12_766 ? N2 C1 N1 P1 -174.6(4) . . . . ? S2 C1 N1 P1 8.5(8) . . . . ? O2' P1 N1 C1 174.1(6) . . . . ? O1 P1 N1 C1 -63.7(6) . . . . ? O2 P1 N1 C1 -161.5(6) . . . . ? S1 P1 N1 C1 67.6(6) . . . . ? N1 C1 N2 C11 6.1(9) . . . . ? S2 C1 N2 C11 -176.7(5) . . . . ? O2' P1 O1 C2 -88.6(7) . . . . ? N1 P1 O1 C2 150.9(5) . . . . ? O2 P1 O1 C2 -108.9(7) . . . . ? S1 P1 O1 C2 18.7(6) . . . . ? P1 O1 C2 C3 75.9(8) . . . . ? P1 O1 C2 C4 -160.8(5) . . . . ? O2' P1 O2 C5 60.4(12) . . . . ? O1 P1 O2 C5 -166.1(10) . . . . ? N1 P1 O2 C5 -58.0(10) . . . . ? S1 P1 O2 C5 70.4(11) . . . . ? P1 O2 C5 C6 -107.3(18) . . . . ? P1 O2 C5 C7 132.4(13) . . . . ? O1 P1 O2' C5' -67.8(8) . . . . ? N1 P1 O2' C5' 51.2(8) . . . . ? O2 P1 O2' C5' -16.4(10) . . . . ? S1 P1 O2' C5' 172.2(7) . . . . ? P1 O2' C5' C6' 101.5(12) . . . . ? P1 O2' C5' C7' -131.9(12) . . . . ? C1 N2 C11 C16 2.2(10) . . . . ? C1 N2 C11 C12 179.4(6) . . . . ? C16 C11 C12 C17' 164.3(10) . . . . ? N2 C11 C12 C17' -13.0(13) . . . . ? C16 C11 C12 C13 0.8(11) . . . . ? N2 C11 C12 C13 -176.6(7) . . . . ? C16 C11 C12 C17 -167.4(8) . . . . ? N2 C11 C12 C17 15.2(10) . . . . ? C17' C12 C13 C14 -169.1(11) . . . . ? C11 C12 C13 C14 -4.0(13) . . . . ? C17 C12 C13 C14 163.3(10) . . . . ? C12 C13 C14 C15 4.1(14) . . . . ? C13 C14 C15 C16 -1.2(13) . . . . ? C12 C11 C16 C15 2.1(10) . . . . ? N2 C11 C16 C15 179.3(6) . . . . ? C14 C15 C16 C11 -2.0(12) . . . . ? C18 O4 C17 O3 0(2) . . . . ? C18 O4 C17 C12 174.2(12) . . . . ? C17' C12 C17 O3 108(3) . . . . ? C11 C12 C17 O3 -7.2(19) . . . . ? C13 C12 C17 O3 -174.8(13) . . . . ? C17' C12 C17 O4 -65.3(18) . . . . ? C11 C12 C17 O4 179.3(9) . . . . ? C13 C12 C17 O4 11.7(15) . . . . ? C11 C12 C17' O3' 23(2) . . . . ? C13 C12 C17' O3' -173.2(13) . . . . ? C17 C12 C17' O3' -56.5(18) . . . . ? C11 C12 C17' O4' -158.9(10) . . . . ? C13 C12 C17' O4' 5.3(16) . . . . ? C17 C12 C17' O4' 122(2) . . . . ? C18' O4' C17' O3' 8(2) . . . . ? C18' O4' C17' C12 -171.1(14) . . . . ? 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 N2 H2 O3 0.88 1.91 2.650(9) 140.3 . N2 H2 O3' 0.88 2.01 2.699(9) 134.8 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.154 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.099 # Attachment '- [Cu3LII3].cif' data_ba1 _database_code_depnum_ccdc_archive 'CCDC 847766' #TrackingRef '- [Cu3LII3].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H72 Cu3 N6 O12 P3 S6' _chemical_formula_sum 'C48 H72 Cu3 N6 O12 P3 S6' _chemical_formula_weight 1401.01 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8107(4) _cell_length_b 19.7508(5) _cell_length_c 27.3802(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.034(3) _cell_angle_gamma 90.00 _cell_volume 6387.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 43842 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 26.9 _exptl_crystal_description block _exptl_crystal_colour 'light brown' _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.37 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2904 _exptl_absorpt_coefficient_mu 1.319 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6272 _exptl_absorpt_correction_T_max 0.6410 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; The bond lengths and angles of some disordered atoms were restrained to be equal. TITL Ba1 in P21/n CELL 0.71073 11.8107 19.7508 27.3802 90.000 90.034 90.000 ZERR 4.00 0.0004 0.0005 0.0010 0.000 0.003 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H Cu N O P S UNIT 192 288 12 24 48 12 24 TEMP-100 SIZE.39 .37 .37 REM light brown block ACTA50 CONF BOND$H HTAB HTAB N2 O3 HTAB N2A O3A HTAB N2B O3B L.S. 20 FMAP 2 PLAN 10 WGHT 0.0775 7.7716 FVAR 0.44606 0.75254 0.50073 0.50630 CU1 3 0.401128 0.817762 0.665430 11.00000 0.03874 0.03426 = 0.03658 -0.00054 -0.00690 0.00432 P1 6 0.637909 0.836428 0.713836 11.00000 0.03254 0.02762 = 0.03418 -0.00278 -0.00055 0.00011 S1 7 0.568580 0.866965 0.651857 11.00000 0.04505 0.03422 = 0.03373 0.00294 -0.00169 -0.00212 S2 7 0.403049 0.739310 0.724013 11.00000 0.02984 0.04080 = 0.04931 0.00995 -0.00531 -0.00110 N1 4 0.634247 0.756860 0.727434 11.00000 0.03175 0.03045 = 0.03539 0.00177 -0.00306 0.00015 N2 4 0.560062 0.652055 0.746493 11.00000 0.03276 0.03522 = 0.06110 0.01423 -0.01128 -0.00573 AFIX 43 H2 2 0.497604 0.627782 0.747188 11.00000 -1.20000 AFIX 0 SAME O2B C5B C6B C7B SAME O2B C5B C6" C7" SAME O2A C5A C6A C7A SAME O2A C5A C6' C7' O1 5 0.589741 0.880393 0.756695 11.00000 0.04762 0.04223 = 0.03319 -0.00876 -0.00131 0.00811 C2 1 0.631572 0.870980 0.806893 11.00000 0.06390 0.05383 = 0.03324 -0.00540 -0.00619 0.00663 AFIX 13 H2A 2 0.689962 0.834317 0.807184 11.00000 -1.20000 AFIX 0 C3 1 0.532306 0.849625 0.837722 11.00000 0.09158 0.08720 = 0.04038 -0.00325 0.00961 -0.00986 AFIX 33 H3A 2 0.502137 0.806651 0.825437 11.00000 -1.50000 H3B 2 0.473245 0.884409 0.836138 11.00000 -1.50000 H3C 2 0.556912 0.843914 0.871661 11.00000 -1.50000 AFIX 0 C4 1 0.685174 0.936347 0.822557 11.00000 0.09160 0.07386 = 0.04586 -0.01309 -0.01164 -0.01221 AFIX 33 H4A 2 0.749531 0.946527 0.801208 11.00000 -1.50000 H4B 2 0.711621 0.932263 0.856361 11.00000 -1.50000 H4C 2 0.629380 0.972945 0.820332 11.00000 -1.50000 AFIX 0 O2 5 0.767562 0.853979 0.715005 11.00000 0.03408 0.03055 = 0.05255 -0.00605 0.00039 -0.00296 O3 5 0.449257 0.567721 0.805459 11.00000 0.03828 0.07211 = 0.09489 0.03954 -0.00200 -0.00788 O4 5 0.555475 0.522553 0.864347 11.00000 0.05213 0.04998 = 0.05400 0.01160 0.01054 -0.00100 C1 1 0.547155 0.717169 0.732053 11.00000 0.03323 0.03228 = 0.03420 0.00501 -0.00457 -0.00076 C5 1 0.851987 0.809983 0.691437 11.00000 0.03492 0.04128 = 0.07375 -0.00810 0.00993 -0.00239 AFIX 13 H5 2 0.812907 0.770539 0.675930 11.00000 -1.20000 AFIX 0 C6 1 0.909663 0.851356 0.652711 11.00000 0.06817 0.07210 = 0.12178 0.00568 0.04841 -0.00619 AFIX 33 H6A 2 0.854055 0.865171 0.628072 11.00000 -1.50000 H6B 2 0.969044 0.824204 0.637190 11.00000 -1.50000 H6C 2 0.943516 0.891681 0.667609 11.00000 -1.50000 AFIX 0 C7 1 0.929491 0.784899 0.731970 11.00000 0.04707 0.05838 = 0.13096 -0.00702 -0.02185 0.00971 AFIX 33 H7A 2 0.885500 0.758070 0.755336 11.00000 -1.50000 H7B 2 0.963405 0.823735 0.748779 11.00000 -1.50000 H7C 2 0.989501 0.756731 0.717910 11.00000 -1.50000 AFIX 0 C11 1 0.659120 0.617785 0.760522 11.00000 0.03744 0.02807 = 0.04586 0.00661 -0.00832 -0.00128 C12 1 0.651860 0.567938 0.797569 11.00000 0.03800 0.03189 = 0.04495 0.00683 -0.00273 -0.00229 C13 1 0.749150 0.532166 0.810557 11.00000 0.04919 0.03525 = 0.04677 0.00971 -0.00246 0.00359 AFIX 43 H13 2 0.744475 0.498324 0.835128 11.00000 -1.20000 AFIX 0 C14 1 0.851591 0.544771 0.788615 11.00000 0.03920 0.04171 = 0.06149 0.00821 -0.00208 0.00915 AFIX 43 H14 2 0.917132 0.520065 0.797956 11.00000 -1.20000 AFIX 0 C15 1 0.858016 0.594106 0.752606 11.00000 0.04172 0.03726 = 0.05809 0.00461 0.00866 0.00531 AFIX 43 H15 2 0.928750 0.603421 0.737532 11.00000 -1.20000 AFIX 0 C16 1 0.762576 0.630007 0.738317 11.00000 0.04530 0.03308 = 0.04040 0.00579 0.00056 0.00034 AFIX 43 H16 2 0.768158 0.663071 0.713235 11.00000 -1.20000 AFIX 0 C17 1 0.541347 0.553460 0.821461 11.00000 0.04686 0.03451 = 0.05746 0.01245 -0.00084 -0.00371 C18 1 0.451620 0.505152 0.890354 11.00000 0.05943 0.05413 = 0.05945 0.00328 0.01890 -0.00520 AFIX 23 H18A 2 0.401153 0.545061 0.892512 11.00000 -1.20000 H18B 2 0.410864 0.468465 0.873083 11.00000 -1.20000 AFIX 0 C19 1 0.485037 0.482929 0.939054 11.00000 0.08270 0.11718 = 0.05530 0.01365 0.01351 -0.01761 AFIX 33 H19A 2 0.417438 0.470581 0.957784 11.00000 -1.50000 H19B 2 0.525046 0.519737 0.955745 11.00000 -1.50000 H19C 2 0.535088 0.443531 0.936366 11.00000 -1.50000 AFIX 0 CU1A 3 0.328665 0.658304 0.677342 11.00000 0.03602 0.04683 = 0.04845 0.00760 -0.00879 -0.00285 P1A 6 0.298189 0.512727 0.631549 11.00000 0.04609 0.04400 = 0.07319 0.02038 0.01841 0.01155 S1A 7 0.425732 0.575326 0.640261 11.00000 0.03612 0.06814 = 0.08678 -0.01369 -0.00645 0.00553 S2A 7 0.143050 0.657721 0.667214 11.00000 0.03324 0.03423 = 0.04876 -0.00173 -0.00189 -0.00502 N1A 4 0.177079 0.538693 0.615143 11.00000 0.04019 0.03499 = 0.06129 -0.00477 0.00478 -0.00169 N2A 4 0.003053 0.591505 0.612558 11.00000 0.03777 0.03003 = 0.04347 -0.00277 -0.00015 -0.00356 AFIX 43 H2A1 2 -0.034004 0.627492 0.622727 11.00000 -1.20000 AFIX 0 O1A 5 0.275832 0.458836 0.671641 11.00000 0.07894 0.05598 = 0.06320 0.00662 0.00394 0.00073 O2A 5 0.321838 0.461168 0.584515 11.00000 0.05981 0.06709 = 0.08250 0.00513 0.00448 0.00204 O3A 5 -0.180949 0.667225 0.621245 11.00000 0.04473 0.03800 = 0.04463 -0.00974 -0.00727 -0.00012 O4A 5 -0.322540 0.645054 0.569559 11.00000 0.03903 0.03993 = 0.04448 -0.00891 -0.00624 0.00170 C1A 1 0.111733 0.588093 0.627914 11.00000 0.03833 0.02969 = 0.04413 0.00329 0.00275 -0.00558 C2A 1 0.268119 0.473826 0.722241 11.00000 0.08272 0.10220 = 0.05101 -0.01128 -0.01630 0.03691 AFIX 13 H2A2 2 0.303087 0.519261 0.727926 11.00000 -1.20000 AFIX 0 C3A 1 0.336482 0.421914 0.749642 11.00000 0.16128 0.16832 = 0.07471 0.05611 0.00660 0.07601 AFIX 33 H3A1 2 0.414431 0.421905 0.737393 11.00000 -1.50000 H3A2 2 0.302978 0.377008 0.744849 11.00000 -1.50000 H3A3 2 0.336549 0.433029 0.784524 11.00000 -1.50000 AFIX 0 C4A 1 0.149164 0.475801 0.740695 11.00000 0.07907 0.12938 = 0.06501 -0.00611 0.01840 -0.00723 AFIX 33 H4A1 2 0.106656 0.510712 0.723059 11.00000 -1.50000 H4A2 2 0.149453 0.486354 0.775669 11.00000 -1.50000 H4A3 2 0.113344 0.431633 0.735466 11.00000 -1.50000 AFIX 0 C5A 1 0.404509 0.409119 0.587240 11.00000 0.08357 0.08424 = 0.07045 -0.00352 0.00177 0.02292 PART 1 AFIX 13 H5A 2 0.432802 0.406543 0.621620 31.00000 -1.20000 AFIX 13 PART 2 H5' 2 0.436341 0.398965 0.620289 -31.00000 -1.20000 AFIX 0 PART 1 C6A 1 0.498089 0.434287 0.555670 31.00000 0.08453 AFIX 33 H6A1 2 0.524118 0.478331 0.567743 31.00000 -1.50000 H6A2 2 0.470725 0.439133 0.522054 31.00000 -1.50000 H6A3 2 0.561017 0.401963 0.556433 31.00000 -1.50000 AFIX 0 C7A 1 0.351502 0.343191 0.574571 31.00000 0.05859 AFIX 33 H7A1 2 0.290497 0.333304 0.597744 31.00000 -1.50000 H7A2 2 0.408664 0.307294 0.576187 31.00000 -1.50000 H7A3 2 0.320383 0.345491 0.541424 31.00000 -1.50000 AFIX 0 PART 2 C6' 1 0.487069 0.419699 0.547146 -31.00000 0.09556 AFIX 33 H6'1 2 0.543221 0.453483 0.557185 -31.00000 -1.50000 H6'2 2 0.447204 0.435742 0.517956 -31.00000 -1.50000 H6'3 2 0.525322 0.376862 0.539810 -31.00000 -1.50000 AFIX 0 C7' 1 0.308923 0.358410 0.566974 -31.00000 0.14662 AFIX 33 H7'1 2 0.252774 0.350031 0.592609 -31.00000 -1.50000 H7'2 2 0.344129 0.315497 0.557380 -31.00000 -1.50000 H7'3 2 0.271602 0.378792 0.538578 -31.00000 -1.50000 AFIX 0 PART 0 C11A 1 -0.060726 0.547571 0.583226 11.00000 0.04330 0.02894 = 0.03277 0.00334 0.00166 -0.00914 C12A 1 -0.172457 0.567175 0.571566 11.00000 0.04501 0.02840 = 0.03485 0.00081 -0.00314 -0.00478 C13A 1 -0.238661 0.524466 0.542423 11.00000 0.05652 0.03948 = 0.05285 -0.00802 -0.01593 -0.00269 AFIX 43 H13A 2 -0.313728 0.537565 0.534277 11.00000 -1.20000 AFIX 0 C14A 1 -0.197108 0.463956 0.525379 11.00000 0.06517 0.03408 = 0.05848 -0.00893 -0.01588 -0.00217 AFIX 43 H14A 2 -0.243293 0.435320 0.505866 11.00000 -1.20000 AFIX 0 C15A 1 -0.087606 0.445063 0.536836 11.00000 0.06866 0.02942 = 0.04246 -0.00403 -0.00033 -0.00366 AFIX 43 H15A 2 -0.058858 0.403238 0.525017 11.00000 -1.20000 AFIX 0 C16A 1 -0.019427 0.485948 0.565145 11.00000 0.05003 0.03026 = 0.04325 0.00094 0.00295 -0.00216 AFIX 43 H16A 2 0.055844 0.472302 0.572426 11.00000 -1.20000 AFIX 0 C17A 1 -0.223627 0.630573 0.590455 11.00000 0.03961 0.03354 = 0.03438 0.00115 0.00073 -0.00646 C18A 1 -0.379812 0.705543 0.587877 11.00000 0.04350 0.04214 = 0.04611 -0.01080 0.00052 0.00450 AFIX 23 H18C 2 -0.327412 0.744667 0.587906 11.00000 -1.20000 H18D 2 -0.407038 0.698050 0.621637 11.00000 -1.20000 AFIX 0 C19A 1 -0.477584 0.718488 0.554235 11.00000 0.04685 0.06255 = 0.05942 -0.01409 -0.00740 0.01104 AFIX 33 H19D 2 -0.518737 0.758823 0.565152 11.00000 -1.50000 H19E 2 -0.528593 0.679356 0.554560 11.00000 -1.50000 H19F 2 -0.449356 0.725750 0.520995 11.00000 -1.50000 AFIX 0 CU1B 3 0.198934 0.732922 0.610353 11.00000 0.03687 0.02782 = 0.05115 0.00252 -0.00705 -0.00153 P1B 6 0.185690 0.794339 0.504360 11.00000 0.04570 0.04018 = 0.03696 -0.00482 -0.00320 -0.00987 S1B 7 0.210145 0.702806 0.531280 11.00000 0.06812 0.03391 = 0.05703 -0.01118 -0.01413 0.00340 S2B 7 0.239913 0.839561 0.626008 11.00000 0.03606 0.02839 = 0.03535 0.00193 -0.00504 -0.00208 N1B 4 0.251916 0.858683 0.526303 11.00000 0.04816 0.03734 = 0.03631 -0.00120 -0.00503 -0.00962 N2B 4 0.325578 0.940595 0.576905 11.00000 0.04470 0.03064 = 0.03547 0.00148 -0.00480 -0.00580 AFIX 43 H2B 2 0.351178 0.948003 0.606619 11.00000 -1.20000 AFIX 0 PART 1 O1B 5 0.208825 0.798215 0.447347 21.00000 0.03607 PART 2 O1" 5 0.246750 0.768932 0.453633 -21.00000 0.07074 PART 0 O2B 5 0.058455 0.816779 0.503788 11.00000 0.04932 0.03906 = 0.05803 0.00309 -0.01327 -0.00716 O3B 5 0.358942 1.031352 0.646585 11.00000 0.10965 0.04111 = 0.04438 -0.00355 -0.01459 -0.00770 O4B 5 0.338620 1.138977 0.625623 11.00000 0.08848 0.03397 = 0.05234 -0.00495 0.01224 -0.00318 C1B 1 0.275136 0.879350 0.569761 11.00000 0.03119 0.03048 = 0.03706 0.00220 -0.00501 0.00062 PART 1 C2B 1 0.321331 0.780456 0.426906 21.00000 0.05496 AFIX 13 H2B1 2 0.378766 0.777297 0.453658 21.00000 -1.20000 AFIX 0 C3B 1 0.350825 0.839194 0.392185 21.00000 0.08909 AFIX 33 H3B1 2 0.356995 0.881318 0.410913 21.00000 -1.50000 H3B2 2 0.291131 0.843881 0.367540 21.00000 -1.50000 H3B3 2 0.423118 0.829764 0.376006 21.00000 -1.50000 AFIX 0 C4B 1 0.313421 0.716038 0.400920 21.00000 0.10696 AFIX 33 H4B1 2 0.294538 0.679928 0.424072 21.00000 -1.50000 H4B2 2 0.386175 0.705942 0.385345 21.00000 -1.50000 H4B3 2 0.254243 0.719025 0.375908 21.00000 -1.50000 AFIX 0 PART 2 C2" 1 0.283523 0.811501 0.420701 -21.00000 0.06396 AFIX 13 H2" 2 0.244748 0.855786 0.426495 -21.00000 -1.20000 AFIX 0 C3" 1 0.402171 0.824238 0.419205 -21.00000 0.06588 AFIX 33 H3"1 2 0.427325 0.841413 0.450990 -21.00000 -1.50000 H3"2 2 0.418414 0.857950 0.393899 -21.00000 -1.50000 H3"3 2 0.442410 0.782115 0.411698 -21.00000 -1.50000 AFIX 0 C4" 1 0.243420 0.784013 0.367269 -21.00000 0.07250 AFIX 33 H4"1 2 0.162097 0.774205 0.367934 -21.00000 -1.50000 H4"2 2 0.285231 0.742638 0.359217 -21.00000 -1.50000 H4"3 2 0.258827 0.818676 0.342540 -21.00000 -1.50000 AFIX 0 PART 0 C5B 1 -0.027650 0.774165 0.480473 11.00000 0.05363 0.05694 = 0.07270 0.00437 -0.02080 -0.01724 PART 1 AFIX 13 H5B 2 0.002930 0.727502 0.475299 41.00000 -1.20000 AFIX 13 PART 2 H5" 2 0.011826 0.736312 0.463210 -41.00000 -1.20000 AFIX 0 PART 1 C6B 1 -0.065656 0.803024 0.433283 41.00000 0.06702 AFIX 33 H6B1 2 -0.002595 0.802630 0.410038 41.00000 -1.50000 H6B2 2 -0.091292 0.849700 0.438291 41.00000 -1.50000 H6B3 2 -0.128219 0.775830 0.420305 41.00000 -1.50000 AFIX 0 C7B 1 -0.124052 0.772481 0.519743 41.00000 0.06505 AFIX 33 H7B1 2 -0.095180 0.751908 0.549846 41.00000 -1.50000 H7B2 2 -0.187811 0.745718 0.507399 41.00000 -1.50000 H7B3 2 -0.149460 0.818763 0.526546 41.00000 -1.50000 AFIX 0 PART 2 C6" 1 -0.081530 0.820011 0.442013 -41.00000 0.05822 AFIX 33 H6"1 2 -0.023042 0.836101 0.419448 -41.00000 -1.50000 H6"2 2 -0.117243 0.858844 0.458101 -41.00000 -1.50000 H6"3 2 -0.138876 0.794505 0.423814 -41.00000 -1.50000 AFIX 0 C7" 1 -0.101483 0.745257 0.516603 -41.00000 0.07353 AFIX 33 H7"1 2 -0.057695 0.715682 0.538275 -41.00000 -1.50000 H7"2 2 -0.160766 0.718799 0.500374 -41.00000 -1.50000 H7"3 2 -0.136327 0.781581 0.535794 -41.00000 -1.50000 AFIX 0 PART 0 C11B 1 0.342480 0.993761 0.543328 11.00000 0.03854 0.03284 = 0.04014 0.00333 -0.00057 -0.00447 C12B 1 0.354093 1.060243 0.561925 11.00000 0.04657 0.03208 = 0.04232 0.00304 0.00353 -0.00419 C13B 1 0.370462 1.113289 0.528809 11.00000 0.07209 0.03047 = 0.05471 0.00318 0.00847 -0.00348 AFIX 43 H13B 2 0.378777 1.158127 0.540847 11.00000 -1.20000 AFIX 0 C14B 1 0.374816 1.102140 0.479246 11.00000 0.08333 0.04169 = 0.05268 0.01109 0.01370 -0.00534 AFIX 43 H14B 2 0.385746 1.138942 0.457412 11.00000 -1.20000 AFIX 0 C15B 1 0.363265 1.037502 0.461566 11.00000 0.07217 0.05144 = 0.03931 0.00412 0.00438 -0.00952 AFIX 43 H15B 2 0.366300 1.029734 0.427351 11.00000 -1.20000 AFIX 0 C16B 1 0.347225 0.983432 0.493053 11.00000 0.06171 0.03674 = 0.04103 0.00142 0.00206 -0.01096 AFIX 43 H16B 2 0.339404 0.938972 0.480250 11.00000 -1.20000 AFIX 0 C17B 1 0.350837 1.074135 0.615005 11.00000 0.05328 0.03422 = 0.04947 -0.00347 0.00037 -0.00736 C18B 1 0.334598 1.155421 0.678358 11.00000 0.09716 0.05422 = 0.05402 -0.01011 0.01206 -0.00497 AFIX 23 H18E 2 0.265474 1.135884 0.693162 11.00000 -1.20000 H18F 2 0.401302 1.135874 0.695127 11.00000 -1.20000 AFIX 0 C19B 1 0.334178 1.228760 0.684066 11.00000 0.10209 0.06224 = 0.07403 -0.01856 0.01496 -0.01181 AFIX 33 H19G 2 0.330909 1.240183 0.718868 11.00000 -1.50000 H19H 2 0.267978 1.247754 0.667378 11.00000 -1.50000 H19I 2 0.403365 1.247675 0.669793 11.00000 -1.50000 HKLF 4 ; _diffrn_ambient_temperature 173(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 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 43431 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.35 _reflns_number_total 12987 _reflns_number_gt 10919 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP (Sheldrick, 2008)' _computing_publication_material SHELXL97 _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^)+(0.0775P)^2^+7.7716P] 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 12987 _refine_ls_number_parameters 698 _refine_ls_number_restraints 53 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1406 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.057 _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 0.40113(4) 0.81776(2) 0.665430(15) 0.03650(11) Uani 1 1 d . . . P1 P 0.63791(7) 0.83643(4) 0.71384(3) 0.03141(18) Uani 1 1 d . . . S1 S 0.56858(8) 0.86696(4) 0.65186(3) 0.03763(19) Uani 1 1 d . . . S2 S 0.40305(7) 0.73931(5) 0.72401(3) 0.0400(2) Uani 1 1 d . . . N1 N 0.6342(2) 0.75686(14) 0.72744(10) 0.0325(6) Uani 1 1 d . . . N2 N 0.5601(3) 0.65206(15) 0.74649(12) 0.0430(7) Uani 1 1 d . . . H2 H 0.4976 0.6278 0.7472 0.052 Uiso 1 1 calc R . . O1 O 0.5897(2) 0.88039(13) 0.75669(9) 0.0409(6) Uani 1 1 d D . . C2 C 0.6316(4) 0.8710(2) 0.80689(13) 0.0503(9) Uani 1 1 d D . . H2A H 0.6900 0.8343 0.8072 0.060 Uiso 1 1 calc R . . C3 C 0.5323(5) 0.8496(3) 0.83773(17) 0.0730(14) Uani 1 1 d D . . H3A H 0.5021 0.8067 0.8254 0.110 Uiso 1 1 calc R . . H3B H 0.4732 0.8844 0.8361 0.110 Uiso 1 1 calc R . . H3C H 0.5569 0.8439 0.8717 0.110 Uiso 1 1 calc R . . C4 C 0.6852(5) 0.9364(3) 0.82255(17) 0.0705(14) Uani 1 1 d D . . H4A H 0.7495 0.9465 0.8012 0.106 Uiso 1 1 calc R . . H4B H 0.7116 0.9323 0.8564 0.106 Uiso 1 1 calc R . . H4C H 0.6294 0.9730 0.8203 0.106 Uiso 1 1 calc R . . O2 O 0.7676(2) 0.85398(12) 0.71501(9) 0.0390(5) Uani 1 1 d . . . O3 O 0.4493(2) 0.56773(18) 0.80547(14) 0.0684(10) Uani 1 1 d . . . O4 O 0.5555(2) 0.52255(15) 0.86435(11) 0.0520(7) Uani 1 1 d . . . C1 C 0.5472(3) 0.71717(17) 0.73206(12) 0.0332(7) Uani 1 1 d . . . C5 C 0.8520(3) 0.8100(2) 0.69144(17) 0.0499(9) Uani 1 1 d . . . H5 H 0.8129 0.7705 0.6759 0.060 Uiso 1 1 calc R . . C6 C 0.9096(5) 0.8514(3) 0.6527(3) 0.0872(19) Uani 1 1 d . . . H6A H 0.8540 0.8652 0.6281 0.131 Uiso 1 1 calc R . . H6B H 0.9690 0.8242 0.6372 0.131 Uiso 1 1 calc R . . H6C H 0.9435 0.8917 0.6676 0.131 Uiso 1 1 calc R . . C7 C 0.9295(4) 0.7849(3) 0.7320(3) 0.0787(17) Uani 1 1 d . . . H7A H 0.8855 0.7581 0.7553 0.118 Uiso 1 1 calc R . . H7B H 0.9634 0.8238 0.7488 0.118 Uiso 1 1 calc R . . H7C H 0.9895 0.7568 0.7179 0.118 Uiso 1 1 calc R . . C11 C 0.6591(3) 0.61777(17) 0.76052(13) 0.0371(7) Uani 1 1 d . . . C12 C 0.6518(3) 0.56794(17) 0.79756(13) 0.0383(7) Uani 1 1 d . . . C13 C 0.7491(3) 0.53217(18) 0.81056(14) 0.0437(8) Uani 1 1 d . . . H13 H 0.7445 0.4983 0.8351 0.052 Uiso 1 1 calc R . . C14 C 0.8516(3) 0.5448(2) 0.78860(15) 0.0474(9) Uani 1 1 d . . . H14 H 0.9171 0.5200 0.7979 0.057 Uiso 1 1 calc R . . C15 C 0.8580(3) 0.59412(19) 0.75261(15) 0.0456(8) Uani 1 1 d . . . H15 H 0.9288 0.6034 0.7375 0.055 Uiso 1 1 calc R . . C16 C 0.7626(3) 0.63001(18) 0.73832(13) 0.0396(7) Uani 1 1 d . . . H16 H 0.7681 0.6631 0.7132 0.048 Uiso 1 1 calc R . . C17 C 0.5414(3) 0.55347(19) 0.82146(15) 0.0463(9) Uani 1 1 d . . . C18 C 0.4516(4) 0.5051(2) 0.89036(17) 0.0577(11) Uani 1 1 d . . . H18A H 0.4012 0.5450 0.8925 0.069 Uiso 1 1 calc R . . H18B H 0.4109 0.4684 0.8731 0.069 Uiso 1 1 calc R . . C19 C 0.4850(5) 0.4829(4) 0.93906(19) 0.0850(17) Uani 1 1 d . . . H19A H 0.4174 0.4706 0.9578 0.128 Uiso 1 1 calc R . . H19B H 0.5250 0.5197 0.9558 0.128 Uiso 1 1 calc R . . H19C H 0.5351 0.4435 0.9364 0.128 Uiso 1 1 calc R . . Cu1A Cu 0.32867(4) 0.65830(2) 0.677343(17) 0.04374(13) Uani 1 1 d . . . P1A P 0.29821(9) 0.51273(6) 0.63156(5) 0.0544(3) Uani 1 1 d . . . S1A S 0.42574(9) 0.57534(7) 0.64026(5) 0.0637(3) Uani 1 1 d . . . S2A S 0.14305(7) 0.65772(4) 0.66721(3) 0.03871(19) Uani 1 1 d . . . N1A N 0.1771(3) 0.53870(16) 0.61515(13) 0.0454(7) Uani 1 1 d . . . N2A N 0.0031(2) 0.59150(14) 0.61256(11) 0.0370(6) Uani 1 1 d . . . H2A1 H -0.0340 0.6275 0.6227 0.044 Uiso 1 1 calc R . . O1A O 0.2759(3) 0.45884(17) 0.67165(12) 0.0661(8) Uani 1 1 d . . . O2A O 0.3219(3) 0.46115(18) 0.58454(14) 0.0700(9) Uani 1 1 d D A . O3A O -0.1810(2) 0.66723(12) 0.62125(9) 0.0424(6) Uani 1 1 d . . . O4A O -0.3225(2) 0.64506(13) 0.56956(9) 0.0411(6) Uani 1 1 d . . . C1A C 0.1117(3) 0.58809(17) 0.62792(13) 0.0374(7) Uani 1 1 d . . . C2A C 0.2682(5) 0.4739(3) 0.72217(18) 0.0793(17) Uani 1 1 d . . . H2A2 H 0.3032 0.5194 0.7278 0.095 Uiso 1 1 calc R . . C3A C 0.3365(8) 0.4219(5) 0.7496(3) 0.135(4) Uani 1 1 d . . . H3A1 H 0.4145 0.4219 0.7374 0.202 Uiso 1 1 calc R . . H3A2 H 0.3029 0.3770 0.7448 0.202 Uiso 1 1 calc R . . H3A3 H 0.3365 0.4330 0.7845 0.202 Uiso 1 1 calc R . . C4A C 0.1492(5) 0.4758(4) 0.7407(2) 0.0912(19) Uani 1 1 d . . . H4A1 H 0.1065 0.5107 0.7231 0.137 Uiso 1 1 calc R . . H4A2 H 0.1495 0.4863 0.7757 0.137 Uiso 1 1 calc R . . H4A3 H 0.1135 0.4316 0.7355 0.137 Uiso 1 1 calc R . . C5A C 0.4045(5) 0.4092(3) 0.5872(2) 0.0795(15) Uani 1 1 d D . . H5A H 0.4329 0.4066 0.6216 0.095 Uiso 0.50(3) 1 calc PR A 1 H5' H 0.4363 0.3990 0.6203 0.095 Uiso 0.50(3) 1 calc PR A 2 C6A C 0.4980(12) 0.4344(10) 0.5556(7) 0.084(5) Uiso 0.50(3) 1 d PD A 1 H6A1 H 0.5240 0.4784 0.5677 0.126 Uiso 0.50(3) 1 calc PR A 1 H6A2 H 0.4705 0.4392 0.5220 0.126 Uiso 0.50(3) 1 calc PR A 1 H6A3 H 0.5610 0.4021 0.5563 0.126 Uiso 0.50(3) 1 calc PR A 1 C7A C 0.3515(11) 0.3432(5) 0.5746(4) 0.059(4) Uiso 0.50(3) 1 d PD A 1 H7A1 H 0.2905 0.3333 0.5978 0.088 Uiso 0.50(3) 1 calc PR A 1 H7A2 H 0.4087 0.3073 0.5762 0.088 Uiso 0.50(3) 1 calc PR A 1 H7A3 H 0.3204 0.3454 0.5414 0.088 Uiso 0.50(3) 1 calc PR A 1 C6' C 0.4872(14) 0.4196(11) 0.5472(6) 0.095(6) Uiso 0.50(3) 1 d PD A 2 H6'1 H 0.5434 0.4534 0.5572 0.143 Uiso 0.50(3) 1 calc PR A 2 H6'2 H 0.4474 0.4356 0.5180 0.143 Uiso 0.50(3) 1 calc PR A 2 H6'3 H 0.5254 0.3767 0.5399 0.143 Uiso 0.50(3) 1 calc PR A 2 C7' C 0.309(2) 0.3583(13) 0.5670(9) 0.146(9) Uiso 0.50(3) 1 d PD A 2 H7'1 H 0.2529 0.3499 0.5926 0.219 Uiso 0.50(3) 1 calc PR A 2 H7'2 H 0.3444 0.3154 0.5575 0.219 Uiso 0.50(3) 1 calc PR A 2 H7'3 H 0.2717 0.3786 0.5386 0.219 Uiso 0.50(3) 1 calc PR A 2 C11A C -0.0607(3) 0.54757(16) 0.58322(12) 0.0350(7) Uani 1 1 d . . . C12A C -0.1725(3) 0.56717(16) 0.57156(12) 0.0361(7) Uani 1 1 d . . . C13A C -0.2387(4) 0.5245(2) 0.54244(15) 0.0496(9) Uani 1 1 d . . . H13A H -0.3138 0.5376 0.5343 0.060 Uiso 1 1 calc R . . C14A C -0.1971(4) 0.46395(19) 0.52539(16) 0.0526(10) Uani 1 1 d . . . H14A H -0.2433 0.4353 0.5059 0.063 Uiso 1 1 calc R . . C15A C -0.0876(4) 0.44506(18) 0.53685(14) 0.0468(9) Uani 1 1 d . . . H15A H -0.0589 0.4032 0.5250 0.056 Uiso 1 1 calc R . . C16A C -0.0194(3) 0.48595(17) 0.56515(13) 0.0411(8) Uani 1 1 d . . . H16A H 0.0558 0.4723 0.5724 0.049 Uiso 1 1 calc R . . C17A C -0.2236(3) 0.63058(17) 0.59045(12) 0.0358(7) Uani 1 1 d . . . C18A C -0.3798(3) 0.70554(19) 0.58787(14) 0.0439(8) Uani 1 1 d . . . H18C H -0.3274 0.7447 0.5879 0.053 Uiso 1 1 calc R . . H18D H -0.4070 0.6980 0.6216 0.053 Uiso 1 1 calc R . . C19A C -0.4776(4) 0.7185(2) 0.55423(17) 0.0562(10) Uani 1 1 d . . . H19D H -0.5187 0.7588 0.5651 0.084 Uiso 1 1 calc R . . H19E H -0.5286 0.6794 0.5546 0.084 Uiso 1 1 calc R . . H19F H -0.4494 0.7258 0.5210 0.084 Uiso 1 1 calc R . . Cu1B Cu 0.19893(4) 0.73292(2) 0.610353(17) 0.03859(12) Uani 1 1 d . . . P1B P 0.18570(8) 0.79434(5) 0.50436(3) 0.0409(2) Uani 1 1 d . . . S1B S 0.21015(10) 0.70281(5) 0.53128(4) 0.0530(3) Uani 1 1 d . B . S2B S 0.23991(7) 0.83956(4) 0.62601(3) 0.03323(17) Uani 1 1 d . B . N1B N 0.2519(3) 0.85867(15) 0.52630(11) 0.0406(7) Uani 1 1 d . B . N2B N 0.3256(3) 0.94059(14) 0.57691(10) 0.0369(6) Uani 1 1 d . B . H2B H 0.3512 0.9480 0.6066 0.044 Uiso 1 1 calc R . . O1B O 0.2088(3) 0.79824(18) 0.44735(12) 0.0360(9) Uiso 0.752(8) 1 d P B 1 O1" O 0.2465(14) 0.7691(9) 0.4536(6) 0.071(4) Uiso 0.248(8) 1 d P B 2 O2B O 0.0585(2) 0.81678(13) 0.50378(11) 0.0487(6) Uani 1 1 d D B . O3B O 0.3589(3) 1.03135(15) 0.64658(11) 0.0650(9) Uani 1 1 d . B . O4B O 0.3386(3) 1.13899(14) 0.62562(11) 0.0582(8) Uani 1 1 d . B . C1B C 0.2751(3) 0.87935(16) 0.56976(12) 0.0329(7) Uani 1 1 d . . . C2B C 0.3214(6) 0.7804(3) 0.4269(2) 0.0549(15) Uiso 0.752(8) 1 d P B 1 H2B1 H 0.3788 0.7773 0.4537 0.066 Uiso 0.752(8) 1 calc PR B 1 C3B C 0.3508(8) 0.8392(5) 0.3922(3) 0.089(3) Uiso 0.752(8) 1 d P B 1 H3B1 H 0.3570 0.8813 0.4109 0.134 Uiso 0.752(8) 1 calc PR B 1 H3B2 H 0.2911 0.8439 0.3675 0.134 Uiso 0.752(8) 1 calc PR B 1 H3B3 H 0.4231 0.8298 0.3760 0.134 Uiso 0.752(8) 1 calc PR B 1 C4B C 0.3135(9) 0.7161(5) 0.4009(4) 0.107(3) Uiso 0.752(8) 1 d P B 1 H4B1 H 0.2946 0.6799 0.4241 0.161 Uiso 0.752(8) 1 calc PR B 1 H4B2 H 0.3863 0.7060 0.3854 0.161 Uiso 0.752(8) 1 calc PR B 1 H4B3 H 0.2544 0.7190 0.3759 0.161 Uiso 0.752(8) 1 calc PR B 1 C2" C 0.2836(19) 0.8114(12) 0.4207(8) 0.065(5) Uiso 0.248(8) 1 d P B 2 H2" H 0.2449 0.8558 0.4265 0.077 Uiso 0.248(8) 1 calc PR B 2 C3" C 0.4022(18) 0.8242(11) 0.4193(8) 0.066(5) Uiso 0.248(8) 1 d P B 2 H3"1 H 0.4274 0.8413 0.4510 0.099 Uiso 0.248(8) 1 calc PR B 2 H3"2 H 0.4185 0.8579 0.3940 0.099 Uiso 0.248(8) 1 calc PR B 2 H3"3 H 0.4424 0.7820 0.4118 0.099 Uiso 0.248(8) 1 calc PR B 2 C4" C 0.243(2) 0.7840(12) 0.3673(8) 0.073(6) Uiso 0.248(8) 1 d P B 2 H4"1 H 0.1622 0.7742 0.3679 0.109 Uiso 0.248(8) 1 calc PR B 2 H4"2 H 0.2853 0.7426 0.3592 0.109 Uiso 0.248(8) 1 calc PR B 2 H4"3 H 0.2589 0.8187 0.3426 0.109 Uiso 0.248(8) 1 calc PR B 2 C5B C -0.0277(4) 0.7742(2) 0.48048(18) 0.0611(12) Uani 1 1 d D . . H5B H 0.0029 0.7275 0.4753 0.073 Uiso 0.51(3) 1 calc PR B 1 H5" H 0.0118 0.7363 0.4632 0.073 Uiso 0.49(3) 1 calc PR B 2 C6B C -0.0656(12) 0.8030(9) 0.4333(4) 0.067(4) Uiso 0.51(3) 1 d PD B 1 H6B1 H -0.0025 0.8026 0.4100 0.101 Uiso 0.51(3) 1 calc PR B 1 H6B2 H -0.0913 0.8497 0.4383 0.101 Uiso 0.51(3) 1 calc PR B 1 H6B3 H -0.1282 0.7758 0.4203 0.101 Uiso 0.51(3) 1 calc PR B 1 C7B C -0.1241(10) 0.7725(9) 0.5198(4) 0.065(4) Uiso 0.51(3) 1 d PD B 1 H7B1 H -0.0952 0.7520 0.5499 0.097 Uiso 0.51(3) 1 calc PR B 1 H7B2 H -0.1878 0.7458 0.5074 0.097 Uiso 0.51(3) 1 calc PR B 1 H7B3 H -0.1494 0.8188 0.5265 0.097 Uiso 0.51(3) 1 calc PR B 1 C6" C -0.0815(11) 0.8200(7) 0.4420(5) 0.058(3) Uiso 0.49(3) 1 d PD B 2 H6"1 H -0.0230 0.8360 0.4194 0.087 Uiso 0.49(3) 1 calc PR B 2 H6"2 H -0.1173 0.8588 0.4581 0.087 Uiso 0.49(3) 1 calc PR B 2 H6"3 H -0.1388 0.7944 0.4238 0.087 Uiso 0.49(3) 1 calc PR B 2 C7" C -0.1015(12) 0.7453(10) 0.5166(4) 0.074(4) Uiso 0.49(3) 1 d PD B 2 H7"1 H -0.0577 0.7157 0.5383 0.110 Uiso 0.49(3) 1 calc PR B 2 H7"2 H -0.1608 0.7188 0.5004 0.110 Uiso 0.49(3) 1 calc PR B 2 H7"3 H -0.1362 0.7816 0.5358 0.110 Uiso 0.49(3) 1 calc PR B 2 C11B C 0.3425(3) 0.99376(17) 0.54332(13) 0.0371(7) Uani 1 1 d . . . C12B C 0.3541(3) 1.06023(18) 0.56191(13) 0.0403(8) Uani 1 1 d . B . C13B C 0.3705(4) 1.11329(19) 0.52880(16) 0.0524(10) Uani 1 1 d . . . H13B H 0.3788 1.1581 0.5408 0.063 Uiso 1 1 calc R B . C14B C 0.3748(4) 1.1021(2) 0.47925(16) 0.0592(11) Uani 1 1 d . B . H14B H 0.3857 1.1389 0.4574 0.071 Uiso 1 1 calc R . . C15B C 0.3633(4) 1.0375(2) 0.46157(15) 0.0543(10) Uani 1 1 d . . . H15B H 0.3663 1.0297 0.4274 0.065 Uiso 1 1 calc R B . C16B C 0.3472(4) 0.98343(19) 0.49305(14) 0.0464(9) Uani 1 1 d . B . H16B H 0.3394 0.9390 0.4802 0.056 Uiso 1 1 calc R . . C17B C 0.3508(3) 1.07413(19) 0.61501(15) 0.0456(8) Uani 1 1 d . . . C18B C 0.3346(5) 1.1554(3) 0.67835(17) 0.0685(13) Uani 1 1 d . . . H18E H 0.2655 1.1359 0.6932 0.082 Uiso 1 1 calc R B . H18F H 0.4013 1.1359 0.6951 0.082 Uiso 1 1 calc R . . C19B C 0.3342(6) 1.2288(3) 0.6841(2) 0.0795(16) Uani 1 1 d . B . H19G H 0.3309 1.2402 0.7189 0.119 Uiso 1 1 calc R . . H19H H 0.2680 1.2478 0.6674 0.119 Uiso 1 1 calc R . . H19I H 0.4034 1.2477 0.6698 0.119 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 0.0387(2) 0.0342(2) 0.0365(2) -0.00053(16) -0.00690(17) 0.00432(16) P1 0.0325(4) 0.0276(4) 0.0341(4) -0.0028(3) -0.0005(3) 0.0001(3) S1 0.0450(5) 0.0342(4) 0.0337(4) 0.0029(3) -0.0017(3) -0.0021(3) S2 0.0298(4) 0.0408(4) 0.0493(5) 0.0100(4) -0.0053(3) -0.0011(3) N1 0.0317(13) 0.0305(13) 0.0353(14) 0.0017(11) -0.0031(11) 0.0001(11) N2 0.0327(15) 0.0352(15) 0.061(2) 0.0142(14) -0.0113(14) -0.0057(12) O1 0.0476(14) 0.0421(13) 0.0331(12) -0.0088(10) -0.0014(10) 0.0081(11) C2 0.064(3) 0.054(2) 0.0332(18) -0.0054(16) -0.0062(17) 0.0066(19) C3 0.092(4) 0.087(4) 0.040(2) -0.003(2) 0.010(2) -0.010(3) C4 0.092(4) 0.074(3) 0.046(2) -0.013(2) -0.012(2) -0.012(3) O2 0.0340(12) 0.0305(12) 0.0525(14) -0.0061(10) 0.0004(10) -0.0030(9) O3 0.0382(16) 0.072(2) 0.095(2) 0.0395(19) -0.0021(15) -0.0079(14) O4 0.0519(16) 0.0500(16) 0.0540(16) 0.0116(13) 0.0105(13) -0.0010(13) C1 0.0332(16) 0.0323(16) 0.0341(16) 0.0050(13) -0.0045(13) -0.0008(13) C5 0.0349(19) 0.041(2) 0.074(3) -0.0081(18) 0.0099(18) -0.0023(15) C6 0.068(3) 0.072(3) 0.122(5) 0.006(3) 0.048(3) -0.006(3) C7 0.047(3) 0.058(3) 0.131(5) -0.007(3) -0.022(3) 0.010(2) C11 0.0373(17) 0.0280(15) 0.0459(19) 0.0066(13) -0.0083(14) -0.0013(13) C12 0.0379(18) 0.0319(16) 0.0449(19) 0.0068(14) -0.0027(14) -0.0023(13) C13 0.049(2) 0.0352(18) 0.047(2) 0.0097(15) -0.0025(16) 0.0036(15) C14 0.0392(19) 0.042(2) 0.061(2) 0.0083(17) -0.0020(17) 0.0091(15) C15 0.042(2) 0.0372(19) 0.058(2) 0.0046(16) 0.0087(17) 0.0053(15) C16 0.0452(19) 0.0331(17) 0.0404(18) 0.0059(14) 0.0006(15) 0.0004(14) C17 0.047(2) 0.0344(18) 0.057(2) 0.0124(16) -0.0008(17) -0.0037(15) C18 0.059(3) 0.054(2) 0.059(3) 0.003(2) 0.019(2) -0.005(2) C19 0.083(4) 0.117(5) 0.055(3) 0.014(3) 0.013(3) -0.018(3) Cu1A 0.0360(2) 0.0468(3) 0.0484(3) 0.00760(19) -0.00879(19) -0.00286(18) P1A 0.0461(6) 0.0440(5) 0.0731(7) 0.0204(5) 0.0184(5) 0.0115(4) S1A 0.0361(5) 0.0681(7) 0.0868(8) -0.0137(6) -0.0064(5) 0.0055(5) S2A 0.0332(4) 0.0342(4) 0.0487(5) -0.0017(3) -0.0019(3) -0.0050(3) N1A 0.0400(16) 0.0350(16) 0.061(2) -0.0047(14) 0.0048(14) -0.0016(13) N2A 0.0376(15) 0.0300(14) 0.0435(16) -0.0028(11) -0.0001(12) -0.0036(11) O1A 0.079(2) 0.0562(18) 0.063(2) 0.0067(15) 0.0041(17) 0.0009(16) O2A 0.060(2) 0.067(2) 0.083(2) 0.0050(17) 0.0048(17) 0.0021(16) O3A 0.0447(14) 0.0380(13) 0.0445(14) -0.0098(11) -0.0072(11) -0.0002(11) O4A 0.0390(13) 0.0399(13) 0.0445(13) -0.0089(11) -0.0062(11) 0.0017(10) C1A 0.0383(18) 0.0297(16) 0.0441(18) 0.0034(13) 0.0027(14) -0.0056(13) C2A 0.083(4) 0.103(4) 0.052(3) -0.013(3) -0.017(2) 0.038(3) C3A 0.161(8) 0.168(8) 0.075(4) 0.056(5) 0.006(5) 0.076(7) C4A 0.079(4) 0.130(6) 0.065(3) -0.006(3) 0.019(3) -0.007(4) C5A 0.084(4) 0.084(4) 0.071(3) -0.003(3) 0.002(3) 0.023(3) C11A 0.0433(18) 0.0288(15) 0.0328(16) 0.0033(12) 0.0016(13) -0.0092(13) C12A 0.0450(19) 0.0284(15) 0.0348(16) 0.0008(13) -0.0031(14) -0.0048(14) C13A 0.057(2) 0.0394(19) 0.053(2) -0.0080(17) -0.0159(18) -0.0027(17) C14A 0.065(3) 0.0340(19) 0.059(2) -0.0090(17) -0.016(2) -0.0022(17) C15A 0.069(3) 0.0294(17) 0.0424(19) -0.0040(14) -0.0003(18) -0.0036(16) C16A 0.050(2) 0.0302(16) 0.0432(19) 0.0010(14) 0.0029(15) -0.0021(15) C17A 0.0395(18) 0.0335(16) 0.0344(16) 0.0012(13) 0.0007(14) -0.0064(14) C18A 0.043(2) 0.0422(19) 0.046(2) -0.0107(16) 0.0005(16) 0.0046(15) C19A 0.047(2) 0.062(3) 0.059(3) -0.014(2) -0.0073(19) 0.0110(19) Cu1B 0.0368(2) 0.0278(2) 0.0511(3) 0.00253(17) -0.00704(18) -0.00153(16) P1B 0.0457(5) 0.0402(5) 0.0369(5) -0.0048(4) -0.0032(4) -0.0099(4) S1B 0.0681(7) 0.0339(5) 0.0570(6) -0.0112(4) -0.0141(5) 0.0034(4) S2B 0.0360(4) 0.0284(4) 0.0353(4) 0.0019(3) -0.0050(3) -0.0021(3) N1B 0.0481(17) 0.0373(15) 0.0363(15) -0.0012(12) -0.0050(13) -0.0096(13) N2B 0.0447(16) 0.0306(14) 0.0354(14) 0.0015(11) -0.0049(12) -0.0058(12) O2B 0.0491(15) 0.0391(14) 0.0580(16) 0.0031(12) -0.0133(13) -0.0072(11) O3B 0.110(3) 0.0411(15) 0.0442(16) -0.0035(13) -0.0146(16) -0.0077(16) O4B 0.089(2) 0.0339(14) 0.0522(16) -0.0050(12) 0.0123(15) -0.0032(14) C1B 0.0312(16) 0.0304(15) 0.0370(16) 0.0022(13) -0.0050(13) 0.0006(12) C5B 0.054(2) 0.057(3) 0.073(3) 0.004(2) -0.021(2) -0.017(2) C11B 0.0385(18) 0.0328(17) 0.0400(18) 0.0033(13) -0.0006(14) -0.0045(13) C12B 0.046(2) 0.0321(17) 0.0422(19) 0.0030(14) 0.0035(15) -0.0042(14) C13B 0.072(3) 0.0304(18) 0.055(2) 0.0032(16) 0.008(2) -0.0035(17) C14B 0.083(3) 0.042(2) 0.053(2) 0.0111(18) 0.014(2) -0.005(2) C15B 0.072(3) 0.051(2) 0.039(2) 0.0041(17) 0.0044(19) -0.009(2) C16B 0.062(2) 0.0367(19) 0.0410(19) 0.0014(15) 0.0021(17) -0.0109(17) C17B 0.053(2) 0.0341(18) 0.049(2) -0.0035(16) 0.0003(17) -0.0073(16) C18B 0.097(4) 0.054(3) 0.054(3) -0.010(2) 0.012(3) -0.005(2) C19B 0.102(4) 0.062(3) 0.074(3) -0.019(3) 0.015(3) -0.012(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 S2B 2.2302(9) . ? Cu1 S2 2.2303(10) . ? Cu1 S1 2.2349(10) . ? P1 O1 1.567(2) . ? P1 O2 1.570(2) . ? P1 N1 1.616(3) . ? P1 S1 1.9780(12) . ? S2 C1 1.771(3) . ? S2 Cu1A 2.2278(11) . ? N1 C1 1.299(4) . ? N2 C1 1.354(4) . ? N2 C11 1.405(4) . ? N2 H2 0.8800 . ? O1 C2 1.472(4) . ? C2 C4 1.501(6) . ? C2 C3 1.505(6) . ? C2 H2A 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? O2 C5 1.472(4) . ? O3 C17 1.206(5) . ? O4 C17 1.334(5) . ? O4 C18 1.460(5) . ? C5 C6 1.502(7) . ? C5 C7 1.521(7) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C11 C16 1.386(5) . ? C11 C12 1.416(5) . ? C12 C13 1.395(5) . ? C12 C17 1.488(5) . ? C13 C14 1.374(6) . ? C13 H13 0.9500 . ? C14 C15 1.388(5) . ? C14 H14 0.9500 . ? C15 C16 1.388(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C18 C19 1.458(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? Cu1A S2A 2.2096(10) . ? Cu1A S1A 2.2433(13) . ? Cu1A Cu1B 2.8073(6) . ? P1A O1A 1.552(3) . ? P1A N1A 1.585(3) . ? P1A O2A 1.665(4) . ? P1A S1A 1.9631(17) . ? S2A C1A 1.785(4) . ? S2A Cu1B 2.2510(10) . ? N1A C1A 1.292(5) . ? N2A C1A 1.352(5) . ? N2A C11A 1.402(4) . ? N2A H2A1 0.8800 . ? O1A C2A 1.418(6) . ? O2A C5A 1.419(6) . ? O3A C17A 1.220(4) . ? O4A C17A 1.332(4) . ? O4A C18A 1.462(4) . ? C2A C4A 1.496(8) . ? C2A C3A 1.507(8) . ? C2A H2A2 1.0000 . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3A H3A3 0.9800 . ? C4A H4A1 0.9800 . ? C4A H4A2 0.9800 . ? C4A H4A3 0.9800 . ? C5A C6' 1.483(11) . ? C5A C7A 1.487(9) . ? C5A C6A 1.489(11) . ? C5A C7' 1.608(14) . ? C5A H5A 1.0000 . ? C5A H5' 1.0000 . ? C6A H6A1 0.9800 . ? C6A H6A2 0.9800 . ? C6A H6A3 0.9800 . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? C6' H6'1 0.9800 . ? C6' H6'2 0.9800 . ? C6' H6'3 0.9800 . ? C7' H7'1 0.9800 . ? C7' H7'2 0.9800 . ? C7' H7'3 0.9800 . ? C11A C16A 1.401(5) . ? C11A C12A 1.412(5) . ? C12A C13A 1.399(5) . ? C12A C17A 1.484(5) . ? C13A C14A 1.374(6) . ? C13A H13A 0.9500 . ? C14A C15A 1.382(6) . ? C14A H14A 0.9500 . ? C15A C16A 1.379(5) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? C18A C19A 1.499(6) . ? C18A H18C 0.9900 . ? C18A H18D 0.9900 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? Cu1B S2B 2.2032(9) . ? Cu1B S1B 2.2492(12) . ? P1B O2B 1.567(3) . ? P1B O1B 1.587(3) . ? P1B N1B 1.608(3) . ? P1B O1" 1.643(16) . ? P1B S1B 1.9735(14) . ? S2B C1B 1.778(3) . ? N1B C1B 1.287(4) . ? N2B C1B 1.362(4) . ? N2B C11B 1.410(4) . ? N2B H2B 0.8800 . ? O1B C2B 1.485(8) . ? O1" C2" 1.30(3) . ? O2B C5B 1.466(5) . ? O3B C17B 1.213(5) . ? O4B C17B 1.321(5) . ? O4B C18B 1.481(5) . ? C2B C4B 1.460(12) . ? C2B C3B 1.541(11) . ? C2B H2B1 1.0000 . ? C3B H3B1 0.9800 . ? C3B H3B2 0.9800 . ? C3B H3B3 0.9800 . ? C4B H4B1 0.9800 . ? C4B H4B2 0.9800 . ? C4B H4B3 0.9800 . ? C2" C3" 1.42(3) . ? C2" C4" 1.63(3) . ? C2" H2" 1.0000 . ? C3" H3"1 0.9800 . ? C3" H3"2 0.9800 . ? C3" H3"3 0.9800 . ? C4" H4"1 0.9800 . ? C4" H4"2 0.9800 . ? C4" H4"3 0.9800 . ? C5B C7" 1.437(10) . ? C5B C6B 1.481(10) . ? C5B C6" 1.527(9) . ? C5B C7B 1.567(10) . ? C5B H5B 1.0000 . ? C5B H5" 1.0000 . ? C6B H6B1 0.9800 . ? C6B H6B2 0.9800 . ? C6B H6B3 0.9800 . ? C7B H7B1 0.9800 . ? C7B H7B2 0.9800 . ? C7B H7B3 0.9800 . ? C6" H6"1 0.9800 . ? C6" H6"2 0.9800 . ? C6" H6"3 0.9800 . ? C7" H7"1 0.9800 . ? C7" H7"2 0.9800 . ? C7" H7"3 0.9800 . ? C11B C16B 1.393(5) . ? C11B C12B 1.415(5) . ? C12B C13B 1.399(5) . ? C12B C17B 1.480(5) . ? C13B C14B 1.376(6) . ? C13B H13B 0.9500 . ? C14B C15B 1.372(6) . ? C14B H14B 0.9500 . ? C15B C16B 1.385(5) . ? C15B H15B 0.9500 . ? C16B H16B 0.9500 . ? C18B C19B 1.457(7) . ? C18B H18E 0.9900 . ? C18B H18F 0.9900 . ? C19B H19G 0.9800 . ? C19B H19H 0.9800 . ? C19B H19I 0.9800 . ? 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 S2B Cu1 S2 119.38(4) . . ? S2B Cu1 S1 126.22(4) . . ? S2 Cu1 S1 114.40(4) . . ? O1 P1 O2 102.52(14) . . ? O1 P1 N1 110.89(15) . . ? O2 P1 N1 103.67(14) . . ? O1 P1 S1 108.86(10) . . ? O2 P1 S1 110.70(11) . . ? N1 P1 S1 118.90(11) . . ? P1 S1 Cu1 95.20(4) . . ? C1 S2 Cu1A 105.82(12) . . ? C1 S2 Cu1 105.69(11) . . ? Cu1A S2 Cu1 94.74(4) . . ? C1 N1 P1 129.1(2) . . ? C1 N2 C11 129.1(3) . . ? C1 N2 H2 115.4 . . ? C11 N2 H2 115.4 . . ? C2 O1 P1 120.5(2) . . ? O1 C2 C4 107.4(3) . . ? O1 C2 C3 107.3(4) . . ? C4 C2 C3 114.2(4) . . ? O1 C2 H2A 109.3 . . ? C4 C2 H2A 109.3 . . ? C3 C2 H2A 109.3 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C5 O2 P1 121.4(2) . . ? C17 O4 C18 115.6(3) . . ? N1 C1 N2 120.8(3) . . ? N1 C1 S2 126.8(3) . . ? N2 C1 S2 112.3(2) . . ? O2 C5 C6 107.2(4) . . ? O2 C5 C7 106.3(4) . . ? C6 C5 C7 114.8(4) . . ? O2 C5 H5 109.5 . . ? C6 C5 H5 109.5 . . ? C7 C5 H5 109.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C16 C11 N2 122.0(3) . . ? C16 C11 C12 119.3(3) . . ? N2 C11 C12 118.7(3) . . ? C13 C12 C11 119.0(3) . . ? C13 C12 C17 120.9(3) . . ? C11 C12 C17 120.2(3) . . ? C14 C13 C12 121.5(3) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 119.1(3) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C16 C15 C14 120.9(4) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C11 C16 C15 120.2(3) . . ? C11 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? O3 C17 O4 122.6(4) . . ? O3 C17 C12 125.9(4) . . ? O4 C17 C12 111.5(3) . . ? C19 C18 O4 106.9(4) . . ? C19 C18 H18A 110.3 . . ? O4 C18 H18A 110.3 . . ? C19 C18 H18B 110.3 . . ? O4 C18 H18B 110.3 . . ? H18A C18 H18B 108.6 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? S2A Cu1A S2 117.82(4) . . ? S2A Cu1A S1A 116.53(4) . . ? S2 Cu1A S1A 125.65(4) . . ? S2A Cu1A Cu1B 51.66(3) . . ? S2 Cu1A Cu1B 102.28(3) . . ? S1A Cu1A Cu1B 111.51(4) . . ? O1A P1A N1A 105.59(19) . . ? O1A P1A O2A 98.98(19) . . ? N1A P1A O2A 97.51(18) . . ? O1A P1A S1A 118.48(16) . . ? N1A P1A S1A 121.54(13) . . ? O2A P1A S1A 110.49(14) . . ? P1A S1A Cu1A 97.05(6) . . ? C1A S2A Cu1A 106.56(12) . . ? C1A S2A Cu1B 98.76(12) . . ? Cu1A S2A Cu1B 78.00(3) . . ? C1A N1A P1A 135.0(3) . . ? C1A N2A C11A 131.1(3) . . ? C1A N2A H2A1 114.5 . . ? C11A N2A H2A1 114.5 . . ? C2A O1A P1A 123.8(4) . . ? C5A O2A P1A 121.2(3) . . ? C17A O4A C18A 115.7(3) . . ? N1A C1A N2A 121.4(3) . . ? N1A C1A S2A 128.4(3) . . ? N2A C1A S2A 110.2(3) . . ? O1A C2A C4A 113.3(5) . . ? O1A C2A C3A 108.0(5) . . ? C4A C2A C3A 110.5(6) . . ? O1A C2A H2A2 108.3 . . ? C4A C2A H2A2 108.3 . . ? C3A C2A H2A2 108.3 . . ? C2A C3A H3A1 109.5 . . ? C2A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C2A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C2A C4A H4A1 109.5 . . ? C2A C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C2A C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? O2A C5A C6' 108.3(9) . . ? O2A C5A C7A 109.4(7) . . ? C6' C5A C7A 103.1(10) . . ? O2A C5A C6A 103.8(8) . . ? C7A C5A C6A 118.0(9) . . ? O2A C5A C7' 87.2(13) . . ? C6' C5A C7' 107.1(11) . . ? C6A C5A C7' 121.9(12) . . ? O2A C5A H5A 108.4 . . ? C6' C5A H5A 118.8 . . ? C7A C5A H5A 108.4 . . ? C6A C5A H5A 108.4 . . ? C7' C5A H5A 121.8 . . ? O2A C5A H5' 116.7 . . ? C6' C5A H5' 116.7 . . ? C7A C5A H5' 101.2 . . ? C6A C5A H5' 108.4 . . ? C7' C5A H5' 116.7 . . ? C5A C6A H6A1 109.5 . . ? C5A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C5A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C5A C7A H7A1 109.5 . . ? C5A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C5A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C5A C6' H6'1 109.5 . . ? C5A C6' H6'2 109.5 . . ? H6'1 C6' H6'2 109.5 . . ? C5A C6' H6'3 109.5 . . ? H6'1 C6' H6'3 109.5 . . ? H6'2 C6' H6'3 109.5 . . ? C5A C7' H7'1 109.5 . . ? C5A C7' H7'2 109.5 . . ? H7'1 C7' H7'2 109.5 . . ? C5A C7' H7'3 109.5 . . ? H7'1 C7' H7'3 109.5 . . ? H7'2 C7' H7'3 109.5 . . ? N2A C11A C16A 123.6(3) . . ? N2A C11A C12A 117.5(3) . . ? C16A C11A C12A 118.9(3) . . ? C13A C12A C11A 119.0(3) . . ? C13A C12A C17A 118.7(3) . . ? C11A C12A C17A 122.2(3) . . ? C14A C13A C12A 121.2(4) . . ? C14A C13A H13A 119.4 . . ? C12A C13A H13A 119.4 . . ? C13A C14A C15A 119.5(4) . . ? C13A C14A H14A 120.3 . . ? C15A C14A H14A 120.3 . . ? C16A C15A C14A 121.0(4) . . ? C16A C15A H15A 119.5 . . ? C14A C15A H15A 119.5 . . ? C15A C16A C11A 120.3(4) . . ? C15A C16A H16A 119.9 . . ? C11A C16A H16A 119.9 . . ? O3A C17A O4A 122.1(3) . . ? O3A C17A C12A 125.0(3) . . ? O4A C17A C12A 112.9(3) . . ? O4A C18A C19A 106.6(3) . . ? O4A C18A H18C 110.4 . . ? C19A C18A H18C 110.4 . . ? O4A C18A H18D 110.4 . . ? C19A C18A H18D 110.4 . . ? H18C C18A H18D 108.6 . . ? C18A C19A H19D 109.5 . . ? C18A C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C18A C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? S2B Cu1B S1B 115.28(4) . . ? S2B Cu1B S2A 124.11(4) . . ? S1B Cu1B S2A 120.58(4) . . ? S2B Cu1B Cu1A 104.77(3) . . ? S1B Cu1B Cu1A 117.24(3) . . ? S2A Cu1B Cu1A 50.34(3) . . ? O2B P1B O1B 98.14(18) . . ? O2B P1B N1B 104.27(16) . . ? O1B P1B N1B 104.20(17) . . ? O2B P1B O1" 119.8(6) . . ? N1B P1B O1" 110.1(6) . . ? O2B P1B S1B 113.77(12) . . ? O1B P1B S1B 112.76(15) . . ? N1B P1B S1B 120.88(13) . . ? O1" P1B S1B 88.5(6) . . ? P1B S1B Cu1B 96.23(5) . . ? C1B S2B Cu1B 107.78(11) . . ? C1B S2B Cu1 107.72(11) . . ? Cu1B S2B Cu1 95.56(3) . . ? C1B N1B P1B 134.3(3) . . ? C1B N2B C11B 129.0(3) . . ? C1B N2B H2B 115.5 . . ? C11B N2B H2B 115.5 . . ? C2B O1B P1B 120.9(4) . . ? C2" O1" P1B 122.4(17) . . ? C5B O2B P1B 120.5(3) . . ? C17B O4B C18B 115.5(3) . . ? N1B C1B N2B 120.5(3) . . ? N1B C1B S2B 127.6(3) . . ? N2B C1B S2B 111.7(2) . . ? C4B C2B O1B 109.5(6) . . ? C4B C2B C3B 111.7(7) . . ? O1B C2B C3B 104.9(6) . . ? C4B C2B H2B1 110.2 . . ? O1B C2B H2B1 110.2 . . ? C3B C2B H2B1 110.2 . . ? C2B C3B H3B1 109.5 . . ? C2B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C2B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C2B C4B H4B1 109.5 . . ? C2B C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C2B C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? O1" C2" C3" 118(2) . . ? O1" C2" C4" 108.0(18) . . ? C3" C2" C4" 108.5(18) . . ? O1" C2" H2" 107.4 . . ? C3" C2" H2" 107.4 . . ? C4" C2" H2" 107.4 . . ? C2" C3" H3"1 109.5 . . ? C2" C3" H3"2 109.5 . . ? H3"1 C3" H3"2 109.5 . . ? C2" C3" H3"3 109.5 . . ? H3"1 C3" H3"3 109.5 . . ? H3"2 C3" H3"3 109.5 . . ? C2" C4" H4"1 109.5 . . ? C2" C4" H4"2 109.5 . . ? H4"1 C4" H4"2 109.5 . . ? C2" C4" H4"3 109.5 . . ? H4"1 C4" H4"3 109.5 . . ? H4"2 C4" H4"3 109.5 . . ? C7" C5B O2B 110.4(6) . . ? C7" C5B C6B 124.8(8) . . ? O2B C5B C6B 111.6(6) . . ? C7" C5B C6" 117.2(8) . . ? O2B C5B C6" 104.4(6) . . ? O2B C5B C7B 102.6(5) . . ? C6B C5B C7B 112.8(7) . . ? C6" C5B C7B 100.6(7) . . ? C7" C5B H5B 87.2 . . ? O2B C5B H5B 109.9 . . ? C6B C5B H5B 109.9 . . ? C6" C5B H5B 126.8 . . ? C7B C5B H5B 109.9 . . ? C7" C5B H5" 108.1 . . ? O2B C5B H5" 108.1 . . ? C6B C5B H5" 90.9 . . ? C6" C5B H5" 108.1 . . ? C7B C5B H5" 130.4 . . ? C5B C6B H6B1 109.5 . . ? C5B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? C5B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C5B C7B H7B1 109.5 . . ? C5B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C5B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C5B C6" H6"1 109.5 . . ? C5B C6" H6"2 109.5 . . ? H6"1 C6" H6"2 109.5 . . ? C5B C6" H6"3 109.5 . . ? H6"1 C6" H6"3 109.5 . . ? H6"2 C6" H6"3 109.5 . . ? C5B C7" H7"1 109.5 . . ? C5B C7" H7"2 109.5 . . ? H7"1 C7" H7"2 109.5 . . ? C5B C7" H7"3 109.5 . . ? H7"1 C7" H7"3 109.5 . . ? H7"2 C7" H7"3 109.5 . . ? C16B C11B N2B 122.8(3) . . ? C16B C11B C12B 119.2(3) . . ? N2B C11B C12B 118.1(3) . . ? C13B C12B C11B 118.4(3) . . ? C13B C12B C17B 120.1(3) . . ? C11B C12B C17B 121.5(3) . . ? C14B C13B C12B 121.6(4) . . ? C14B C13B H13B 119.2 . . ? C12B C13B H13B 119.2 . . ? C15B C14B C13B 119.5(4) . . ? C15B C14B H14B 120.2 . . ? C13B C14B H14B 120.2 . . ? C14B C15B C16B 120.8(4) . . ? C14B C15B H15B 119.6 . . ? C16B C15B H15B 119.6 . . ? C15B C16B C11B 120.5(4) . . ? C15B C16B H16B 119.7 . . ? C11B C16B H16B 119.7 . . ? O3B C17B O4B 121.8(4) . . ? O3B C17B C12B 124.7(3) . . ? O4B C17B C12B 113.5(3) . . ? C19B C18B O4B 108.8(4) . . ? C19B C18B H18E 109.9 . . ? O4B C18B H18E 109.9 . . ? C19B C18B H18F 109.9 . . ? O4B C18B H18F 109.9 . . ? H18E C18B H18F 108.3 . . ? C18B C19B H19G 109.5 . . ? C18B C19B H19H 109.5 . . ? H19G C19B H19H 109.5 . . ? C18B C19B H19I 109.5 . . ? H19G C19B H19I 109.5 . . ? H19H C19B H19I 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 P1 S1 Cu1 -75.59(12) . . . . ? O2 P1 S1 Cu1 172.45(10) . . . . ? N1 P1 S1 Cu1 52.65(13) . . . . ? S2B Cu1 S1 P1 164.30(4) . . . . ? S2 Cu1 S1 P1 -16.33(6) . . . . ? S2B Cu1 S2 C1 161.47(12) . . . . ? S1 Cu1 S2 C1 -17.94(13) . . . . ? S2B Cu1 S2 Cu1A 53.57(5) . . . . ? S1 Cu1 S2 Cu1A -125.85(4) . . . . ? O1 P1 N1 C1 69.7(3) . . . . ? O2 P1 N1 C1 179.1(3) . . . . ? S1 P1 N1 C1 -57.6(3) . . . . ? O2 P1 O1 C2 -59.4(3) . . . . ? N1 P1 O1 C2 50.7(3) . . . . ? S1 P1 O1 C2 -176.7(3) . . . . ? P1 O1 C2 C4 118.0(4) . . . . ? P1 O1 C2 C3 -118.8(4) . . . . ? O1 P1 O2 C5 161.2(3) . . . . ? N1 P1 O2 C5 45.8(3) . . . . ? S1 P1 O2 C5 -82.8(3) . . . . ? P1 N1 C1 N2 -176.2(3) . . . . ? P1 N1 C1 S2 0.6(5) . . . . ? C11 N2 C1 N1 3.3(6) . . . . ? C11 N2 C1 S2 -174.0(3) . . . . ? Cu1A S2 C1 N1 133.1(3) . . . . ? Cu1 S2 C1 N1 33.4(3) . . . . ? Cu1A S2 C1 N2 -49.9(3) . . . . ? Cu1 S2 C1 N2 -149.6(2) . . . . ? P1 O2 C5 C6 118.9(4) . . . . ? P1 O2 C5 C7 -117.9(3) . . . . ? C1 N2 C11 C16 -36.5(6) . . . . ? C1 N2 C11 C12 145.3(4) . . . . ? C16 C11 C12 C13 -0.3(5) . . . . ? N2 C11 C12 C13 178.0(3) . . . . ? C16 C11 C12 C17 -179.3(3) . . . . ? N2 C11 C12 C17 -1.0(5) . . . . ? C11 C12 C13 C14 0.7(6) . . . . ? C17 C12 C13 C14 179.7(4) . . . . ? C12 C13 C14 C15 -0.2(6) . . . . ? C13 C14 C15 C16 -0.7(6) . . . . ? N2 C11 C16 C15 -178.8(4) . . . . ? C12 C11 C16 C15 -0.5(6) . . . . ? C14 C15 C16 C11 1.1(6) . . . . ? C18 O4 C17 O3 1.7(6) . . . . ? C18 O4 C17 C12 -179.0(3) . . . . ? C13 C12 C17 O3 -159.9(4) . . . . ? C11 C12 C17 O3 19.0(6) . . . . ? C13 C12 C17 O4 20.8(5) . . . . ? C11 C12 C17 O4 -160.2(3) . . . . ? C17 O4 C18 C19 -170.5(4) . . . . ? C1 S2 Cu1A S2A 171.01(11) . . . . ? Cu1 S2 Cu1A S2A -81.20(5) . . . . ? C1 S2 Cu1A S1A -7.91(13) . . . . ? Cu1 S2 Cu1A S1A 99.87(6) . . . . ? C1 S2 Cu1A Cu1B -136.07(11) . . . . ? Cu1 S2 Cu1A Cu1B -28.29(4) . . . . ? O1A P1A S1A Cu1A -92.31(17) . . . . ? N1A P1A S1A Cu1A 41.46(18) . . . . ? O2A P1A S1A Cu1A 154.60(14) . . . . ? S2A Cu1A S1A P1A -19.99(8) . . . . ? S2 Cu1A S1A P1A 158.95(5) . . . . ? Cu1B Cu1A S1A P1A -76.72(7) . . . . ? S2 Cu1A S2A C1A 179.33(12) . . . . ? S1A Cu1A S2A C1A -1.64(13) . . . . ? Cu1B Cu1A S2A C1A 95.69(12) . . . . ? S2 Cu1A S2A Cu1B 83.64(4) . . . . ? S1A Cu1A S2A Cu1B -97.33(5) . . . . ? O1A P1A N1A C1A 92.9(4) . . . . ? O2A P1A N1A C1A -165.5(4) . . . . ? S1A P1A N1A C1A -45.9(5) . . . . ? N1A P1A O1A C2A -90.1(4) . . . . ? O2A P1A O1A C2A 169.5(4) . . . . ? S1A P1A O1A C2A 50.2(4) . . . . ? O1A P1A O2A C5A -54.0(4) . . . . ? N1A P1A O2A C5A -161.1(4) . . . . ? S1A P1A O2A C5A 71.1(4) . . . . ? P1A N1A C1A N2A -169.1(3) . . . . ? P1A N1A C1A S2A 9.0(6) . . . . ? C11A N2A C1A N1A 1.2(6) . . . . ? C11A N2A C1A S2A -177.2(3) . . . . ? Cu1A S2A C1A N1A 13.0(4) . . . . ? Cu1B S2A C1A N1A 93.0(3) . . . . ? Cu1A S2A C1A N2A -168.6(2) . . . . ? Cu1B S2A C1A N2A -88.6(2) . . . . ? P1A O1A C2A C4A 102.3(6) . . . . ? P1A O1A C2A C3A -134.9(6) . . . . ? P1A O2A C5A C6' -122.4(10) . . . . ? P1A O2A C5A C7A 125.9(5) . . . . ? P1A O2A C5A C6A -107.2(9) . . . . ? P1A O2A C5A C7' 130.6(9) . . . . ? C1A N2A C11A C16A 3.1(6) . . . . ? C1A N2A C11A C12A -176.9(3) . . . . ? N2A C11A C12A C13A -179.9(3) . . . . ? C16A C11A C12A C13A 0.2(5) . . . . ? N2A C11A C12A C17A -1.9(5) . . . . ? C16A C11A C12A C17A 178.1(3) . . . . ? C11A C12A C13A C14A 0.4(6) . . . . ? C17A C12A C13A C14A -177.6(4) . . . . ? C12A C13A C14A C15A -0.5(7) . . . . ? C13A C14A C15A C16A 0.0(6) . . . . ? C14A C15A C16A C11A 0.5(6) . . . . ? N2A C11A C16A C15A 179.4(3) . . . . ? C12A C11A C16A C15A -0.6(5) . . . . ? C18A O4A C17A O3A -3.4(5) . . . . ? C18A O4A C17A C12A 177.7(3) . . . . ? C13A C12A C17A O3A 169.5(4) . . . . ? C11A C12A C17A O3A -8.4(5) . . . . ? C13A C12A C17A O4A -11.6(5) . . . . ? C11A C12A C17A O4A 170.4(3) . . . . ? C17A O4A C18A C19A 170.8(3) . . . . ? C1A S2A Cu1B S2B 174.09(12) . . . . ? Cu1A S2A Cu1B S2B -80.72(4) . . . . ? C1A S2A Cu1B S1B -3.62(13) . . . . ? Cu1A S2A Cu1B S1B 101.58(5) . . . . ? C1A S2A Cu1B Cu1A -105.19(12) . . . . ? S2A Cu1A Cu1B S2B 122.32(4) . . . . ? S2 Cu1A Cu1B S2B 6.42(4) . . . . ? S1A Cu1A Cu1B S2B -130.20(5) . . . . ? S2A Cu1A Cu1B S1B -108.45(5) . . . . ? S2 Cu1A Cu1B S1B 135.65(5) . . . . ? S1A Cu1A Cu1B S1B -0.97(6) . . . . ? S2 Cu1A Cu1B S2A -115.90(4) . . . . ? S1A Cu1A Cu1B S2A 107.48(5) . . . . ? O2B P1B S1B Cu1B -79.49(13) . . . . ? O1B P1B S1B Cu1B 169.86(14) . . . . ? N1B P1B S1B Cu1B 45.76(16) . . . . ? O1" P1B S1B Cu1B 158.4(6) . . . . ? S2B Cu1B S1B P1B -24.59(7) . . . . ? S2A Cu1B S1B P1B 153.31(5) . . . . ? Cu1A Cu1B S1B P1B -148.66(4) . . . . ? S1B Cu1B S2B C1B -0.38(12) . . . . ? S2A Cu1B S2B C1B -178.19(11) . . . . ? Cu1A Cu1B S2B C1B 130.01(11) . . . . ? S1B Cu1B S2B Cu1 -111.01(4) . . . . ? S2A Cu1B S2B Cu1 71.18(5) . . . . ? Cu1A Cu1B S2B Cu1 19.38(4) . . . . ? S2 Cu1 S2B C1B -159.63(12) . . . . ? S1 Cu1 S2B C1B 19.71(13) . . . . ? S2 Cu1 S2B Cu1B -48.94(5) . . . . ? S1 Cu1 S2B Cu1B 130.40(4) . . . . ? O2B P1B N1B C1B 85.9(4) . . . . ? O1B P1B N1B C1B -171.6(4) . . . . ? O1" P1B N1B C1B -144.3(8) . . . . ? S1B P1B N1B C1B -43.6(4) . . . . ? O2B P1B O1B C2B -179.3(4) . . . . ? N1B P1B O1B C2B 73.7(4) . . . . ? O1" P1B O1B C2B -32.9(12) . . . . ? S1B P1B O1B C2B -59.2(4) . . . . ? O2B P1B O1" C2" 79.6(18) . . . . ? O1B P1B O1" C2" 40.4(16) . . . . ? N1B P1B O1" C2" -41.2(19) . . . . ? S1B P1B O1" C2" -163.7(18) . . . . ? O1B P1B O2B C5B 65.6(3) . . . . ? N1B P1B O2B C5B 172.6(3) . . . . ? O1" P1B O2B C5B 48.9(8) . . . . ? S1B P1B O2B C5B -53.7(3) . . . . ? P1B N1B C1B N2B -174.1(3) . . . . ? P1B N1B C1B S2B 0.8(6) . . . . ? C11B N2B C1B N1B 11.7(6) . . . . ? C11B N2B C1B S2B -164.0(3) . . . . ? Cu1B S2B C1B N1B 18.3(4) . . . . ? Cu1 S2B C1B N1B 120.4(3) . . . . ? Cu1B S2B C1B N2B -166.4(2) . . . . ? Cu1 S2B C1B N2B -64.3(3) . . . . ? P1B O1B C2B C4B 108.4(6) . . . . ? P1B O1B C2B C3B -131.7(5) . . . . ? P1B O1" C2" C3" 102(2) . . . . ? P1B O1" C2" C4" -135.1(15) . . . . ? P1B O2B C5B C7" 110.7(10) . . . . ? P1B O2B C5B C6B -106.0(9) . . . . ? P1B O2B C5B C6" -122.4(7) . . . . ? P1B O2B C5B C7B 133.0(7) . . . . ? C1B N2B C11B C16B -24.4(6) . . . . ? C1B N2B C11B C12B 155.1(4) . . . . ? C16B C11B C12B C13B -0.2(6) . . . . ? N2B C11B C12B C13B -179.8(4) . . . . ? C16B C11B C12B C17B -179.4(4) . . . . ? N2B C11B C12B C17B 1.1(5) . . . . ? C11B C12B C13B C14B 0.3(7) . . . . ? C17B C12B C13B C14B 179.5(4) . . . . ? C12B C13B C14B C15B -0.2(8) . . . . ? C13B C14B C15B C16B 0.1(8) . . . . ? C14B C15B C16B C11B 0.0(7) . . . . ? N2B C11B C16B C15B 179.6(4) . . . . ? C12B C11B C16B C15B 0.1(6) . . . . ? C18B O4B C17B O3B -0.5(6) . . . . ? C18B O4B C17B C12B 179.9(4) . . . . ? C13B C12B C17B O3B -165.2(4) . . . . ? C11B C12B C17B O3B 14.0(6) . . . . ? C13B C12B C17B O4B 14.5(6) . . . . ? C11B C12B C17B O4B -166.3(4) . . . . ? C17B O4B C18B C19B 173.5(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 N2 H2 O3 0.88 2.07 2.664(4) 124.1 . N2A H2A1 O3A 0.88 1.91 2.649(4) 141.2 . N2B H2B O3B 0.88 1.98 2.647(4) 131.7 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.154 _refine_diff_density_min -1.416 _refine_diff_density_rms 0.088