# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Babashkina, Maria' _publ_contact_author_email maria.babashkina@ksu.ru _publ_section_title ; Polynuclear and heteroligand mononuclear CuI complexes with N-thiophosphorylated thioureas and 1,10-phenanthroline or PPh3 ; _publ_author_name M.Babashkina # Attachment '- C0CE00337A_ccdc_684171_739994_cif.txt' data_safin6 #TrackingRef '- C0CE00337A_ccdc_684171_739994_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 684171' #TrackingRef '- [Cu4LI4].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H80 Cu4 N8 O8 P4 S8' _chemical_formula_sum 'C36 H80 Cu4 N8 O8 P4 S8' _chemical_formula_weight 1387.60 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 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 14.6549(9) _cell_length_b 14.8054(8) _cell_length_c 28.178(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.782(5) _cell_angle_gamma 90.00 _cell_volume 6082.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19730 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 26.1 _exptl_crystal_description plate _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 1.808 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6812 _exptl_absorpt_correction_T_max 0.8259 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _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 '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 21129 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.72 _reflns_number_total 10081 _reflns_number_gt 8535 _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, 1990) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _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^)+(0.0850P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00211(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.035(13) _refine_ls_number_reflns 10081 _refine_ls_number_parameters 622 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1348 _refine_ls_wR_factor_gt 0.1309 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.57744(5) 0.34958(6) 0.61916(4) 0.0436(2) Uani 1 1 d . . . P1 P 0.62617(15) 0.28506(14) 0.52148(8) 0.0493(5) Uani 1 1 d . . . S1 S 0.64121(11) 0.21442(12) 0.63390(7) 0.0430(4) Uani 1 1 d . . . S2 S 0.54091(13) 0.37823(13) 0.53996(8) 0.0483(4) Uani 1 1 d . . . N1 N 0.6136(5) 0.1824(4) 0.5377(3) 0.0497(15) Uani 1 1 d . . . N2 N 0.5950(4) 0.0616(4) 0.5852(3) 0.0470(15) Uani 1 1 d . . . O1 O 0.6118(5) 0.2841(4) 0.4640(2) 0.0666(16) Uani 1 1 d . . . O2 O 0.7312(4) 0.3072(4) 0.5365(2) 0.0544(14) Uani 1 1 d . . . C1 C 0.6116(5) 0.1515(5) 0.5809(3) 0.0471(18) Uani 1 1 d . . . C2 C 0.5875(5) 0.0170(5) 0.6312(3) 0.053(2) Uani 1 1 d . . . H2A H 0.6287 0.0465 0.6560 0.080 Uiso 1 1 calc R . . H2B H 0.6045 -0.0467 0.6289 0.080 Uiso 1 1 calc R . . H2C H 0.5242 0.0215 0.6393 0.080 Uiso 1 1 calc R . . C3 C 0.5790(6) 0.0068(5) 0.5416(3) 0.057(2) Uani 1 1 d . . . H3A H 0.5228 0.0272 0.5230 0.085 Uiso 1 1 calc R . . H3B H 0.5726 -0.0568 0.5503 0.085 Uiso 1 1 calc R . . H3C H 0.6310 0.0136 0.5226 0.085 Uiso 1 1 calc R . . C11 C 0.6494(11) 0.2148(8) 0.4367(4) 0.098(4) Uani 1 1 d . . . H11 H 0.6474 0.1547 0.4528 0.118 Uiso 1 1 calc R . . C12 C 0.7434(10) 0.2375(12) 0.4259(6) 0.121(6) Uani 1 1 d . . . H12A H 0.7838 0.2417 0.4557 0.181 Uiso 1 1 calc R . . H12B H 0.7426 0.2955 0.4092 0.181 Uiso 1 1 calc R . . H12C H 0.7659 0.1903 0.4057 0.181 Uiso 1 1 calc R . . C13 C 0.5872(12) 0.2166(15) 0.3897(6) 0.144(8) Uani 1 1 d . . . H13A H 0.5252 0.1974 0.3954 0.216 Uiso 1 1 calc R . . H13B H 0.6116 0.1754 0.3669 0.216 Uiso 1 1 calc R . . H13C H 0.5849 0.2780 0.3767 0.216 Uiso 1 1 calc R . . C21 C 0.7688(5) 0.3981(6) 0.5447(3) 0.0525(19) Uani 1 1 d . . . H21 H 0.7277 0.4329 0.5642 0.063 Uiso 1 1 calc R . . C22 C 0.8619(6) 0.3887(8) 0.5725(4) 0.072(3) Uani 1 1 d . . . H22A H 0.8556 0.3565 0.6024 0.108 Uiso 1 1 calc R . . H22B H 0.8877 0.4489 0.5797 0.108 Uiso 1 1 calc R . . H22C H 0.9028 0.3548 0.5536 0.108 Uiso 1 1 calc R . . C23 C 0.7740(8) 0.4468(7) 0.4974(4) 0.075(3) Uani 1 1 d . . . H23A H 0.7126 0.4502 0.4801 0.113 Uiso 1 1 calc R . . H23B H 0.8149 0.4136 0.4781 0.113 Uiso 1 1 calc R . . H23C H 0.7979 0.5080 0.5035 0.113 Uiso 1 1 calc R . . Cu1A Cu 0.36926(5) 0.25253(6) 0.63242(3) 0.0423(2) Uani 1 1 d . . . P1A P 0.27593(13) 0.26144(14) 0.52872(7) 0.0446(4) Uani 1 1 d . . . S1A S 0.36482(13) 0.17609(13) 0.56190(8) 0.0477(4) Uani 1 1 d . . . S2A S 0.31039(11) 0.39129(12) 0.62564(7) 0.0419(4) Uani 1 1 d . . . N1A N 0.3024(4) 0.3661(4) 0.5286(3) 0.0476(15) Uani 1 1 d . . . N2A N 0.3341(4) 0.5080(4) 0.5547(3) 0.0488(15) Uani 1 1 d . . . O1A O 0.1756(3) 0.2575(3) 0.5444(2) 0.0481(12) Uani 1 1 d . . . O2A O 0.2581(4) 0.2333(4) 0.4741(2) 0.0591(15) Uani 1 1 d . . . C1A C 0.3160(4) 0.4204(5) 0.5645(3) 0.0407(16) Uani 1 1 d . . . C2A C 0.3390(6) 0.5334(6) 0.5054(3) 0.061(2) Uani 1 1 d . . . H2A1 H 0.3783 0.4907 0.4904 0.091 Uiso 1 1 calc R . . H2A2 H 0.3646 0.5944 0.5040 0.091 Uiso 1 1 calc R . . H2A3 H 0.2773 0.5324 0.4884 0.091 Uiso 1 1 calc R . . C3A C 0.3456(6) 0.5795(5) 0.5919(4) 0.058(2) Uani 1 1 d . . . H3A1 H 0.3201 0.5584 0.6208 0.087 Uiso 1 1 calc R . . H3A2 H 0.3133 0.6342 0.5801 0.087 Uiso 1 1 calc R . . H3A3 H 0.4109 0.5929 0.5993 0.087 Uiso 1 1 calc R . . C11A C 0.1344(6) 0.1811(5) 0.5683(4) 0.056(2) Uani 1 1 d . . . H11A H 0.1837 0.1451 0.5868 0.067 Uiso 1 1 calc R . . C12A C 0.0840(9) 0.1234(7) 0.5322(5) 0.091(4) Uani 1 1 d . . . H12D H 0.1271 0.0966 0.5118 0.136 Uiso 1 1 calc R . . H12E H 0.0387 0.1599 0.5127 0.136 Uiso 1 1 calc R . . H12F H 0.0526 0.0753 0.5481 0.136 Uiso 1 1 calc R . . C13A C 0.0725(6) 0.2224(7) 0.6019(4) 0.068(3) Uani 1 1 d . . . H13D H 0.1087 0.2611 0.6249 0.102 Uiso 1 1 calc R . . H13E H 0.0435 0.1743 0.6190 0.102 Uiso 1 1 calc R . . H13F H 0.0251 0.2585 0.5837 0.102 Uiso 1 1 calc R . . C21A C 0.3329(7) 0.2393(6) 0.4436(3) 0.061(2) Uani 1 1 d . . . H21A H 0.3926 0.2460 0.4638 0.073 Uiso 1 1 calc R . . C22A C 0.3178(19) 0.3180(12) 0.4114(8) 0.182(11) Uani 1 1 d . . . H22D H 0.3174 0.3735 0.4303 0.273 Uiso 1 1 calc R . . H22E H 0.2588 0.3115 0.3919 0.273 Uiso 1 1 calc R . . H22F H 0.3673 0.3212 0.3904 0.273 Uiso 1 1 calc R . . C23A C 0.3326(18) 0.1531(11) 0.4159(8) 0.196(13) Uani 1 1 d . . . H23D H 0.3358 0.1017 0.4380 0.295 Uiso 1 1 calc R . . H23E H 0.3857 0.1518 0.3974 0.295 Uiso 1 1 calc R . . H23F H 0.2761 0.1491 0.3942 0.295 Uiso 1 1 calc R . . Cu1B Cu 0.54446(5) 0.21289(6) 0.69127(3) 0.0421(2) Uani 1 1 d . . . P1B P 0.53027(13) 0.16587(13) 0.79608(7) 0.0426(4) Uani 1 1 d . . . S1B S 0.61447(12) 0.24611(13) 0.76534(8) 0.0469(4) Uani 1 1 d . . . S2B S 0.40465(12) 0.15350(12) 0.69173(7) 0.0407(4) Uani 1 1 d . . . N1B N 0.4229(4) 0.1825(4) 0.7888(2) 0.0428(14) Uani 1 1 d . . . N2B N 0.2785(4) 0.1983(4) 0.7500(2) 0.0454(14) Uani 1 1 d . . . O1B O 0.5557(4) 0.1754(4) 0.8520(2) 0.0543(13) Uani 1 1 d . . . O2B O 0.5410(3) 0.0623(3) 0.7841(2) 0.0449(12) Uani 1 1 d . . . C1B C 0.3692(4) 0.1827(5) 0.7483(3) 0.0365(14) Uani 1 1 d . . . C2B C 0.2454(6) 0.2207(7) 0.7968(3) 0.059(2) Uani 1 1 d . . . H2B1 H 0.2545 0.1686 0.8182 0.088 Uiso 1 1 calc R . . H2B2 H 0.1800 0.2358 0.7920 0.088 Uiso 1 1 calc R . . H2B3 H 0.2798 0.2725 0.8109 0.088 Uiso 1 1 calc R . . C3B C 0.2112(5) 0.1995(6) 0.7090(3) 0.0494(18) Uani 1 1 d . . . H3B1 H 0.2055 0.2610 0.6962 0.074 Uiso 1 1 calc R . . H3B2 H 0.1518 0.1796 0.7185 0.074 Uiso 1 1 calc R . . H3B3 H 0.2305 0.1587 0.6845 0.074 Uiso 1 1 calc R . . C11B C 0.4957(8) 0.1484(8) 0.8871(3) 0.075(3) Uani 1 1 d . . . H11B H 0.4357 0.1792 0.8782 0.090 Uiso 1 1 calc R . . C12B C 0.4756(15) 0.0513(11) 0.8895(7) 0.151(8) Uani 1 1 d . . . H12G H 0.4553 0.0288 0.8575 0.226 Uiso 1 1 calc R . . H12H H 0.4270 0.0416 0.9105 0.226 Uiso 1 1 calc R . . H12I H 0.5310 0.0188 0.9022 0.226 Uiso 1 1 calc R . . C13B C 0.5324(11) 0.1866(11) 0.9329(5) 0.112(5) Uani 1 1 d . . . H13G H 0.5433 0.2514 0.9292 0.168 Uiso 1 1 calc R . . H13H H 0.5903 0.1566 0.9439 0.168 Uiso 1 1 calc R . . H13I H 0.4882 0.1774 0.9564 0.168 Uiso 1 1 calc R . . C21B C 0.6276(6) 0.0207(5) 0.7714(3) 0.0512(19) Uani 1 1 d . . . H21B H 0.6544 0.0602 0.7476 0.061 Uiso 1 1 calc R . . C22B C 0.6961(6) 0.0109(7) 0.8143(4) 0.065(2) Uani 1 1 d . . . H22G H 0.7100 0.0706 0.8283 0.097 Uiso 1 1 calc R . . H22H H 0.7524 -0.0163 0.8048 0.097 Uiso 1 1 calc R . . H22I H 0.6706 -0.0278 0.8379 0.097 Uiso 1 1 calc R . . C23B C 0.6003(7) -0.0671(6) 0.7481(4) 0.072(3) Uani 1 1 d . . . H23G H 0.5549 -0.0562 0.7207 0.108 Uiso 1 1 calc R . . H23H H 0.5736 -0.1064 0.7711 0.108 Uiso 1 1 calc R . . H23I H 0.6544 -0.0964 0.7372 0.108 Uiso 1 1 calc R . . Cu1C Cu 0.43837(5) 0.42182(6) 0.67305(3) 0.0431(2) Uani 1 1 d . . . P1C P 0.50212(13) 0.51267(13) 0.77019(7) 0.0419(4) Uani 1 1 d . . . S1C S 0.40401(13) 0.42460(13) 0.74976(7) 0.0472(4) Uani 1 1 d . . . S2C S 0.57604(11) 0.47695(12) 0.66249(7) 0.0408(4) Uani 1 1 d . . . N1C N 0.6042(4) 0.4890(4) 0.7597(2) 0.0459(14) Uani 1 1 d . . . N2C N 0.7289(4) 0.4539(4) 0.7214(3) 0.0493(16) Uani 1 1 d . . . O1C O 0.4843(3) 0.6114(3) 0.7504(2) 0.0454(12) Uani 1 1 d . . . O2C O 0.5059(4) 0.5297(4) 0.8256(2) 0.0548(14) Uani 1 1 d . . . C1C C 0.6389(5) 0.4712(4) 0.7199(3) 0.0428(17) Uani 1 1 d . . . C2C C 0.7837(5) 0.4540(6) 0.7686(3) 0.059(2) Uani 1 1 d . . . H2C1 H 0.7896 0.5161 0.7807 0.088 Uiso 1 1 calc R . . H2C2 H 0.8447 0.4292 0.7654 0.088 Uiso 1 1 calc R . . H2C3 H 0.7529 0.4169 0.7910 0.088 Uiso 1 1 calc R . . C3C C 0.7772(5) 0.4387(6) 0.6792(4) 0.057(2) Uani 1 1 d . . . H3C1 H 0.7690 0.3758 0.6688 0.086 Uiso 1 1 calc R . . H3C2 H 0.8427 0.4511 0.6869 0.086 Uiso 1 1 calc R . . H3C3 H 0.7524 0.4790 0.6534 0.086 Uiso 1 1 calc R . . C11C C 0.3951(6) 0.6565(6) 0.7480(5) 0.081(4) Uani 1 1 d . . . H11C H 0.3456 0.6102 0.7485 0.097 Uiso 1 1 calc R . . C12C C 0.3840(16) 0.7048(14) 0.7030(5) 0.190(13) Uani 1 1 d . . . H12J H 0.3839 0.6617 0.6766 0.285 Uiso 1 1 calc R . . H12K H 0.4347 0.7475 0.7016 0.285 Uiso 1 1 calc R . . H12L H 0.3257 0.7379 0.7003 0.285 Uiso 1 1 calc R . . C13C C 0.3930(15) 0.7162(13) 0.7886(6) 0.162(9) Uani 1 1 d . . . H13J H 0.3927 0.6801 0.8178 0.243 Uiso 1 1 calc R . . H13K H 0.3376 0.7535 0.7845 0.243 Uiso 1 1 calc R . . H13L H 0.4473 0.7552 0.7911 0.243 Uiso 1 1 calc R . . C21C C 0.5231(6) 0.4544(6) 0.8596(3) 0.061(2) Uani 1 1 d . . . H21C H 0.5317 0.3973 0.8416 0.073 Uiso 1 1 calc R . . C22C C 0.6069(13) 0.4754(18) 0.8893(8) 0.214(15) Uani 1 1 d . . . H22J H 0.6571 0.4835 0.8692 0.321 Uiso 1 1 calc R . . H22K H 0.6218 0.4258 0.9118 0.321 Uiso 1 1 calc R . . H22L H 0.5984 0.5312 0.9070 0.321 Uiso 1 1 calc R . . C23C C 0.4460(11) 0.4446(16) 0.8871(7) 0.167(10) Uani 1 1 d . . . H23J H 0.3916 0.4269 0.8661 0.250 Uiso 1 1 calc R . . H23K H 0.4343 0.5021 0.9026 0.250 Uiso 1 1 calc R . . H23L H 0.4596 0.3979 0.9115 0.250 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 0.0420(4) 0.0398(5) 0.0502(5) -0.0069(4) 0.0108(4) -0.0017(4) P1 0.0609(12) 0.0424(11) 0.0477(12) -0.0014(9) 0.0208(9) -0.0055(9) S1 0.0393(8) 0.0397(9) 0.0521(11) -0.0023(8) 0.0142(7) -0.0019(7) S2 0.0489(10) 0.0449(10) 0.0521(12) -0.0019(9) 0.0097(8) -0.0033(8) N1 0.064(4) 0.038(3) 0.052(4) -0.001(3) 0.025(3) -0.005(3) N2 0.050(3) 0.032(3) 0.062(4) -0.005(3) 0.023(3) -0.008(2) O1 0.096(5) 0.054(3) 0.052(4) -0.006(3) 0.019(3) 0.000(3) O2 0.056(3) 0.040(3) 0.073(4) -0.002(3) 0.032(3) -0.001(2) C1 0.037(3) 0.041(4) 0.067(6) -0.002(4) 0.024(3) -0.004(3) C2 0.057(4) 0.033(4) 0.074(6) 0.004(4) 0.026(4) -0.002(3) C3 0.065(5) 0.040(4) 0.067(6) -0.010(4) 0.018(4) -0.012(4) C11 0.170(13) 0.069(7) 0.067(8) 0.003(6) 0.067(8) 0.007(7) C12 0.114(10) 0.149(14) 0.110(12) 0.003(10) 0.064(9) 0.042(10) C13 0.145(14) 0.21(2) 0.078(10) -0.069(12) 0.025(9) -0.036(13) C21 0.050(4) 0.045(4) 0.064(5) 0.000(4) 0.010(4) -0.007(3) C22 0.046(4) 0.094(7) 0.077(7) 0.000(6) 0.012(4) -0.005(5) C23 0.087(6) 0.059(6) 0.081(7) 0.008(5) 0.020(5) -0.029(5) Cu1A 0.0417(4) 0.0414(5) 0.0438(5) 0.0033(4) 0.0035(4) -0.0015(4) P1A 0.0445(9) 0.0447(11) 0.0438(11) 0.0007(8) 0.0005(8) -0.0060(8) S1A 0.0478(9) 0.0432(10) 0.0511(12) -0.0028(8) 0.0000(8) 0.0015(8) S2A 0.0366(8) 0.0412(9) 0.0479(11) 0.0024(8) 0.0051(7) -0.0009(7) N1A 0.044(3) 0.043(4) 0.055(4) 0.003(3) 0.002(3) -0.004(3) N2A 0.049(3) 0.037(3) 0.059(4) 0.009(3) -0.001(3) -0.007(3) O1A 0.041(2) 0.043(3) 0.061(4) 0.005(2) 0.006(2) -0.007(2) O2A 0.063(3) 0.068(4) 0.044(3) -0.004(3) -0.009(3) -0.007(3) C1A 0.031(3) 0.041(4) 0.049(4) 0.001(3) -0.005(3) -0.007(3) C2A 0.071(5) 0.051(5) 0.061(6) 0.018(4) 0.006(4) -0.013(4) C3A 0.058(5) 0.024(3) 0.091(7) -0.001(4) 0.007(4) 0.000(3) C11A 0.049(4) 0.043(4) 0.075(6) 0.009(4) 0.005(4) -0.007(3) C12A 0.102(8) 0.060(6) 0.109(10) -0.011(6) 0.007(7) -0.033(6) C13A 0.060(5) 0.067(6) 0.079(7) 0.016(5) 0.018(5) -0.005(4) C21A 0.073(5) 0.065(5) 0.046(5) -0.002(4) 0.013(4) -0.011(4) C22A 0.32(3) 0.102(12) 0.150(17) 0.054(11) 0.147(19) 0.043(14) C23A 0.32(3) 0.095(11) 0.22(2) -0.078(13) 0.21(2) -0.092(14) Cu1B 0.0434(4) 0.0382(5) 0.0462(5) 0.0023(4) 0.0118(4) 0.0010(4) P1B 0.0479(10) 0.0369(10) 0.0427(11) 0.0020(8) 0.0030(8) 0.0035(7) S1B 0.0489(9) 0.0397(10) 0.0515(12) 0.0015(8) 0.0024(8) -0.0034(7) S2B 0.0449(9) 0.0356(9) 0.0425(10) 0.0016(7) 0.0081(7) 0.0020(7) N1B 0.045(3) 0.043(3) 0.040(4) 0.000(3) 0.002(3) 0.012(3) N2B 0.043(3) 0.051(4) 0.043(4) -0.002(3) 0.010(3) 0.007(3) O1B 0.060(3) 0.061(3) 0.041(3) 0.005(3) -0.001(2) 0.005(3) O2B 0.047(3) 0.032(3) 0.056(3) 0.003(2) 0.006(2) 0.008(2) C1B 0.042(3) 0.032(3) 0.036(4) 0.002(3) 0.009(3) 0.004(3) C2B 0.059(5) 0.068(5) 0.052(5) 0.003(4) 0.024(4) 0.016(4) C3B 0.042(4) 0.054(5) 0.052(5) 0.003(4) 0.004(3) -0.006(3) C11B 0.093(7) 0.091(7) 0.041(5) 0.009(5) 0.008(5) -0.023(6) C12B 0.23(2) 0.097(11) 0.151(17) -0.005(11) 0.118(16) -0.032(12) C13B 0.128(11) 0.130(12) 0.080(9) -0.018(8) 0.023(8) -0.033(9) C21B 0.059(4) 0.041(4) 0.056(5) 0.003(4) 0.021(4) 0.012(3) C22B 0.052(5) 0.065(6) 0.078(7) 0.020(5) 0.009(4) 0.018(4) C23B 0.090(7) 0.046(5) 0.081(7) -0.007(5) 0.015(5) 0.007(4) Cu1C 0.0407(4) 0.0415(5) 0.0467(5) -0.0040(4) 0.0030(3) 0.0002(4) P1C 0.0476(9) 0.0374(9) 0.0402(10) -0.0016(8) 0.0031(8) 0.0050(8) S1C 0.0513(10) 0.0427(10) 0.0493(11) -0.0006(8) 0.0126(8) -0.0023(8) S2C 0.0408(9) 0.0348(9) 0.0475(10) -0.0029(8) 0.0076(7) 0.0021(7) N1C 0.049(3) 0.042(3) 0.046(4) -0.007(3) 0.002(3) 0.013(3) N2C 0.038(3) 0.043(3) 0.067(5) 0.001(3) 0.007(3) 0.008(3) O1C 0.037(2) 0.034(3) 0.066(4) -0.001(2) 0.007(2) 0.0104(19) O2C 0.067(3) 0.052(3) 0.044(3) -0.005(3) 0.003(3) 0.009(3) C1C 0.044(4) 0.024(3) 0.058(5) -0.004(3) -0.002(3) 0.007(3) C2C 0.048(4) 0.057(5) 0.067(6) 0.006(4) -0.013(4) 0.006(4) C3C 0.044(4) 0.042(4) 0.086(7) -0.014(4) 0.010(4) -0.001(3) C11C 0.040(4) 0.043(5) 0.160(12) -0.001(6) 0.016(5) 0.015(4) C12C 0.28(3) 0.190(18) 0.078(10) -0.046(11) -0.077(14) 0.17(2) C13C 0.23(2) 0.160(15) 0.090(11) -0.028(10) 0.011(11) 0.153(16) C21C 0.071(5) 0.058(5) 0.053(5) 0.015(4) -0.001(4) 0.025(4) C22C 0.128(14) 0.33(3) 0.17(2) 0.17(2) -0.062(14) -0.075(18) C23C 0.109(11) 0.27(3) 0.129(15) 0.118(16) 0.065(10) 0.078(13) _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 S1 2.230(2) . ? Cu1 S2C 2.248(2) . ? Cu1 S2 2.282(2) . ? Cu1 Cu1C 2.8682(13) . ? Cu1 Cu1B 2.9420(13) . ? P1 O2 1.589(6) . ? P1 N1 1.603(7) . ? P1 O1 1.612(7) . ? P1 S2 1.966(3) . ? S1 C1 1.776(9) . ? S1 Cu1B 2.2553(19) . ? N1 C1 1.303(11) . ? N2 C1 1.360(10) . ? N2 C2 1.469(11) . ? N2 C3 1.469(11) . ? O1 C11 1.425(13) . ? O2 C21 1.463(10) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C11 C12 1.48(2) . ? C11 C13 1.53(2) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 C22 1.511(12) . ? C21 C23 1.524(14) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? Cu1A S2A 2.229(2) . ? Cu1A S2B 2.244(2) . ? Cu1A S1A 2.282(2) . ? Cu1A Cu1C 2.8956(13) . ? Cu1A Cu1B 2.9712(12) . ? P1A O1A 1.579(5) . ? P1A O2A 1.591(6) . ? P1A N1A 1.598(7) . ? P1A S1A 1.980(3) . ? S2A C1A 1.787(8) . ? S2A Cu1C 2.2365(19) . ? N1A C1A 1.291(10) . ? N2A C1A 1.357(9) . ? N2A C2A 1.449(11) . ? N2A C3A 1.486(11) . ? O1A C11A 1.477(10) . ? O2A C21A 1.462(11) . ? C2A H2A1 0.9800 . ? C2A H2A2 0.9800 . ? C2A H2A3 0.9800 . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3A H3A3 0.9800 . ? C11A C12A 1.469(14) . ? C11A C13A 1.505(14) . ? C11A H11A 1.0000 . ? C12A H12D 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 0.9800 . ? C13A H13D 0.9800 . ? C13A H13E 0.9800 . ? C13A H13F 0.9800 . ? C21A C22A 1.481(19) . ? C21A C23A 1.495(16) . ? C21A H21A 1.0000 . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? Cu1B S2B 2.231(2) . ? Cu1B S1B 2.285(2) . ? P1B O2B 1.582(5) . ? P1B N1B 1.586(6) . ? P1B O1B 1.590(6) . ? P1B S1B 1.975(3) . ? S2B C1B 1.780(7) . ? N1B C1B 1.318(9) . ? N2B C1B 1.353(9) . ? N2B C3B 1.441(10) . ? N2B C2B 1.487(11) . ? O1B C11B 1.443(12) . ? O2B C21B 1.486(9) . ? C2B H2B1 0.9800 . ? C2B H2B2 0.9800 . ? C2B H2B3 0.9800 . ? C3B H3B1 0.9800 . ? C3B H3B2 0.9800 . ? C3B H3B3 0.9800 . ? C11B C13B 1.461(17) . ? C11B C12B 1.471(18) . ? C11B H11B 1.0000 . ? C12B H12G 0.9800 . ? C12B H12H 0.9800 . ? C12B H12I 0.9800 . ? C13B H13G 0.9800 . ? C13B H13H 0.9800 . ? C13B H13I 0.9800 . ? C21B C23B 1.493(13) . ? C21B C22B 1.498(13) . ? C21B H21B 1.0000 . ? C22B H22G 0.9800 . ? C22B H22H 0.9800 . ? C22B H22I 0.9800 . ? C23B H23G 0.9800 . ? C23B H23H 0.9800 . ? C23B H23I 0.9800 . ? Cu1C S2C 2.2241(19) . ? Cu1C S1C 2.269(2) . ? P1C O2C 1.577(6) . ? P1C O1C 1.577(5) . ? P1C N1C 1.592(6) . ? P1C S1C 1.983(3) . ? S2C C1C 1.780(8) . ? N1C C1C 1.305(11) . ? N2C C1C 1.340(9) . ? N2C C3C 1.463(12) . ? N2C C2C 1.484(11) . ? O1C C11C 1.462(9) . ? O2C C21C 1.475(10) . ? C2C H2C1 0.9800 . ? C2C H2C2 0.9800 . ? C2C H2C3 0.9800 . ? C3C H3C1 0.9800 . ? C3C H3C2 0.9800 . ? C3C H3C3 0.9800 . ? C11C C13C 1.449(19) . ? C11C C12C 1.45(2) . ? C11C H11C 1.0000 . ? C12C H12J 0.9800 . ? C12C H12K 0.9800 . ? C12C H12L 0.9800 . ? C13C H13J 0.9800 . ? C13C H13K 0.9800 . ? C13C H13L 0.9800 . ? C21C C23C 1.442(16) . ? C21C C22C 1.448(19) . ? C21C H21C 1.0000 . ? C22C H22J 0.9800 . ? C22C H22K 0.9800 . ? C22C H22L 0.9800 . ? C23C H23J 0.9800 . ? C23C H23K 0.9800 . ? C23C H23L 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 S1 Cu1 S2C 132.72(8) . . ? S1 Cu1 S2 113.67(8) . . ? S2C Cu1 S2 111.17(8) . . ? S1 Cu1 Cu1C 122.88(6) . . ? S2C Cu1 Cu1C 49.74(5) . . ? S2 Cu1 Cu1C 109.84(6) . . ? S1 Cu1 Cu1B 49.39(5) . . ? S2C Cu1 Cu1B 101.01(6) . . ? S2 Cu1 Cu1B 139.88(6) . . ? Cu1C Cu1 Cu1B 73.50(3) . . ? O2 P1 N1 104.8(3) . . ? O2 P1 O1 107.1(3) . . ? N1 P1 O1 105.7(4) . . ? O2 P1 S2 114.2(2) . . ? N1 P1 S2 119.7(3) . . ? O1 P1 S2 104.5(3) . . ? C1 S1 Cu1 104.6(3) . . ? C1 S1 Cu1B 118.7(2) . . ? Cu1 S1 Cu1B 81.98(7) . . ? P1 S2 Cu1 92.06(11) . . ? C1 N1 P1 127.9(6) . . ? C1 N2 C2 123.2(7) . . ? C1 N2 C3 118.8(7) . . ? C2 N2 C3 117.9(6) . . ? C11 O1 P1 122.0(8) . . ? C21 O2 P1 124.8(5) . . ? N1 C1 N2 116.6(8) . . ? N1 C1 S1 125.0(6) . . ? N2 C1 S1 118.0(7) . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O1 C11 C12 111.5(12) . . ? O1 C11 C13 103.1(12) . . ? C12 C11 C13 107.7(12) . . ? O1 C11 H11 111.4 . . ? C12 C11 H11 111.4 . . ? C13 C11 H11 111.4 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O2 C21 C22 107.7(7) . . ? O2 C21 C23 110.4(7) . . ? C22 C21 C23 112.1(8) . . ? O2 C21 H21 108.9 . . ? C22 C21 H21 108.9 . . ? C23 C21 H21 108.9 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? S2A Cu1A S2B 136.42(8) . . ? S2A Cu1A S1A 113.93(8) . . ? S2B Cu1A S1A 107.97(8) . . ? S2A Cu1A Cu1C 49.69(5) . . ? S2B Cu1A Cu1C 103.04(6) . . ? S1A Cu1A Cu1C 138.74(7) . . ? S2A Cu1A Cu1B 122.35(6) . . ? S2B Cu1A Cu1B 48.21(5) . . ? S1A Cu1A Cu1B 109.59(6) . . ? Cu1C Cu1A Cu1B 72.67(3) . . ? O1A P1A O2A 101.2(3) . . ? O1A P1A N1A 105.6(3) . . ? O2A P1A N1A 105.5(4) . . ? O1A P1A S1A 115.5(2) . . ? O2A P1A S1A 109.0(3) . . ? N1A P1A S1A 118.1(3) . . ? P1A S1A Cu1A 93.11(10) . . ? C1A S2A Cu1A 104.5(2) . . ? C1A S2A Cu1C 114.2(2) . . ? Cu1A S2A Cu1C 80.85(6) . . ? C1A N1A P1A 128.3(6) . . ? C1A N2A C2A 118.1(7) . . ? C1A N2A C3A 123.3(7) . . ? C2A N2A C3A 118.6(7) . . ? C11A O1A P1A 126.2(5) . . ? C21A O2A P1A 119.6(5) . . ? N1A C1A N2A 117.1(7) . . ? N1A C1A S2A 125.9(6) . . ? N2A C1A S2A 117.0(6) . . ? N2A C2A H2A1 109.5 . . ? N2A C2A H2A2 109.5 . . ? H2A1 C2A H2A2 109.5 . . ? N2A C2A H2A3 109.5 . . ? H2A1 C2A H2A3 109.5 . . ? H2A2 C2A H2A3 109.5 . . ? N2A C3A H3A1 109.5 . . ? N2A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? N2A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C12A C11A O1A 109.2(9) . . ? C12A C11A C13A 112.3(8) . . ? O1A C11A C13A 106.0(7) . . ? C12A C11A H11A 109.8 . . ? O1A C11A H11A 109.8 . . ? C13A C11A H11A 109.8 . . ? C11A C12A H12D 109.5 . . ? C11A C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? C11A C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? C11A C13A H13D 109.5 . . ? C11A C13A H13E 109.5 . . ? H13D C13A H13E 109.5 . . ? C11A C13A H13F 109.5 . . ? H13D C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? O2A C21A C22A 109.5(11) . . ? O2A C21A C23A 107.0(8) . . ? C22A C21A C23A 111.1(15) . . ? O2A C21A H21A 109.7 . . ? C22A C21A H21A 109.7 . . ? C23A C21A H21A 109.7 . . ? C21A C22A H22D 109.5 . . ? C21A C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? C21A C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? C21A C23A H23D 109.5 . . ? C21A C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C21A C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? S2B Cu1B S1 130.71(8) . . ? S2B Cu1B S1B 114.07(8) . . ? S1 Cu1B S1B 113.32(8) . . ? S2B Cu1B Cu1 119.34(6) . . ? S1 Cu1B Cu1 48.63(5) . . ? S1B Cu1B Cu1 113.14(6) . . ? S2B Cu1B Cu1A 48.59(5) . . ? S1 Cu1B Cu1A 99.69(6) . . ? S1B Cu1B Cu1A 138.65(6) . . ? Cu1 Cu1B Cu1A 70.82(3) . . ? O2B P1B N1B 104.0(3) . . ? O2B P1B O1B 106.3(3) . . ? N1B P1B O1B 104.2(3) . . ? O2B P1B S1B 114.2(2) . . ? N1B P1B S1B 120.4(3) . . ? O1B P1B S1B 106.7(2) . . ? P1B S1B Cu1B 91.62(9) . . ? C1B S2B Cu1B 105.1(2) . . ? C1B S2B Cu1A 116.2(2) . . ? Cu1B S2B Cu1A 83.20(7) . . ? C1B N1B P1B 127.6(5) . . ? C1B N2B C3B 124.7(7) . . ? C1B N2B C2B 118.6(6) . . ? C3B N2B C2B 116.7(6) . . ? C11B O1B P1B 123.8(6) . . ? C21B O2B P1B 124.0(5) . . ? N1B C1B N2B 118.2(6) . . ? N1B C1B S2B 124.8(5) . . ? N2B C1B S2B 116.7(5) . . ? N2B C2B H2B1 109.5 . . ? N2B C2B H2B2 109.5 . . ? H2B1 C2B H2B2 109.5 . . ? N2B C2B H2B3 109.5 . . ? H2B1 C2B H2B3 109.5 . . ? H2B2 C2B H2B3 109.5 . . ? N2B C3B H3B1 109.5 . . ? N2B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? N2B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? O1B C11B C13B 107.6(9) . . ? O1B C11B C12B 116.2(11) . . ? C13B C11B C12B 113.3(13) . . ? O1B C11B H11B 106.4 . . ? C13B C11B H11B 106.4 . . ? C12B C11B H11B 106.4 . . ? C11B C12B H12G 109.5 . . ? C11B C12B H12H 109.5 . . ? H12G C12B H12H 109.5 . . ? C11B C12B H12I 109.5 . . ? H12G C12B H12I 109.5 . . ? H12H C12B H12I 109.5 . . ? C11B C13B H13G 109.5 . . ? C11B C13B H13H 109.5 . . ? H13G C13B H13H 109.5 . . ? C11B C13B H13I 109.5 . . ? H13G C13B H13I 109.5 . . ? H13H C13B H13I 109.5 . . ? O2B C21B C23B 105.6(7) . . ? O2B C21B C22B 111.4(7) . . ? C23B C21B C22B 113.5(8) . . ? O2B C21B H21B 108.7 . . ? C23B C21B H21B 108.7 . . ? C22B C21B H21B 108.7 . . ? C21B C22B H22G 109.5 . . ? C21B C22B H22H 109.5 . . ? H22G C22B H22H 109.5 . . ? C21B C22B H22I 109.5 . . ? H22G C22B H22I 109.5 . . ? H22H C22B H22I 109.5 . . ? C21B C23B H23G 109.5 . . ? C21B C23B H23H 109.5 . . ? H23G C23B H23H 109.5 . . ? C21B C23B H23I 109.5 . . ? H23G C23B H23I 109.5 . . ? H23H C23B H23I 109.5 . . ? S2C Cu1C S2A 135.37(8) . . ? S2C Cu1C S1C 114.35(8) . . ? S2A Cu1C S1C 108.63(8) . . ? S2C Cu1C Cu1 50.47(5) . . ? S2A Cu1C Cu1 101.90(6) . . ? S1C Cu1C Cu1 138.50(6) . . ? S2C Cu1C Cu1A 123.41(6) . . ? S2A Cu1C Cu1A 49.46(5) . . ? S1C Cu1C Cu1A 106.86(6) . . ? Cu1 Cu1C Cu1A 72.95(3) . . ? O2C P1C O1C 100.9(3) . . ? O2C P1C N1C 106.2(3) . . ? O1C P1C N1C 105.3(3) . . ? O2C P1C S1C 110.2(2) . . ? O1C P1C S1C 114.7(2) . . ? N1C P1C S1C 117.9(3) . . ? P1C S1C Cu1C 93.70(10) . . ? C1C S2C Cu1C 104.7(3) . . ? C1C S2C Cu1 114.9(2) . . ? Cu1C S2C Cu1 79.79(6) . . ? C1C N1C P1C 131.2(6) . . ? C1C N2C C3C 124.0(7) . . ? C1C N2C C2C 118.1(7) . . ? C3C N2C C2C 117.9(6) . . ? C11C O1C P1C 123.7(6) . . ? C21C O2C P1C 120.5(5) . . ? N1C C1C N2C 118.6(7) . . ? N1C C1C S2C 124.1(5) . . ? N2C C1C S2C 117.1(6) . . ? N2C C2C H2C1 109.5 . . ? N2C C2C H2C2 109.5 . . ? H2C1 C2C H2C2 109.5 . . ? N2C C2C H2C3 109.5 . . ? H2C1 C2C H2C3 109.5 . . ? H2C2 C2C H2C3 109.5 . . ? N2C C3C H3C1 109.5 . . ? N2C C3C H3C2 109.5 . . ? H3C1 C3C H3C2 109.5 . . ? N2C C3C H3C3 109.5 . . ? H3C1 C3C H3C3 109.5 . . ? H3C2 C3C H3C3 109.5 . . ? C13C C11C C12C 112.4(12) . . ? C13C C11C O1C 109.4(10) . . ? C12C C11C O1C 106.7(11) . . ? C13C C11C H11C 109.4 . . ? C12C C11C H11C 109.4 . . ? O1C C11C H11C 109.4 . . ? C11C C12C H12J 109.5 . . ? C11C C12C H12K 109.5 . . ? H12J C12C H12K 109.5 . . ? C11C C12C H12L 109.5 . . ? H12J C12C H12L 109.5 . . ? H12K C12C H12L 109.5 . . ? C11C C13C H13J 109.5 . . ? C11C C13C H13K 109.5 . . ? H13J C13C H13K 109.5 . . ? C11C C13C H13L 109.5 . . ? H13J C13C H13L 109.5 . . ? H13K C13C H13L 109.5 . . ? C23C C21C C22C 112.0(15) . . ? C23C C21C O2C 109.5(9) . . ? C22C C21C O2C 107.0(10) . . ? C23C C21C H21C 109.4 . . ? C22C C21C H21C 109.4 . . ? O2C C21C H21C 109.4 . . ? C21C C22C H22J 109.5 . . ? C21C C22C H22K 109.5 . . ? H22J C22C H22K 109.5 . . ? C21C C22C H22L 109.5 . . ? H22J C22C H22L 109.5 . . ? H22K C22C H22L 109.5 . . ? C21C C23C H23J 109.5 . . ? C21C C23C H23K 109.5 . . ? H23J C23C H23K 109.5 . . ? C21C C23C H23L 109.5 . . ? H23J C23C H23L 109.5 . . ? H23K C23C H23L 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 S2C Cu1 S1 C1 -179.1(2) . . . . ? S2 Cu1 S1 C1 -18.7(2) . . . . ? Cu1C Cu1 S1 C1 117.7(2) . . . . ? Cu1B Cu1 S1 C1 117.6(2) . . . . ? S2C Cu1 S1 Cu1B 63.29(10) . . . . ? S2 Cu1 S1 Cu1B -136.38(7) . . . . ? Cu1C Cu1 S1 Cu1B 0.06(9) . . . . ? O2 P1 S2 Cu1 -66.6(3) . . . . ? N1 P1 S2 Cu1 58.7(3) . . . . ? O1 P1 S2 Cu1 176.7(3) . . . . ? S1 Cu1 S2 P1 -19.96(11) . . . . ? S2C Cu1 S2 P1 144.66(9) . . . . ? Cu1C Cu1 S2 P1 -161.99(8) . . . . ? Cu1B Cu1 S2 P1 -74.31(12) . . . . ? O2 P1 N1 C1 73.1(7) . . . . ? O1 P1 N1 C1 -173.9(7) . . . . ? S2 P1 N1 C1 -56.5(8) . . . . ? O2 P1 O1 C11 69.7(9) . . . . ? N1 P1 O1 C11 -41.7(9) . . . . ? S2 P1 O1 C11 -168.8(8) . . . . ? N1 P1 O2 C21 -157.4(6) . . . . ? O1 P1 O2 C21 90.6(7) . . . . ? S2 P1 O2 C21 -24.6(7) . . . . ? P1 N1 C1 N2 176.5(5) . . . . ? P1 N1 C1 S1 -10.7(10) . . . . ? C2 N2 C1 N1 -177.8(7) . . . . ? C3 N2 C1 N1 -1.0(10) . . . . ? C2 N2 C1 S1 8.9(9) . . . . ? C3 N2 C1 S1 -174.3(5) . . . . ? Cu1 S1 C1 N1 42.3(7) . . . . ? Cu1B S1 C1 N1 131.0(6) . . . . ? Cu1 S1 C1 N2 -145.0(5) . . . . ? Cu1B S1 C1 N2 -56.3(6) . . . . ? P1 O1 C11 C12 -88.6(12) . . . . ? P1 O1 C11 C13 156.2(9) . . . . ? P1 O2 C21 C22 162.5(6) . . . . ? P1 O2 C21 C23 -74.9(9) . . . . ? O1A P1A S1A Cu1A -70.3(3) . . . . ? O2A P1A S1A Cu1A 176.6(3) . . . . ? N1A P1A S1A Cu1A 56.2(3) . . . . ? S2A Cu1A S1A P1A -15.12(11) . . . . ? S2B Cu1A S1A P1A 152.60(9) . . . . ? Cu1C Cu1A S1A P1A -70.55(12) . . . . ? Cu1B Cu1A S1A P1A -156.32(8) . . . . ? S2B Cu1A S2A C1A 175.3(2) . . . . ? S1A Cu1A S2A C1A -21.8(2) . . . . ? Cu1C Cu1A S2A C1A 112.8(2) . . . . ? Cu1B Cu1A S2A C1A 113.9(2) . . . . ? S2B Cu1A S2A Cu1C 62.47(11) . . . . ? S1A Cu1A S2A Cu1C -134.59(8) . . . . ? Cu1B Cu1A S2A Cu1C 1.08(8) . . . . ? O1A P1A N1A C1A 67.5(7) . . . . ? O2A P1A N1A C1A 174.2(6) . . . . ? S1A P1A N1A C1A -63.6(7) . . . . ? O2A P1A O1A C11A 96.6(7) . . . . ? N1A P1A O1A C11A -153.6(7) . . . . ? S1A P1A O1A C11A -21.0(7) . . . . ? O1A P1A O2A C21A 172.3(6) . . . . ? N1A P1A O2A C21A 62.4(7) . . . . ? S1A P1A O2A C21A -65.5(7) . . . . ? P1A N1A C1A N2A -177.2(5) . . . . ? P1A N1A C1A S2A 1.1(10) . . . . ? C2A N2A C1A N1A -1.5(10) . . . . ? C3A N2A C1A N1A 176.1(6) . . . . ? C2A N2A C1A S2A -180.0(6) . . . . ? C3A N2A C1A S2A -2.3(9) . . . . ? Cu1A S2A C1A N1A 37.1(6) . . . . ? Cu1C S2A C1A N1A 123.4(6) . . . . ? Cu1A S2A C1A N2A -144.6(5) . . . . ? Cu1C S2A C1A N2A -58.2(6) . . . . ? P1A O1A C11A C12A -93.8(9) . . . . ? P1A O1A C11A C13A 145.1(6) . . . . ? P1A O2A C21A C22A -105.7(14) . . . . ? P1A O2A C21A C23A 133.7(14) . . . . ? C1 S1 Cu1B S2B -6.3(3) . . . . ? Cu1 S1 Cu1B S2B 95.95(10) . . . . ? C1 S1 Cu1B S1B 156.7(3) . . . . ? Cu1 S1 Cu1B S1B -100.99(8) . . . . ? C1 S1 Cu1B Cu1 -102.3(3) . . . . ? C1 S1 Cu1B Cu1A -48.8(3) . . . . ? Cu1 S1 Cu1B Cu1A 53.54(6) . . . . ? S1 Cu1 Cu1B S2B -120.13(10) . . . . ? S2C Cu1 Cu1B S2B 101.83(8) . . . . ? S2 Cu1 Cu1B S2B -41.48(12) . . . . ? Cu1C Cu1 Cu1B S2B 59.92(7) . . . . ? S2C Cu1 Cu1B S1 -138.04(9) . . . . ? S2 Cu1 Cu1B S1 78.65(11) . . . . ? Cu1C Cu1 Cu1B S1 -179.95(8) . . . . ? S1 Cu1 Cu1B S1B 101.38(9) . . . . ? S2C Cu1 Cu1B S1B -36.67(8) . . . . ? S2 Cu1 Cu1B S1B -179.97(10) . . . . ? Cu1C Cu1 Cu1B S1B -78.57(7) . . . . ? S1 Cu1 Cu1B Cu1A -122.93(7) . . . . ? S2C Cu1 Cu1B Cu1A 99.03(5) . . . . ? S2 Cu1 Cu1B Cu1A -44.28(10) . . . . ? Cu1C Cu1 Cu1B Cu1A 57.12(3) . . . . ? S2A Cu1A Cu1B S2B 125.72(10) . . . . ? S1A Cu1A Cu1B S2B -96.96(9) . . . . ? Cu1C Cu1A Cu1B S2B 126.59(7) . . . . ? S2A Cu1A Cu1B S1 -97.25(9) . . . . ? S2B Cu1A Cu1B S1 137.02(9) . . . . ? S1A Cu1A Cu1B S1 40.06(8) . . . . ? Cu1C Cu1A Cu1B S1 -96.39(6) . . . . ? S2A Cu1A Cu1B S1B 46.03(12) . . . . ? S2B Cu1A Cu1B S1B -79.69(11) . . . . ? S1A Cu1A Cu1B S1B -176.65(10) . . . . ? Cu1C Cu1A Cu1B S1B 46.90(9) . . . . ? S2A Cu1A Cu1B Cu1 -57.53(7) . . . . ? S2B Cu1A Cu1B Cu1 176.74(7) . . . . ? S1A Cu1A Cu1B Cu1 79.78(7) . . . . ? Cu1C Cu1A Cu1B Cu1 -56.67(3) . . . . ? O2B P1B S1B Cu1B 66.0(2) . . . . ? N1B P1B S1B Cu1B -58.7(3) . . . . ? O1B P1B S1B Cu1B -176.9(2) . . . . ? S2B Cu1B S1B P1B 18.40(11) . . . . ? S1 Cu1B S1B P1B -147.60(9) . . . . ? Cu1 Cu1B S1B P1B 159.16(7) . . . . ? Cu1A Cu1B S1B P1B 72.32(12) . . . . ? S1 Cu1B S2B C1B -177.8(2) . . . . ? S1B Cu1B S2B C1B 19.2(2) . . . . ? Cu1 Cu1B S2B C1B -118.9(2) . . . . ? Cu1A Cu1B S2B C1B -115.4(2) . . . . ? S1 Cu1B S2B Cu1A -62.44(10) . . . . ? S1B Cu1B S2B Cu1A 134.61(7) . . . . ? Cu1 Cu1B S2B Cu1A -3.53(8) . . . . ? S2A Cu1A S2B C1B 7.7(3) . . . . ? S1A Cu1A S2B C1B -155.9(3) . . . . ? Cu1C Cu1A S2B C1B 51.6(3) . . . . ? Cu1B Cu1A S2B C1B 103.5(3) . . . . ? S2A Cu1A S2B Cu1B -95.85(10) . . . . ? S1A Cu1A S2B Cu1B 100.53(8) . . . . ? Cu1C Cu1A S2B Cu1B -51.89(6) . . . . ? O2B P1B N1B C1B -69.7(7) . . . . ? O1B P1B N1B C1B 179.2(6) . . . . ? S1B P1B N1B C1B 59.8(7) . . . . ? O2B P1B O1B C11B -75.7(8) . . . . ? N1B P1B O1B C11B 33.8(8) . . . . ? S1B P1B O1B C11B 162.2(7) . . . . ? N1B P1B O2B C21B 160.5(6) . . . . ? O1B P1B O2B C21B -89.9(6) . . . . ? S1B P1B O2B C21B 27.5(6) . . . . ? P1B N1B C1B N2B 179.8(6) . . . . ? P1B N1B C1B S2B 6.1(10) . . . . ? C3B N2B C1B N1B -179.2(7) . . . . ? C2B N2B C1B N1B 4.3(10) . . . . ? C3B N2B C1B S2B -5.0(10) . . . . ? C2B N2B C1B S2B 178.5(6) . . . . ? Cu1B S2B C1B N1B -39.5(7) . . . . ? Cu1A S2B C1B N1B -129.3(6) . . . . ? Cu1B S2B C1B N2B 146.7(5) . . . . ? Cu1A S2B C1B N2B 56.9(6) . . . . ? P1B O1B C11B C13B -166.8(9) . . . . ? P1B O1B C11B C12B 65.0(15) . . . . ? P1B O2B C21B C23B -162.2(6) . . . . ? P1B O2B C21B C22B 74.2(8) . . . . ? C1A S2A Cu1C S2C -2.3(3) . . . . ? Cu1A S2A Cu1C S2C 99.50(10) . . . . ? C1A S2A Cu1C S1C 161.6(3) . . . . ? Cu1A S2A Cu1C S1C -96.57(8) . . . . ? C1A S2A Cu1C Cu1 -46.9(3) . . . . ? Cu1A S2A Cu1C Cu1 54.93(6) . . . . ? C1A S2A Cu1C Cu1A -101.8(3) . . . . ? S1 Cu1 Cu1C S2C 120.74(10) . . . . ? S2 Cu1 Cu1C S2C -101.40(9) . . . . ? Cu1B Cu1 Cu1C S2C 120.79(7) . . . . ? S1 Cu1 Cu1C S2A -98.99(9) . . . . ? S2C Cu1 Cu1C S2A 140.27(9) . . . . ? S2 Cu1 Cu1C S2A 38.87(8) . . . . ? Cu1B Cu1 Cu1C S2A -98.95(6) . . . . ? S1 Cu1 Cu1C S1C 37.98(13) . . . . ? S2C Cu1 Cu1C S1C -82.76(11) . . . . ? S2 Cu1 Cu1C S1C 175.84(10) . . . . ? Cu1B Cu1 Cu1C S1C 38.03(10) . . . . ? S1 Cu1 Cu1C Cu1A -58.41(7) . . . . ? S2C Cu1 Cu1C Cu1A -179.15(7) . . . . ? S2 Cu1 Cu1C Cu1A 79.45(6) . . . . ? Cu1B Cu1 Cu1C Cu1A -58.36(3) . . . . ? S2A Cu1A Cu1C S2C -123.89(10) . . . . ? S2B Cu1A Cu1C S2C 94.98(9) . . . . ? S1A Cu1A Cu1C S2C -43.13(12) . . . . ? Cu1B Cu1A Cu1C S2C 57.06(7) . . . . ? S2B Cu1A Cu1C S2A -141.13(8) . . . . ? S1A Cu1A Cu1C S2A 80.77(11) . . . . ? Cu1B Cu1A Cu1C S2A -179.05(7) . . . . ? S2A Cu1A Cu1C S1C 100.38(9) . . . . ? S2B Cu1A Cu1C S1C -40.76(8) . . . . ? S1A Cu1A Cu1C S1C -178.86(10) . . . . ? Cu1B Cu1A Cu1C S1C -78.67(6) . . . . ? S2A Cu1A Cu1C Cu1 -123.10(7) . . . . ? S2B Cu1A Cu1C Cu1 95.77(6) . . . . ? S1A Cu1A Cu1C Cu1 -42.34(9) . . . . ? Cu1B Cu1A Cu1C Cu1 57.85(3) . . . . ? O2C P1C S1C Cu1C -176.5(2) . . . . ? O1C P1C S1C Cu1C 70.5(3) . . . . ? N1C P1C S1C Cu1C -54.4(3) . . . . ? S2C Cu1C S1C P1C 16.86(12) . . . . ? S2A Cu1C S1C P1C -150.82(9) . . . . ? Cu1 Cu1C S1C P1C 73.98(12) . . . . ? Cu1A Cu1C S1C P1C 157.10(8) . . . . ? S2A Cu1C S2C C1C -176.2(2) . . . . ? S1C Cu1C S2C C1C 20.5(2) . . . . ? Cu1 Cu1C S2C C1C -113.3(2) . . . . ? Cu1A Cu1C S2C C1C -112.3(2) . . . . ? S2A Cu1C S2C Cu1 -62.91(11) . . . . ? S1C Cu1C S2C Cu1 133.82(8) . . . . ? Cu1A Cu1C S2C Cu1 0.98(9) . . . . ? S1 Cu1 S2C C1C 0.8(3) . . . . ? S2 Cu1 S2C C1C -159.8(3) . . . . ? Cu1C Cu1 S2C C1C 101.6(3) . . . . ? Cu1B Cu1 S2C C1C 44.5(3) . . . . ? S1 Cu1 S2C Cu1C -100.74(9) . . . . ? S2 Cu1 S2C Cu1C 98.56(8) . . . . ? Cu1B Cu1 S2C Cu1C -57.05(6) . . . . ? O2C P1C N1C C1C -178.3(7) . . . . ? O1C P1C N1C C1C -71.8(8) . . . . ? S1C P1C N1C C1C 57.6(8) . . . . ? O2C P1C O1C C11C -76.5(8) . . . . ? N1C P1C O1C C11C 173.2(8) . . . . ? S1C P1C O1C C11C 41.8(8) . . . . ? O1C P1C O2C C21C -179.1(6) . . . . ? N1C P1C O2C C21C -69.4(7) . . . . ? S1C P1C O2C C21C 59.4(6) . . . . ? P1C N1C C1C N2C 179.5(6) . . . . ? P1C N1C C1C S2C 4.6(11) . . . . ? C3C N2C C1C N1C -176.0(7) . . . . ? C2C N2C C1C N1C 1.2(10) . . . . ? C3C N2C C1C S2C -0.7(10) . . . . ? C2C N2C C1C S2C 176.5(6) . . . . ? Cu1C S2C C1C N1C -39.1(7) . . . . ? Cu1 S2C C1C N1C -124.5(6) . . . . ? Cu1C S2C C1C N2C 145.9(5) . . . . ? Cu1 S2C C1C N2C 60.5(6) . . . . ? P1C O1C C11C C13C 98.6(12) . . . . ? P1C O1C C11C C12C -139.6(11) . . . . ? P1C O2C C21C C23C -119.3(13) . . . . ? P1C O2C C21C C22C 119.2(14) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.789 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.121 # Attachment '- [Cu8LII8].cif' data_sad #TrackingRef '- C0CE00337A_ccdc_684171_739994_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 717087' #TrackingRef '- [Cu8LII8].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H176 Cu8 N16 O16 P8 S16' _chemical_formula_weight 2887.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.742(2) _cell_length_b 18.063(2) _cell_length_c 23.031(3) _cell_angle_alpha 78.498(3) _cell_angle_beta 77.747(3) _cell_angle_gamma 79.888(3) _cell_volume 6604.7(14) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'transparent plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 1.668 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8509 _exptl_absorpt_correction_T_max 0.9363 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.870621 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65444 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 27.50 _reflns_number_total 30295 _reflns_number_gt 20801 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _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^)+(0.0533P)^2^+1.6305P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 30295 _refine_ls_number_parameters 1297 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0870 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1331 _refine_ls_wR_factor_gt 0.1190 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.72806(3) 0.27671(3) 0.37663(2) 0.02304(12) Uani 1 1 d . . . Cu2 Cu 0.88414(3) 0.22631(3) 0.32788(2) 0.02210(12) Uani 1 1 d . . . Cu3 Cu 0.85635(3) 0.09885(3) 0.28596(2) 0.02231(12) Uani 1 1 d . . . Cu4 Cu 0.71530(3) 0.17191(3) 0.14992(2) 0.02250(12) Uani 1 1 d . . . Cu5 Cu 0.87966(3) 0.15034(3) 0.16754(2) 0.02142(11) Uani 1 1 d . . . Cu6 Cu 0.68661(3) 0.32519(3) 0.13301(2) 0.02139(11) Uani 1 1 d . . . Cu7 Cu 0.58624(3) 0.34905(3) 0.24041(2) 0.02284(12) Uani 1 1 d . . . Cu8 Cu 0.69285(3) 0.40283(3) 0.29228(2) 0.02228(12) Uani 1 1 d . . . S1 S 0.77144(6) 0.14898(6) 0.36841(4) 0.0205(2) Uani 1 1 d . . . S2 S 0.73167(7) 0.29740(6) 0.47115(5) 0.0255(2) Uani 1 1 d . . . S3 S 0.82865(6) 0.35421(6) 0.30878(4) 0.0190(2) Uani 1 1 d . . . S4 S 0.96055(7) 0.20526(6) 0.40311(5) 0.0238(2) Uani 1 1 d . . . S5 S 0.76625(6) 0.08130(6) 0.22699(4) 0.0202(2) Uani 1 1 d . . . S6 S 0.95178(6) -0.00878(6) 0.29925(5) 0.0235(2) Uani 1 1 d . . . S7 S 0.59542(6) 0.23754(6) 0.19941(4) 0.0195(2) Uani 1 1 d . . . S8 S 0.69145(7) 0.13588(6) 0.06535(5) 0.0253(2) Uani 1 1 d . . . S9 S 0.94196(6) 0.19879(6) 0.23099(4) 0.0190(2) Uani 1 1 d . . . S10 S 0.97039(6) 0.05815(6) 0.12280(5) 0.0237(2) Uani 1 1 d . . . S11 S 0.81903(6) 0.25999(6) 0.11060(4) 0.0187(2) Uani 1 1 d . . . S12 S 0.62829(6) 0.36053(6) 0.04804(5) 0.0234(2) Uani 1 1 d . . . S13 S 0.60345(6) 0.30504(6) 0.33929(4) 0.0204(2) Uani 1 1 d . . . S14 S 0.47504(6) 0.44327(6) 0.23559(5) 0.0258(2) Uani 1 1 d . . . S15 S 0.70561(6) 0.41552(6) 0.18827(4) 0.0190(2) Uani 1 1 d . . . S16 S 0.62645(6) 0.51366(6) 0.32575(5) 0.0239(2) Uani 1 1 d . . . N1 N 0.7737(2) 0.1209(2) 0.49014(15) 0.0256(8) Uani 1 1 d . . . N2 N 0.8518(2) 0.0359(2) 0.43310(15) 0.0263(8) Uani 1 1 d . . . H2N H 0.8731 0.0250 0.3969 0.032 Uiso 1 1 calc R . . N3 N 0.9260(2) 0.3807(2) 0.38284(16) 0.0254(8) Uani 1 1 d . . . N4 N 0.8073(2) 0.4615(2) 0.37488(16) 0.0285(8) Uani 1 1 d . . . H4N H 0.7620 0.4738 0.3595 0.034 Uiso 1 1 calc R . . N5 N 0.8382(2) -0.06886(19) 0.23464(16) 0.0251(8) Uani 1 1 d . . . N6 N 0.7780(2) -0.01658(19) 0.15383(16) 0.0252(8) Uani 1 1 d . . . H6N H 0.7553 0.0247 0.1326 0.030 Uiso 1 1 calc R . . N7 N 0.5137(2) 0.1966(2) 0.12136(16) 0.0259(8) Uani 1 1 d . . . N8 N 0.4609(2) 0.30649(19) 0.15800(16) 0.0237(8) Uani 1 1 d . . . H8N H 0.4647 0.3393 0.1805 0.028 Uiso 1 1 calc R . . N9 N 1.0875(2) 0.1173(2) 0.18404(15) 0.0252(8) Uani 1 1 d . . . N10 N 1.0705(2) 0.1337(2) 0.28097(15) 0.0281(8) Uani 1 1 d . . . H10N H 1.0399 0.1534 0.3117 0.034 Uiso 1 1 calc R . . N11 N 0.8067(2) 0.2995(2) -0.00920(15) 0.0234(8) Uani 1 1 d . . . N12 N 0.8986(2) 0.1966(2) 0.01712(15) 0.0255(8) Uani 1 1 d . . . H12N H 0.9189 0.1637 0.0459 0.031 Uiso 1 1 calc R . . N13 N 0.4533(2) 0.3899(2) 0.37434(16) 0.0254(8) Uani 1 1 d . . . N14 N 0.5405(2) 0.3553(2) 0.44098(15) 0.0276(8) Uani 1 1 d . . . H14N H 0.5906 0.3370 0.4478 0.033 Uiso 1 1 calc R . . N15 N 0.6471(2) 0.56746(19) 0.18856(15) 0.0242(8) Uani 1 1 d . . . N16 N 0.6224(2) 0.51388(19) 0.11437(15) 0.0245(8) Uani 1 1 d . . . H16N H 0.6263 0.4727 0.0984 0.029 Uiso 1 1 calc R . . P1 P 0.71145(7) 0.19304(7) 0.50963(5) 0.0262(3) Uani 1 1 d . . . P2 P 0.99529(7) 0.30794(7) 0.38054(5) 0.0235(2) Uani 1 1 d . . . P3 P 0.87490(7) -0.07764(6) 0.29469(5) 0.0240(2) Uani 1 1 d . . . P4 P 0.57572(7) 0.12426(6) 0.10238(5) 0.0242(2) Uani 1 1 d . . . P5 P 1.06806(7) 0.10585(7) 0.12185(5) 0.0231(2) Uani 1 1 d . . . P6 P 0.73555(7) 0.37088(6) -0.00589(5) 0.0226(2) Uani 1 1 d . . . P7 P 0.41435(7) 0.40010(7) 0.31483(5) 0.0257(2) Uani 1 1 d . . . P8 P 0.67070(7) 0.57817(6) 0.24959(5) 0.0230(2) Uani 1 1 d . . . O1 O 0.61958(18) 0.18469(18) 0.50641(14) 0.0328(7) Uani 1 1 d . . . O2 O 0.7064(2) 0.18412(19) 0.57969(13) 0.0375(8) Uani 1 1 d D . . O3 O 1.05663(18) 0.31188(18) 0.31824(13) 0.0320(7) Uani 1 1 d . . . O4 O 1.05379(18) 0.31764(18) 0.42367(14) 0.0310(7) Uani 1 1 d . . . O5 O 0.80468(18) -0.07735(17) 0.35265(13) 0.0305(7) Uani 1 1 d . . . O6 O 0.91815(19) -0.16336(16) 0.30424(14) 0.0308(7) Uani 1 1 d . . . O7 O 0.57630(18) 0.05407(17) 0.15547(14) 0.0301(7) Uani 1 1 d . . . O8 O 0.53191(18) 0.09533(17) 0.05808(14) 0.0313(7) Uani 1 1 d . . . O9 O 1.06575(18) 0.18188(17) 0.07416(13) 0.0278(7) Uani 1 1 d . . . O10 O 1.14944(18) 0.05701(18) 0.09312(13) 0.0332(8) Uani 1 1 d . . . O11 O 0.76832(17) 0.44150(16) 0.00759(13) 0.0258(7) Uani 1 1 d . . . O12 O 0.72253(19) 0.39766(17) -0.07346(13) 0.0319(7) Uani 1 1 d . . . O13 O 0.32849(17) 0.45223(18) 0.32970(14) 0.0330(7) Uani 1 1 d . . . O14 O 0.38774(18) 0.32258(18) 0.30848(14) 0.0328(7) Uani 1 1 d . . . O15 O 0.64128(19) 0.66544(16) 0.25383(14) 0.0303(7) Uani 1 1 d . . . O16 O 0.76668(17) 0.57417(18) 0.24443(13) 0.0301(7) Uani 1 1 d . . . C1 C 0.8011(2) 0.1010(2) 0.43701(18) 0.0222(9) Uani 1 1 d . . . C2 C 0.8744(3) -0.0189(3) 0.4851(2) 0.0329(11) Uani 1 1 d . . . H2 H 0.8773 0.0095 0.5175 0.040 Uiso 1 1 calc R . . C3 C 0.9592(3) -0.0625(3) 0.4653(2) 0.0458(14) Uani 1 1 d . . . H3A H 0.9564 -0.0916 0.4343 0.069 Uiso 1 1 calc . . . H3B H 0.9768 -0.0976 0.5000 0.069 Uiso 1 1 calc . . . H3C H 0.9990 -0.0264 0.4488 0.069 Uiso 1 1 calc . . . C4 C 0.8089(4) -0.0720(3) 0.5090(2) 0.0515(15) Uani 1 1 d . . . H4A H 0.7559 -0.0421 0.5228 0.077 Uiso 1 1 calc . . . H4B H 0.8253 -0.1100 0.5426 0.077 Uiso 1 1 calc . . . H4C H 0.8035 -0.0978 0.4767 0.077 Uiso 1 1 calc . . . C5 C 0.5946(3) 0.1110(3) 0.5064(2) 0.0392(12) Uani 1 1 d . . . H5 H 0.6414 0.0793 0.4838 0.047 Uiso 1 1 calc R . . C6 C 0.5232(4) 0.1280(3) 0.4734(3) 0.0562(16) Uani 1 1 d . . . H6A H 0.4754 0.1547 0.4973 0.084 Uiso 1 1 calc . . . H6B H 0.5092 0.0801 0.4670 0.084 Uiso 1 1 calc . . . H6C H 0.5385 0.1603 0.4343 0.084 Uiso 1 1 calc . . . C7 C 0.5743(4) 0.0704(4) 0.5711(3) 0.0667(19) Uani 1 1 d . . . H7A H 0.6240 0.0595 0.5891 0.100 Uiso 1 1 calc . . . H7B H 0.5540 0.0225 0.5716 0.100 Uiso 1 1 calc . . . H7C H 0.5316 0.1032 0.5943 0.100 Uiso 1 1 calc . . . C8 C 0.7752(3) 0.1642(6) 0.6117(2) 0.198(7) Uani 1 1 d D . . H8 H 0.7939 0.1086 0.6113 0.238 Uiso 1 1 calc R . . C9 C 0.8515(5) 0.2026(6) 0.5880(3) 0.109(3) Uani 1 1 d D . . H9A H 0.8619 0.2117 0.5439 0.163 Uiso 1 1 calc . . . H9B H 0.8988 0.1698 0.6025 0.163 Uiso 1 1 calc . . . H9C H 0.8432 0.2515 0.6024 0.163 Uiso 1 1 calc . . . C10 C 0.7361(5) 0.1705(9) 0.6763(3) 0.186(7) Uani 1 1 d D . . H10A H 0.7629 0.1293 0.7034 0.279 Uiso 1 1 calc . . . H10B H 0.6772 0.1664 0.6827 0.279 Uiso 1 1 calc . . . H10C H 0.7429 0.2199 0.6847 0.279 Uiso 1 1 calc . . . C11 C 0.8577(2) 0.4001(2) 0.36070(18) 0.0216(9) Uani 1 1 d . . . C12 C 0.8211(3) 0.5108(3) 0.4144(2) 0.0377(12) Uani 1 1 d . . . H12 H 0.8754 0.4918 0.4274 0.045 Uiso 1 1 calc R . . C13 C 0.8219(7) 0.5892(5) 0.3813(3) 0.142(5) Uani 1 1 d . . . H13A H 0.8753 0.5934 0.3543 0.213 Uiso 1 1 calc . . . H13B H 0.8131 0.6246 0.4100 0.213 Uiso 1 1 calc . . . H13C H 0.7777 0.6020 0.3575 0.213 Uiso 1 1 calc . . . C14 C 0.7545(6) 0.5092(5) 0.4678(3) 0.109(3) Uani 1 1 d . . . H14A H 0.7016 0.5303 0.4552 0.164 Uiso 1 1 calc . . . H14B H 0.7653 0.5399 0.4952 0.164 Uiso 1 1 calc . . . H14C H 0.7524 0.4565 0.4885 0.164 Uiso 1 1 calc . . . C15 C 1.0252(4) 0.3186(5) 0.4866(3) 0.079(2) Uani 1 1 d . . . H15 H 0.9727 0.2957 0.5004 0.095 Uiso 1 1 calc R . . C16 C 1.0114(11) 0.3968(8) 0.4968(6) 0.332(14) Uani 1 1 d . . . H16A H 1.0639 0.4121 0.4989 0.498 Uiso 1 1 calc . . . H16B H 0.9727 0.4009 0.5348 0.498 Uiso 1 1 calc . . . H16C H 0.9882 0.4302 0.4636 0.498 Uiso 1 1 calc . . . C17 C 1.0871(6) 0.2762(4) 0.5198(3) 0.087(3) Uani 1 1 d . . . H17A H 1.0951 0.2225 0.5152 0.131 Uiso 1 1 calc . . . H17B H 1.0692 0.2802 0.5626 0.131 Uiso 1 1 calc . . . H17C H 1.1392 0.2970 0.5044 0.131 Uiso 1 1 calc . . . C18 C 1.0677(3) 0.3820(3) 0.2750(2) 0.0415(13) Uani 1 1 d . . . H18 H 1.0168 0.4201 0.2804 0.050 Uiso 1 1 calc R . . C19 C 1.1395(7) 0.4129(6) 0.2858(4) 0.153(5) Uani 1 1 d . . . H19A H 1.1249 0.4309 0.3246 0.230 Uiso 1 1 calc . . . H19B H 1.1535 0.4554 0.2535 0.230 Uiso 1 1 calc . . . H19C H 1.1870 0.3725 0.2865 0.230 Uiso 1 1 calc . . . C20 C 1.0831(4) 0.3610(4) 0.2144(2) 0.0560(16) Uani 1 1 d . . . H20A H 1.1324 0.3228 0.2099 0.084 Uiso 1 1 calc . . . H20B H 1.0917 0.4065 0.1837 0.084 Uiso 1 1 calc . . . H20C H 1.0355 0.3399 0.2093 0.084 Uiso 1 1 calc . . . C21 C 0.7991(2) -0.0095(2) 0.20466(19) 0.0233(9) Uani 1 1 d . . . C22 C 0.7897(3) -0.0886(3) 0.1306(2) 0.0383(12) Uani 1 1 d . . . H22 H 0.8445 -0.1174 0.1377 0.046 Uiso 1 1 calc R . . C23 C 0.7922(4) -0.0695(3) 0.0627(3) 0.0626(18) Uani 1 1 d . . . H23A H 0.7383 -0.0431 0.0548 0.094 Uiso 1 1 calc . . . H23B H 0.8053 -0.1167 0.0456 0.094 Uiso 1 1 calc . . . H23C H 0.8346 -0.0365 0.0441 0.094 Uiso 1 1 calc . . . C24 C 0.7243(4) -0.1365(3) 0.1637(3) 0.0668(19) Uani 1 1 d . . . H24A H 0.7281 -0.1491 0.2065 0.100 Uiso 1 1 calc . . . H24B H 0.7322 -0.1837 0.1470 0.100 Uiso 1 1 calc . . . H24C H 0.6698 -0.1081 0.1592 0.100 Uiso 1 1 calc . . . C25 C 0.7219(3) -0.0961(3) 0.3558(2) 0.0398(12) Uani 1 1 d . . . H25 H 0.7100 -0.0894 0.3142 0.048 Uiso 1 1 calc R . . C26 C 0.6634(3) -0.0404(4) 0.3899(3) 0.0582(16) Uani 1 1 d . . . H26A H 0.6718 -0.0500 0.4317 0.087 Uiso 1 1 calc . . . H26B H 0.6065 -0.0462 0.3892 0.087 Uiso 1 1 calc . . . H26C H 0.6735 0.0116 0.3711 0.087 Uiso 1 1 calc . . . C27 C 0.7204(4) -0.1776(4) 0.3854(3) 0.077(2) Uani 1 1 d . . . H27A H 0.7630 -0.2103 0.3621 0.116 Uiso 1 1 calc . . . H27B H 0.6661 -0.1920 0.3870 0.116 Uiso 1 1 calc . . . H27C H 0.7312 -0.1840 0.4264 0.116 Uiso 1 1 calc . . . C28 C 0.9724(3) -0.1980(3) 0.2555(2) 0.0399(12) Uani 1 1 d . . . H28 H 0.9490 -0.1775 0.2181 0.048 Uiso 1 1 calc R . . C29 C 1.0522(6) -0.1799(8) 0.2442(9) 0.281(11) Uani 1 1 d . . . H29A H 1.0800 -0.2055 0.2777 0.422 Uiso 1 1 calc . . . H29B H 1.0501 -0.1246 0.2401 0.422 Uiso 1 1 calc . . . H29C H 1.0828 -0.1968 0.2068 0.422 Uiso 1 1 calc . . . C30 C 0.9697(8) -0.2780(5) 0.2684(5) 0.186(7) Uani 1 1 d . . . H30A H 0.9856 -0.2989 0.2308 0.280 Uiso 1 1 calc . . . H30B H 0.9136 -0.2877 0.2877 0.280 Uiso 1 1 calc . . . H30C H 1.0081 -0.3026 0.2956 0.280 Uiso 1 1 calc . . . C31 C 0.5190(2) 0.2464(2) 0.15431(18) 0.0201(8) Uani 1 1 d . . . C32 C 0.3906(3) 0.3210(3) 0.1264(2) 0.0301(10) Uani 1 1 d . . . H32 H 0.4110 0.3104 0.0844 0.036 Uiso 1 1 calc R . . C33 C 0.3272(3) 0.2692(3) 0.1581(3) 0.0516(15) Uani 1 1 d . . . H33A H 0.3520 0.2159 0.1578 0.077 Uiso 1 1 calc . . . H33B H 0.2801 0.2804 0.1371 0.077 Uiso 1 1 calc . . . H33C H 0.3083 0.2777 0.1998 0.077 Uiso 1 1 calc . . . C34 C 0.3551(3) 0.4048(3) 0.1235(3) 0.0510(15) Uani 1 1 d . . . H34A H 0.3371 0.4163 0.1645 0.076 Uiso 1 1 calc . . . H34B H 0.3078 0.4158 0.1028 0.076 Uiso 1 1 calc . . . H34C H 0.3975 0.4364 0.1014 0.076 Uiso 1 1 calc . . . C35 C 0.5074(3) 0.0433(3) 0.2056(2) 0.0434(13) Uani 1 1 d . . . H35 H 0.4722 0.0934 0.2099 0.052 Uiso 1 1 calc R . . C36 C 0.5437(4) 0.0128(4) 0.2612(3) 0.0683(19) Uani 1 1 d . . . H36A H 0.5822 -0.0338 0.2553 0.102 Uiso 1 1 calc . . . H36B H 0.4995 0.0012 0.2956 0.102 Uiso 1 1 calc . . . H36C H 0.5733 0.0510 0.2689 0.102 Uiso 1 1 calc . . . C37 C 0.4580(5) -0.0101(6) 0.1919(4) 0.111(3) Uani 1 1 d . . . H37A H 0.4349 0.0131 0.1557 0.167 Uiso 1 1 calc . . . H37B H 0.4130 -0.0206 0.2260 0.167 Uiso 1 1 calc . . . H37C H 0.4936 -0.0579 0.1850 0.167 Uiso 1 1 calc . . . C38 C 0.5018(3) 0.1476(3) 0.0078(2) 0.0377(12) Uani 1 1 d . . . H38 H 0.5054 0.2015 0.0104 0.045 Uiso 1 1 calc R . . C39 C 0.4178(5) 0.1380(5) 0.0096(4) 0.119(4) Uani 1 1 d . . . H39A H 0.4156 0.0855 0.0054 0.178 Uiso 1 1 calc . . . H39B H 0.3964 0.1735 -0.0234 0.178 Uiso 1 1 calc . . . H39C H 0.3840 0.1484 0.0482 0.178 Uiso 1 1 calc . . . C40 C 0.5543(6) 0.1260(8) -0.0471(4) 0.174(6) Uani 1 1 d . . . H40A H 0.5280 0.0913 -0.0624 0.260 Uiso 1 1 calc . . . H40B H 0.6080 0.1003 -0.0382 0.260 Uiso 1 1 calc . . . H40C H 0.5620 0.1717 -0.0775 0.260 Uiso 1 1 calc . . . C41 C 1.0408(2) 0.1449(2) 0.23014(19) 0.0224(9) Uani 1 1 d . . . C42 C 1.1513(3) 0.0905(3) 0.2885(2) 0.0380(12) Uani 1 1 d . . . H42 H 1.1655 0.0526 0.2603 0.046 Uiso 1 1 calc R . . C43 C 1.1448(4) 0.0475(5) 0.3510(3) 0.109(3) Uani 1 1 d . . . H43A H 1.1957 0.0122 0.3548 0.163 Uiso 1 1 calc . . . H43B H 1.0979 0.0187 0.3603 0.163 Uiso 1 1 calc . . . H43C H 1.1364 0.0834 0.3793 0.163 Uiso 1 1 calc . . . C44 C 1.2140(5) 0.1405(5) 0.2722(6) 0.159(5) Uani 1 1 d . . . H44A H 1.2121 0.1697 0.2317 0.238 Uiso 1 1 calc . . . H44B H 1.2684 0.1101 0.2728 0.238 Uiso 1 1 calc . . . H44C H 1.2038 0.1757 0.3011 0.238 Uiso 1 1 calc . . . C45 C 1.1039(3) 0.2476(3) 0.0774(2) 0.0353(11) Uani 1 1 d . . . H45 H 1.1149 0.2433 0.1191 0.042 Uiso 1 1 calc R . . C46 C 1.1844(3) 0.2468(4) 0.0332(3) 0.0597(17) Uani 1 1 d . . . H46A H 1.2198 0.1984 0.0427 0.090 Uiso 1 1 calc . . . H46B H 1.2121 0.2892 0.0359 0.090 Uiso 1 1 calc . . . H46C H 1.1736 0.2523 -0.0078 0.090 Uiso 1 1 calc . . . C47 C 1.0426(3) 0.3171(3) 0.0644(3) 0.0529(15) Uani 1 1 d . . . H47A H 1.0336 0.3227 0.0230 0.079 Uiso 1 1 calc . . . H47B H 1.0639 0.3623 0.0692 0.079 Uiso 1 1 calc . . . H47C H 0.9903 0.3117 0.0925 0.079 Uiso 1 1 calc . . . C48 C 1.1906(3) -0.0078(3) 0.1293(2) 0.0402(12) Uani 1 1 d . . . H48 H 1.1541 -0.0199 0.1693 0.048 Uiso 1 1 calc R . . C49 C 1.2009(6) -0.0725(5) 0.0958(5) 0.129(4) Uani 1 1 d . . . H49A H 1.2503 -0.0701 0.0642 0.194 Uiso 1 1 calc . . . H49B H 1.1524 -0.0690 0.0774 0.194 Uiso 1 1 calc . . . H49C H 1.2068 -0.1208 0.1238 0.194 Uiso 1 1 calc . . . C50 C 1.2677(5) 0.0075(5) 0.1382(4) 0.097(3) Uani 1 1 d . . . H50A H 1.3049 0.0162 0.0992 0.146 Uiso 1 1 calc . . . H50B H 1.2925 -0.0362 0.1644 0.146 Uiso 1 1 calc . . . H50C H 1.2585 0.0530 0.1571 0.146 Uiso 1 1 calc . . . C51 C 0.8400(2) 0.2527(2) 0.03309(17) 0.0206(9) Uani 1 1 d . . . C52 C 0.9314(3) 0.1864(3) -0.04523(19) 0.0314(11) Uani 1 1 d . . . H52 H 0.8845 0.1942 -0.0674 0.038 Uiso 1 1 calc R . . C53 C 0.9744(4) 0.1047(3) -0.0441(2) 0.0584(17) Uani 1 1 d . . . H53A H 1.0183 0.0957 -0.0203 0.088 Uiso 1 1 calc . . . H53B H 0.9983 0.0965 -0.0854 0.088 Uiso 1 1 calc . . . H53C H 0.9342 0.0694 -0.0259 0.088 Uiso 1 1 calc . . . C54 C 0.9898(3) 0.2424(4) -0.0762(2) 0.0515(15) Uani 1 1 d . . . H54A H 0.9606 0.2944 -0.0764 0.077 Uiso 1 1 calc . . . H54B H 1.0110 0.2340 -0.1178 0.077 Uiso 1 1 calc . . . H54C H 1.0358 0.2353 -0.0546 0.077 Uiso 1 1 calc . . . C55 C 0.8556(3) 0.4498(3) -0.0038(2) 0.0294(10) Uani 1 1 d . . . H55 H 0.8892 0.3983 0.0021 0.035 Uiso 1 1 calc R . . C56 C 0.8658(3) 0.4941(3) 0.0415(2) 0.0449(13) Uani 1 1 d . . . H56A H 0.8304 0.5435 0.0372 0.067 Uiso 1 1 calc . . . H56B H 0.9236 0.5024 0.0350 0.067 Uiso 1 1 calc . . . H56C H 0.8503 0.4656 0.0821 0.067 Uiso 1 1 calc . . . C57 C 0.8791(4) 0.4891(4) -0.0681(2) 0.0544(16) Uani 1 1 d . . . H57A H 0.8727 0.4565 -0.0957 0.082 Uiso 1 1 calc . . . H57B H 0.9366 0.4983 -0.0757 0.082 Uiso 1 1 calc . . . H57C H 0.8431 0.5378 -0.0747 0.082 Uiso 1 1 calc . . . C58 C 0.7336(3) 0.3463(3) -0.1166(2) 0.0465(14) Uani 1 1 d . . . H58 H 0.7803 0.3047 -0.1096 0.056 Uiso 1 1 calc R . . C59 C 0.6636(8) 0.3153(11) -0.1137(6) 0.284(12) Uani 1 1 d . . . H59A H 0.6310 0.3471 -0.1426 0.426 Uiso 1 1 calc . . . H59B H 0.6308 0.3128 -0.0729 0.426 Uiso 1 1 calc . . . H59C H 0.6789 0.2637 -0.1236 0.426 Uiso 1 1 calc . . . C60 C 0.7533(11) 0.3907(8) -0.1743(4) 0.251(10) Uani 1 1 d . . . H60A H 0.7044 0.4032 -0.1933 0.377 Uiso 1 1 calc . . . H60B H 0.7978 0.3618 -0.1993 0.377 Uiso 1 1 calc . . . H60C H 0.7712 0.4380 -0.1703 0.377 Uiso 1 1 calc . . . C61 C 0.5251(2) 0.3560(2) 0.38698(19) 0.0223(9) Uani 1 1 d . . . C62 C 0.4790(3) 0.3835(3) 0.4905(2) 0.0329(11) Uani 1 1 d . . . H62 H 0.4449 0.4310 0.4740 0.039 Uiso 1 1 calc R . . C63 C 0.5260(3) 0.4017(3) 0.5347(2) 0.0429(13) Uani 1 1 d . . . H63A H 0.5579 0.3548 0.5521 0.064 Uiso 1 1 calc . . . H63B H 0.4867 0.4236 0.5670 0.064 Uiso 1 1 calc . . . H63C H 0.5634 0.4385 0.5135 0.064 Uiso 1 1 calc . . . C64 C 0.4236(3) 0.3237(3) 0.5206(2) 0.0536(15) Uani 1 1 d . . . H64A H 0.3940 0.3136 0.4912 0.080 Uiso 1 1 calc . . . H64B H 0.3837 0.3423 0.5541 0.080 Uiso 1 1 calc . . . H64C H 0.4570 0.2766 0.5359 0.080 Uiso 1 1 calc . . . C65 C 0.3160(3) 0.5138(4) 0.3625(3) 0.0661(19) Uani 1 1 d . . . H65 H 0.3277 0.4922 0.4038 0.079 Uiso 1 1 calc R . . C66 C 0.3649(4) 0.5745(4) 0.3375(4) 0.072(2) Uani 1 1 d . . . H66A H 0.4236 0.5536 0.3329 0.108 Uiso 1 1 calc . . . H66B H 0.3527 0.6122 0.3644 0.108 Uiso 1 1 calc . . . H66C H 0.3519 0.5989 0.2980 0.108 Uiso 1 1 calc . . . C67 C 0.2234(4) 0.5427(4) 0.3685(4) 0.097(3) Uani 1 1 d . . . H67A H 0.2102 0.5638 0.3285 0.146 Uiso 1 1 calc . . . H67B H 0.2087 0.5825 0.3939 0.146 Uiso 1 1 calc . . . H67C H 0.1921 0.5002 0.3871 0.146 Uiso 1 1 calc . . . C68 C 0.3765(3) 0.2591(3) 0.3582(2) 0.0443(13) Uani 1 1 d . . . H68 H 0.4141 0.2593 0.3865 0.053 Uiso 1 1 calc R . . C69 C 0.4026(4) 0.1881(3) 0.3299(3) 0.0549(15) Uani 1 1 d . . . H69A H 0.3686 0.1893 0.2999 0.082 Uiso 1 1 calc . . . H69B H 0.3953 0.1430 0.3612 0.082 Uiso 1 1 calc . . . H69C H 0.4607 0.1859 0.3104 0.082 Uiso 1 1 calc . . . C70 C 0.2889(5) 0.2672(4) 0.3915(4) 0.094(3) Uani 1 1 d . . . H70A H 0.2768 0.3142 0.4089 0.141 Uiso 1 1 calc . . . H70B H 0.2813 0.2233 0.4238 0.141 Uiso 1 1 calc . . . H70C H 0.2514 0.2696 0.3636 0.141 Uiso 1 1 calc . . . C71 C 0.6531(2) 0.5070(2) 0.16392(18) 0.0189(8) Uani 1 1 d . . . C72 C 0.5823(3) 0.5856(3) 0.0844(2) 0.0321(11) Uani 1 1 d . . . H72 H 0.5467 0.6138 0.1160 0.039 Uiso 1 1 calc R . . C73 C 0.6461(4) 0.6350(3) 0.0473(2) 0.0505(15) Uani 1 1 d . . . H73A H 0.6798 0.6460 0.0737 0.076 Uiso 1 1 calc . . . H73B H 0.6180 0.6829 0.0280 0.076 Uiso 1 1 calc . . . H73C H 0.6816 0.6078 0.0163 0.076 Uiso 1 1 calc . . . C74 C 0.5275(4) 0.5677(3) 0.0456(3) 0.0532(16) Uani 1 1 d . . . H74A H 0.5605 0.5350 0.0174 0.080 Uiso 1 1 calc . . . H74B H 0.5036 0.6153 0.0229 0.080 Uiso 1 1 calc . . . H74C H 0.4831 0.5411 0.0714 0.080 Uiso 1 1 calc . . . C75 C 0.5541(3) 0.6960(3) 0.2649(3) 0.0521(15) Uani 1 1 d . . . H75 H 0.5199 0.6538 0.2815 0.063 Uiso 1 1 calc R . . C76 C 0.5426(5) 0.7484(4) 0.3090(3) 0.085(3) Uani 1 1 d . . . H76A H 0.5626 0.7207 0.3455 0.128 Uiso 1 1 calc . . . H76B H 0.4839 0.7679 0.3193 0.128 Uiso 1 1 calc . . . H76C H 0.5739 0.7911 0.2912 0.128 Uiso 1 1 calc . . . C77 C 0.5331(5) 0.7379(4) 0.2050(4) 0.102(3) Uani 1 1 d . . . H77A H 0.5624 0.7825 0.1914 0.153 Uiso 1 1 calc . . . H77B H 0.4734 0.7546 0.2098 0.153 Uiso 1 1 calc . . . H77C H 0.5497 0.7037 0.1751 0.153 Uiso 1 1 calc . . . C78 C 0.8254(3) 0.5752(3) 0.1880(2) 0.0333(11) Uani 1 1 d . . . H78 H 0.8088 0.5426 0.1635 0.040 Uiso 1 1 calc R . . C79 C 0.9073(3) 0.5388(3) 0.2043(3) 0.0549(16) Uani 1 1 d . . . H79A H 0.9236 0.5690 0.2297 0.082 Uiso 1 1 calc . . . H79B H 0.9490 0.5367 0.1675 0.082 Uiso 1 1 calc . . . H79C H 0.9027 0.4869 0.2264 0.082 Uiso 1 1 calc . . . C80 C 0.8269(4) 0.6531(4) 0.1527(3) 0.0683(19) Uani 1 1 d . . . H80A H 0.7731 0.6721 0.1409 0.102 Uiso 1 1 calc . . . H80B H 0.8699 0.6519 0.1165 0.102 Uiso 1 1 calc . . . H80C H 0.8386 0.6869 0.1773 0.102 Uiso 1 1 calc . . . 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 0.0251(3) 0.0239(3) 0.0192(3) -0.0033(2) -0.0043(2) -0.0012(2) Cu2 0.0235(3) 0.0226(3) 0.0206(3) -0.0038(2) -0.0067(2) -0.0010(2) Cu3 0.0258(3) 0.0211(3) 0.0204(3) -0.0024(2) -0.0072(2) -0.0019(2) Cu4 0.0229(3) 0.0225(3) 0.0232(3) -0.0057(2) -0.0072(2) -0.0002(2) Cu5 0.0226(3) 0.0218(3) 0.0197(3) -0.0034(2) -0.0060(2) -0.0002(2) Cu6 0.0220(3) 0.0223(3) 0.0196(3) -0.0037(2) -0.0060(2) 0.0004(2) Cu7 0.0223(3) 0.0255(3) 0.0209(3) -0.0058(2) -0.0055(2) 0.0005(2) Cu8 0.0255(3) 0.0219(3) 0.0197(3) -0.0040(2) -0.0063(2) -0.0010(2) S1 0.0240(5) 0.0196(5) 0.0175(5) -0.0014(4) -0.0052(4) -0.0026(4) S2 0.0308(6) 0.0256(6) 0.0207(5) -0.0045(4) -0.0051(4) -0.0043(5) S3 0.0214(5) 0.0189(5) 0.0174(5) -0.0032(4) -0.0058(4) -0.0017(4) S4 0.0275(6) 0.0238(6) 0.0203(5) -0.0012(4) -0.0089(4) -0.0013(4) S5 0.0214(5) 0.0196(5) 0.0207(5) -0.0031(4) -0.0067(4) -0.0020(4) S6 0.0250(5) 0.0207(5) 0.0252(5) -0.0022(4) -0.0081(4) -0.0019(4) S7 0.0191(5) 0.0206(5) 0.0195(5) -0.0043(4) -0.0057(4) -0.0009(4) S8 0.0270(6) 0.0271(6) 0.0227(5) -0.0081(5) -0.0069(4) 0.0010(4) S9 0.0204(5) 0.0190(5) 0.0181(5) -0.0035(4) -0.0055(4) -0.0015(4) S10 0.0272(6) 0.0212(5) 0.0226(5) -0.0061(4) -0.0049(4) -0.0004(4) S11 0.0184(5) 0.0206(5) 0.0161(5) -0.0025(4) -0.0043(4) 0.0004(4) S12 0.0224(5) 0.0253(6) 0.0233(5) -0.0034(4) -0.0093(4) -0.0002(4) S13 0.0208(5) 0.0221(5) 0.0180(5) -0.0042(4) -0.0035(4) -0.0012(4) S14 0.0235(5) 0.0279(6) 0.0257(6) -0.0060(5) -0.0062(4) 0.0012(4) S15 0.0220(5) 0.0183(5) 0.0170(5) -0.0027(4) -0.0058(4) -0.0011(4) S16 0.0259(5) 0.0233(6) 0.0227(5) -0.0071(4) -0.0053(4) 0.0011(4) N1 0.033(2) 0.025(2) 0.0180(18) -0.0029(15) -0.0041(15) -0.0036(16) N2 0.034(2) 0.026(2) 0.0168(18) 0.0004(15) -0.0064(15) 0.0017(16) N3 0.0247(19) 0.023(2) 0.030(2) -0.0057(16) -0.0101(16) -0.0011(15) N4 0.0254(19) 0.031(2) 0.034(2) -0.0160(17) -0.0126(16) 0.0041(16) N5 0.030(2) 0.0196(19) 0.028(2) -0.0031(15) -0.0115(16) -0.0029(15) N6 0.030(2) 0.0185(19) 0.028(2) -0.0056(15) -0.0123(16) 0.0025(15) N7 0.0207(18) 0.026(2) 0.034(2) -0.0097(17) -0.0100(16) 0.0004(15) N8 0.0189(18) 0.025(2) 0.031(2) -0.0124(16) -0.0107(15) 0.0031(15) N9 0.0183(18) 0.036(2) 0.0212(19) -0.0070(16) -0.0049(14) 0.0003(15) N10 0.0218(19) 0.043(2) 0.0188(18) -0.0095(17) -0.0069(15) 0.0052(16) N11 0.0279(19) 0.0242(19) 0.0168(17) -0.0033(15) -0.0061(14) 0.0022(15) N12 0.028(2) 0.027(2) 0.0178(18) -0.0020(15) -0.0080(15) 0.0091(16) N13 0.0193(18) 0.031(2) 0.0246(19) -0.0064(16) -0.0049(15) 0.0018(15) N14 0.0246(19) 0.037(2) 0.0204(19) -0.0081(16) -0.0035(15) 0.0001(16) N15 0.031(2) 0.0186(19) 0.0247(19) -0.0037(15) -0.0114(15) 0.0006(15) N16 0.033(2) 0.0189(19) 0.0238(19) -0.0036(15) -0.0124(16) 0.0002(15) P1 0.0325(6) 0.0284(6) 0.0167(5) -0.0033(5) -0.0014(5) -0.0054(5) P2 0.0232(6) 0.0261(6) 0.0230(6) -0.0040(5) -0.0099(4) -0.0021(5) P3 0.0300(6) 0.0182(6) 0.0250(6) -0.0006(5) -0.0103(5) -0.0032(5) P4 0.0261(6) 0.0228(6) 0.0265(6) -0.0077(5) -0.0103(5) 0.0001(5) P5 0.0219(6) 0.0269(6) 0.0192(5) -0.0051(5) -0.0044(4) 0.0026(5) P6 0.0272(6) 0.0219(6) 0.0172(5) -0.0011(4) -0.0067(4) 0.0014(5) P7 0.0207(6) 0.0286(6) 0.0284(6) -0.0083(5) -0.0053(5) 0.0001(5) P8 0.0266(6) 0.0208(6) 0.0235(6) -0.0060(5) -0.0082(5) -0.0013(5) O1 0.0289(17) 0.0335(19) 0.0334(18) -0.0060(15) 0.0009(14) -0.0047(14) O2 0.052(2) 0.041(2) 0.0160(16) -0.0053(14) -0.0037(14) -0.0013(16) O3 0.0287(17) 0.0362(19) 0.0276(17) -0.0007(14) -0.0017(13) -0.0049(14) O4 0.0280(17) 0.0369(19) 0.0338(18) -0.0088(15) -0.0173(14) -0.0024(14) O5 0.0319(17) 0.0358(19) 0.0254(17) 0.0014(14) -0.0089(13) -0.0121(14) O6 0.0415(19) 0.0173(16) 0.0347(18) -0.0003(13) -0.0173(15) 0.0013(13) O7 0.0265(16) 0.0288(18) 0.0343(18) -0.0054(14) -0.0060(13) -0.0013(13) O8 0.0350(18) 0.0271(17) 0.0379(19) -0.0141(15) -0.0168(15) 0.0015(14) O9 0.0333(17) 0.0286(17) 0.0228(16) -0.0008(13) -0.0086(13) -0.0074(14) O10 0.0258(17) 0.046(2) 0.0251(17) -0.0118(15) -0.0047(13) 0.0103(14) O11 0.0253(16) 0.0244(16) 0.0249(16) -0.0031(13) -0.0011(12) -0.0016(13) O12 0.046(2) 0.0267(17) 0.0196(16) -0.0017(13) -0.0106(14) 0.0084(14) O13 0.0202(16) 0.041(2) 0.0379(19) -0.0143(16) -0.0045(13) 0.0034(14) O14 0.0318(18) 0.0336(19) 0.0362(19) -0.0066(15) -0.0085(14) -0.0095(14) O15 0.0366(18) 0.0206(16) 0.0365(18) -0.0092(14) -0.0119(14) -0.0006(13) O16 0.0233(16) 0.041(2) 0.0261(17) -0.0067(14) -0.0054(13) -0.0035(14) C1 0.023(2) 0.023(2) 0.021(2) 0.0009(17) -0.0063(17) -0.0078(18) C2 0.044(3) 0.032(3) 0.022(2) 0.002(2) -0.013(2) -0.001(2) C3 0.063(4) 0.038(3) 0.030(3) 0.003(2) -0.022(3) 0.017(3) C4 0.070(4) 0.044(3) 0.036(3) 0.018(3) -0.015(3) -0.018(3) C5 0.034(3) 0.032(3) 0.048(3) -0.003(2) 0.000(2) -0.010(2) C6 0.059(4) 0.057(4) 0.064(4) -0.013(3) -0.022(3) -0.021(3) C7 0.066(4) 0.072(5) 0.061(4) 0.012(3) -0.009(3) -0.037(4) C8 0.111(8) 0.48(2) 0.023(4) -0.038(8) -0.021(4) -0.088(11) C9 0.099(7) 0.171(9) 0.064(5) 0.013(6) -0.042(5) -0.044(6) C10 0.079(6) 0.46(2) 0.020(4) -0.032(7) -0.005(4) -0.059(9) C11 0.023(2) 0.023(2) 0.020(2) -0.0026(17) -0.0059(17) -0.0054(17) C12 0.042(3) 0.032(3) 0.049(3) -0.028(2) -0.021(2) 0.006(2) C13 0.312(14) 0.097(6) 0.051(5) -0.016(4) -0.011(6) -0.146(8) C14 0.173(9) 0.109(7) 0.062(5) -0.056(5) 0.030(5) -0.075(6) C15 0.039(3) 0.171(8) 0.050(4) -0.066(5) -0.014(3) -0.013(4) C16 0.48(2) 0.317(18) 0.257(15) -0.256(15) -0.322(18) 0.332(19) C17 0.170(8) 0.052(4) 0.042(4) -0.003(3) -0.051(5) 0.011(5) C18 0.047(3) 0.035(3) 0.036(3) 0.007(2) 0.001(2) -0.015(2) C19 0.242(12) 0.184(10) 0.079(6) 0.022(6) -0.043(7) -0.186(10) C20 0.067(4) 0.064(4) 0.033(3) 0.004(3) -0.001(3) -0.024(3) C21 0.022(2) 0.023(2) 0.025(2) -0.0054(18) -0.0027(17) -0.0051(17) C22 0.049(3) 0.027(3) 0.047(3) -0.021(2) -0.025(3) 0.008(2) C23 0.097(5) 0.048(4) 0.047(4) -0.022(3) -0.037(3) 0.024(3) C24 0.075(5) 0.035(3) 0.105(6) -0.027(4) -0.033(4) -0.009(3) C25 0.034(3) 0.052(3) 0.036(3) 0.002(2) -0.007(2) -0.022(2) C26 0.033(3) 0.075(5) 0.060(4) -0.005(3) -0.001(3) -0.010(3) C27 0.082(5) 0.053(4) 0.100(6) -0.008(4) -0.003(4) -0.040(4) C28 0.042(3) 0.029(3) 0.044(3) -0.002(2) -0.013(2) 0.007(2) C29 0.059(6) 0.242(14) 0.60(3) -0.345(19) 0.071(11) -0.031(7) C30 0.254(13) 0.065(6) 0.196(12) -0.081(7) 0.138(10) -0.057(7) C31 0.0155(19) 0.022(2) 0.021(2) -0.0039(17) 0.0011(16) -0.0040(16) C32 0.023(2) 0.035(3) 0.035(3) -0.013(2) -0.0105(19) 0.0025(19) C33 0.028(3) 0.059(4) 0.075(4) -0.022(3) -0.019(3) -0.001(3) C34 0.046(3) 0.047(3) 0.067(4) -0.022(3) -0.039(3) 0.022(3) C35 0.035(3) 0.038(3) 0.048(3) 0.003(3) 0.002(2) -0.007(2) C36 0.075(5) 0.089(5) 0.038(3) 0.010(3) -0.006(3) -0.033(4) C37 0.092(6) 0.172(9) 0.084(6) 0.016(6) -0.022(5) -0.092(6) C38 0.045(3) 0.038(3) 0.036(3) -0.011(2) -0.021(2) 0.001(2) C39 0.071(5) 0.152(9) 0.126(7) 0.069(6) -0.066(5) -0.040(5) C40 0.089(7) 0.357(18) 0.041(5) 0.001(8) -0.018(4) 0.027(9) C41 0.019(2) 0.025(2) 0.024(2) -0.0013(18) -0.0045(17) -0.0081(17) C42 0.027(2) 0.061(4) 0.025(2) -0.012(2) -0.011(2) 0.010(2) C43 0.065(5) 0.154(8) 0.076(5) 0.013(5) -0.033(4) 0.055(5) C44 0.049(5) 0.081(6) 0.346(16) 0.042(8) -0.100(7) -0.020(4) C45 0.038(3) 0.035(3) 0.035(3) -0.002(2) -0.008(2) -0.014(2) C46 0.039(3) 0.060(4) 0.075(4) 0.000(3) 0.002(3) -0.019(3) C47 0.051(3) 0.033(3) 0.074(4) -0.009(3) -0.005(3) -0.010(3) C48 0.030(3) 0.048(3) 0.042(3) -0.017(3) -0.011(2) 0.013(2) C49 0.126(8) 0.070(6) 0.225(12) -0.072(7) -0.106(8) 0.042(5) C50 0.070(5) 0.088(6) 0.139(8) -0.028(6) -0.036(5) 0.005(4) C51 0.027(2) 0.021(2) 0.015(2) -0.0018(17) -0.0051(16) -0.0070(17) C52 0.036(3) 0.034(3) 0.022(2) -0.010(2) -0.0043(19) 0.006(2) C53 0.086(5) 0.052(4) 0.028(3) -0.020(3) -0.010(3) 0.027(3) C54 0.047(3) 0.073(4) 0.030(3) -0.013(3) 0.007(2) -0.008(3) C55 0.023(2) 0.029(3) 0.032(3) -0.003(2) 0.0010(19) -0.0041(19) C56 0.042(3) 0.060(4) 0.038(3) -0.009(3) -0.007(2) -0.019(3) C57 0.059(4) 0.077(4) 0.032(3) -0.008(3) 0.006(3) -0.038(3) C58 0.061(4) 0.052(3) 0.026(3) -0.014(2) -0.027(3) 0.023(3) C59 0.168(12) 0.57(3) 0.221(14) -0.312(19) 0.075(10) -0.204(16) C60 0.49(2) 0.276(16) 0.036(5) -0.063(8) 0.058(9) -0.261(17) C61 0.020(2) 0.021(2) 0.025(2) -0.0047(18) 0.0010(17) -0.0058(17) C62 0.032(3) 0.039(3) 0.025(2) -0.009(2) -0.0004(19) 0.002(2) C63 0.044(3) 0.055(4) 0.031(3) -0.024(3) -0.008(2) 0.008(3) C64 0.053(4) 0.064(4) 0.039(3) -0.013(3) 0.013(3) -0.019(3) C65 0.036(3) 0.068(5) 0.098(5) -0.051(4) -0.006(3) 0.015(3) C66 0.058(4) 0.052(4) 0.110(6) -0.034(4) -0.008(4) 0.000(3) C67 0.037(4) 0.095(6) 0.171(9) -0.083(6) -0.011(4) 0.018(4) C68 0.049(3) 0.041(3) 0.043(3) -0.001(3) -0.004(3) -0.020(3) C69 0.057(4) 0.039(3) 0.068(4) -0.006(3) -0.010(3) -0.010(3) C70 0.090(6) 0.068(5) 0.104(6) -0.022(5) 0.046(5) -0.030(4) C71 0.019(2) 0.016(2) 0.022(2) -0.0003(16) -0.0065(16) -0.0034(16) C72 0.042(3) 0.024(2) 0.034(3) -0.006(2) -0.023(2) 0.007(2) C73 0.069(4) 0.040(3) 0.041(3) 0.011(3) -0.022(3) -0.008(3) C74 0.071(4) 0.036(3) 0.063(4) 0.000(3) -0.052(3) 0.002(3) C75 0.039(3) 0.025(3) 0.086(5) -0.007(3) -0.010(3) 0.007(2) C76 0.104(6) 0.090(6) 0.046(4) -0.028(4) -0.018(4) 0.051(4) C77 0.118(6) 0.090(6) 0.117(7) -0.068(5) -0.085(6) 0.071(5) C78 0.028(2) 0.042(3) 0.029(3) -0.001(2) -0.001(2) -0.013(2) C79 0.034(3) 0.060(4) 0.058(4) 0.005(3) 0.003(3) -0.002(3) C80 0.065(4) 0.064(4) 0.067(4) 0.027(3) -0.017(3) -0.022(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 S2 2.2958(12) . ? Cu1 S1 2.3268(12) . ? Cu1 S13 2.3590(11) . ? Cu1 S3 2.4648(11) . ? Cu1 Cu2 2.6914(8) . ? Cu1 Cu8 2.7496(8) . ? Cu2 S4 2.3002(11) . ? Cu2 S3 2.3256(11) . ? Cu2 S9 2.3495(11) . ? Cu2 S1 2.4576(11) . ? Cu2 Cu3 2.8112(8) . ? Cu3 S6 2.3033(12) . ? Cu3 S5 2.3302(11) . ? Cu3 S1 2.3526(11) . ? Cu3 S9 2.4785(11) . ? Cu3 Cu5 2.6684(8) . ? Cu4 S8 2.3030(12) . ? Cu4 S7 2.3377(11) . ? Cu4 S5 2.3560(11) . ? Cu4 S11 2.4688(11) . ? Cu4 Cu6 2.6889(8) . ? Cu4 Cu5 2.8147(8) . ? Cu5 S10 2.2966(12) . ? Cu5 S9 2.3381(11) . ? Cu5 S11 2.3443(11) . ? Cu5 S5 2.4661(11) . ? Cu6 S12 2.2988(11) . ? Cu6 S11 2.3255(11) . ? Cu6 S15 2.3591(11) . ? Cu6 S7 2.4634(11) . ? Cu6 Cu7 2.7449(8) . ? Cu7 S14 2.2967(12) . ? Cu7 S13 2.3189(11) . ? Cu7 S7 2.3581(11) . ? Cu7 S15 2.4751(11) . ? Cu7 Cu8 2.7447(7) . ? Cu8 S16 2.3039(12) . ? Cu8 S15 2.3276(11) . ? Cu8 S3 2.3700(11) . ? Cu8 S13 2.4517(11) . ? S1 C1 1.769(4) . ? S2 P1 1.9709(16) . ? S3 C11 1.771(4) . ? S4 P2 1.9786(16) . ? S5 C21 1.776(4) . ? S6 P3 1.9713(15) . ? S7 C31 1.779(4) . ? S8 P4 1.9737(16) . ? S9 C41 1.765(4) . ? S10 P5 1.9720(16) . ? S11 C51 1.772(4) . ? S12 P6 1.9701(15) . ? S13 C61 1.773(4) . ? S14 P7 1.9735(16) . ? S15 C71 1.774(4) . ? S16 P8 1.9799(16) . ? N1 C1 1.311(5) . ? N1 P1 1.594(4) . ? N2 C1 1.330(5) . ? N2 C2 1.465(5) . ? N3 C11 1.315(5) . ? N3 P2 1.594(4) . ? N4 C11 1.322(5) . ? N4 C12 1.469(5) . ? N5 C21 1.306(5) . ? N5 P3 1.599(4) . ? N6 C21 1.328(5) . ? N6 C22 1.471(5) . ? N7 C31 1.311(5) . ? N7 P4 1.593(4) . ? N8 C31 1.328(5) . ? N8 C32 1.470(5) . ? N9 C41 1.307(5) . ? N9 P5 1.594(3) . ? N10 C41 1.333(5) . ? N10 C42 1.464(5) . ? N11 C51 1.308(5) . ? N11 P6 1.595(3) . ? N12 C51 1.331(5) . ? N12 C52 1.460(5) . ? N13 C61 1.312(5) . ? N13 P7 1.604(4) . ? N14 C61 1.320(5) . ? N14 C62 1.473(5) . ? N15 C71 1.307(5) . ? N15 P8 1.594(3) . ? N16 C71 1.324(5) . ? N16 C72 1.462(5) . ? P1 O2 1.575(3) . ? P1 O1 1.590(3) . ? P2 O3 1.574(3) . ? P2 O4 1.587(3) . ? P3 O5 1.581(3) . ? P3 O6 1.584(3) . ? P4 O7 1.577(3) . ? P4 O8 1.586(3) . ? P5 O9 1.579(3) . ? P5 O10 1.581(3) . ? P6 O11 1.581(3) . ? P6 O12 1.584(3) . ? P7 O14 1.584(3) . ? P7 O13 1.586(3) . ? P8 O16 1.576(3) . ? P8 O15 1.583(3) . ? O1 C5 1.464(5) . ? O2 C8 1.4508(10) . ? O3 C18 1.460(5) . ? O4 C15 1.428(6) . ? O5 C25 1.468(5) . ? O6 C28 1.457(6) . ? O7 C35 1.457(6) . ? O8 C38 1.459(5) . ? O9 C45 1.465(5) . ? O10 C48 1.452(6) . ? O11 C55 1.457(5) . ? O12 C58 1.452(6) . ? O13 C65 1.428(6) . ? O14 C68 1.457(6) . ? O15 C75 1.455(6) . ? O16 C78 1.453(5) . ? C2 C3 1.524(7) . ? C2 C4 1.524(7) . ? C5 C6 1.506(7) . ? C5 C7 1.520(7) . ? C8 C9 1.5085(10) . ? C8 C10 1.5108(10) . ? C12 C13 1.470(9) . ? C12 C14 1.475(9) . ? C15 C17 1.439(9) . ? C15 C16 1.449(14) . ? C18 C20 1.478(7) . ? C18 C19 1.494(9) . ? C22 C24 1.498(8) . ? C22 C23 1.525(7) . ? C25 C26 1.494(8) . ? C25 C27 1.496(8) . ? C28 C29 1.389(10) . ? C28 C30 1.424(9) . ? C32 C33 1.511(7) . ? C32 C34 1.520(7) . ? C35 C37 1.493(9) . ? C35 C36 1.498(8) . ? C38 C39 1.438(8) . ? C38 C40 1.459(10) . ? C42 C44 1.446(9) . ? C42 C43 1.486(8) . ? C45 C47 1.498(7) . ? C45 C46 1.507(7) . ? C48 C50 1.430(8) . ? C48 C49 1.490(9) . ? C52 C54 1.499(7) . ? C52 C53 1.522(7) . ? C55 C56 1.487(7) . ? C55 C57 1.512(7) . ? C58 C59 1.370(11) . ? C58 C60 1.415(11) . ? C62 C64 1.512(7) . ? C62 C63 1.525(6) . ? C65 C66 1.437(9) . ? C65 C67 1.532(8) . ? C68 C70 1.501(8) . ? C68 C69 1.507(8) . ? C72 C74 1.521(6) . ? C72 C73 1.520(7) . ? C75 C76 1.482(8) . ? C75 C77 1.515(9) . ? C78 C80 1.480(7) . ? C78 C79 1.502(7) . ? 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 110.72(4) . . ? S2 Cu1 S13 120.58(4) . . ? S1 Cu1 S13 103.65(4) . . ? S2 Cu1 S3 104.35(4) . . ? S1 Cu1 S3 108.90(4) . . ? S13 Cu1 S3 108.34(4) . . ? S2 Cu1 Cu2 106.46(4) . . ? S1 Cu1 Cu2 58.10(3) . . ? S13 Cu1 Cu2 132.90(3) . . ? S3 Cu1 Cu2 53.40(3) . . ? S2 Cu1 Cu8 117.15(4) . . ? S1 Cu1 Cu8 131.69(3) . . ? S13 Cu1 Cu8 56.74(3) . . ? S3 Cu1 Cu8 53.73(3) . . ? Cu2 Cu1 Cu8 100.81(2) . . ? S4 Cu2 S3 110.55(4) . . ? S4 Cu2 S9 122.05(4) . . ? S3 Cu2 S9 102.98(4) . . ? S4 Cu2 S1 104.83(4) . . ? S3 Cu2 S1 109.18(4) . . ? S9 Cu2 S1 106.85(4) . . ? S4 Cu2 Cu1 106.82(3) . . ? S3 Cu2 Cu1 58.31(3) . . ? S9 Cu2 Cu1 131.05(3) . . ? S1 Cu2 Cu1 53.50(3) . . ? S4 Cu2 Cu3 117.98(4) . . ? S3 Cu2 Cu3 130.95(3) . . ? S9 Cu2 Cu3 56.56(3) . . ? S1 Cu2 Cu3 52.52(3) . . ? Cu1 Cu2 Cu3 99.50(2) . . ? S6 Cu3 S5 109.99(4) . . ? S6 Cu3 S1 121.62(4) . . ? S5 Cu3 S1 105.30(4) . . ? S6 Cu3 S9 103.43(4) . . ? S5 Cu3 S9 110.14(4) . . ? S1 Cu3 S9 106.08(4) . . ? S6 Cu3 Cu5 105.84(3) . . ? S5 Cu3 Cu5 58.66(3) . . ? S1 Cu3 Cu5 132.26(3) . . ? S9 Cu3 Cu5 53.88(3) . . ? S6 Cu3 Cu2 115.88(3) . . ? S5 Cu3 Cu2 133.46(3) . . ? S1 Cu3 Cu2 56.00(3) . . ? S9 Cu3 Cu2 52.28(3) . . ? Cu5 Cu3 Cu2 100.28(2) . . ? S8 Cu4 S7 110.88(4) . . ? S8 Cu4 S5 121.23(4) . . ? S7 Cu4 S5 104.48(4) . . ? S8 Cu4 S11 104.43(4) . . ? S7 Cu4 S11 108.98(4) . . ? S5 Cu4 S11 106.39(4) . . ? S8 Cu4 Cu6 106.74(4) . . ? S7 Cu4 Cu6 58.19(3) . . ? S5 Cu4 Cu6 131.82(3) . . ? S11 Cu4 Cu6 53.39(3) . . ? S8 Cu4 Cu5 117.53(3) . . ? S7 Cu4 Cu5 130.94(3) . . ? S5 Cu4 Cu5 56.13(3) . . ? S11 Cu4 Cu5 52.18(3) . . ? Cu6 Cu4 Cu5 99.14(2) . . ? S10 Cu5 S9 110.41(4) . . ? S10 Cu5 S11 121.79(4) . . ? S9 Cu5 S11 103.63(4) . . ? S10 Cu5 S5 103.66(4) . . ? S9 Cu5 S5 110.31(4) . . ? S11 Cu5 S5 106.85(4) . . ? S10 Cu5 Cu3 106.48(3) . . ? S9 Cu5 Cu3 58.91(3) . . ? S11 Cu5 Cu3 131.58(3) . . ? S5 Cu5 Cu3 53.80(3) . . ? S10 Cu5 Cu4 117.41(3) . . ? S9 Cu5 Cu4 131.65(3) . . ? S11 Cu5 Cu4 56.29(3) . . ? S5 Cu5 Cu4 52.49(3) . . ? Cu3 Cu5 Cu4 99.54(2) . . ? S12 Cu6 S11 110.54(4) . . ? S12 Cu6 S15 122.01(4) . . ? S11 Cu6 S15 102.71(4) . . ? S12 Cu6 S7 103.09(4) . . ? S11 Cu6 S7 109.58(4) . . ? S15 Cu6 S7 108.68(4) . . ? S12 Cu6 Cu4 105.19(3) . . ? S11 Cu6 Cu4 58.45(3) . . ? S15 Cu6 Cu4 132.75(3) . . ? S7 Cu6 Cu4 53.75(3) . . ? S12 Cu6 Cu7 116.90(4) . . ? S11 Cu6 Cu7 132.00(3) . . ? S15 Cu6 Cu7 57.42(3) . . ? S7 Cu6 Cu7 53.51(3) . . ? Cu4 Cu6 Cu7 100.96(2) . . ? S14 Cu7 S13 111.04(4) . . ? S14 Cu7 S7 121.27(4) . . ? S13 Cu7 S7 104.59(4) . . ? S14 Cu7 S15 103.69(4) . . ? S13 Cu7 S15 107.27(4) . . ? S7 Cu7 S15 108.33(4) . . ? S14 Cu7 Cu8 105.80(4) . . ? S13 Cu7 Cu8 57.18(3) . . ? S7 Cu7 Cu8 132.80(3) . . ? S15 Cu7 Cu8 52.65(3) . . ? S14 Cu7 Cu6 116.74(4) . . ? S13 Cu7 Cu6 131.35(3) . . ? S7 Cu7 Cu6 57.12(3) . . ? S15 Cu7 Cu6 53.43(3) . . ? Cu8 Cu7 Cu6 100.06(2) . . ? S16 Cu8 S15 110.93(4) . . ? S16 Cu8 S3 119.92(4) . . ? S15 Cu8 S3 103.30(4) . . ? S16 Cu8 S13 106.02(4) . . ? S15 Cu8 S13 107.76(4) . . ? S3 Cu8 S13 108.42(4) . . ? S16 Cu8 Cu7 108.01(3) . . ? S15 Cu8 Cu7 57.71(3) . . ? S3 Cu8 Cu7 132.04(3) . . ? S13 Cu8 Cu7 52.64(3) . . ? S16 Cu8 Cu1 118.30(4) . . ? S15 Cu8 Cu1 130.38(3) . . ? S3 Cu8 Cu1 56.98(3) . . ? S13 Cu8 Cu1 53.57(3) . . ? Cu7 Cu8 Cu1 99.65(2) . . ? C1 S1 Cu1 108.11(14) . . ? C1 S1 Cu3 110.90(15) . . ? Cu1 S1 Cu3 127.70(5) . . ? C1 S1 Cu2 100.31(13) . . ? Cu1 S1 Cu2 68.40(3) . . ? Cu3 S1 Cu2 71.48(3) . . ? P1 S2 Cu1 93.36(5) . . ? C11 S3 Cu2 106.89(14) . . ? C11 S3 Cu8 111.76(14) . . ? Cu2 S3 Cu8 126.49(5) . . ? C11 S3 Cu1 100.77(14) . . ? Cu2 S3 Cu1 68.29(3) . . ? Cu8 S3 Cu1 69.29(3) . . ? P2 S4 Cu2 93.39(5) . . ? C21 S5 Cu3 107.95(14) . . ? C21 S5 Cu4 111.56(14) . . ? Cu3 S5 Cu4 126.63(5) . . ? C21 S5 Cu5 100.13(14) . . ? Cu3 S5 Cu5 67.54(3) . . ? Cu4 S5 Cu5 71.38(3) . . ? P3 S6 Cu3 93.35(5) . . ? C31 S7 Cu4 106.39(13) . . ? C31 S7 Cu7 111.37(14) . . ? Cu4 S7 Cu7 126.41(5) . . ? C31 S7 Cu6 99.48(13) . . ? Cu4 S7 Cu6 68.06(3) . . ? Cu7 S7 Cu6 69.36(3) . . ? P4 S8 Cu4 92.33(5) . . ? C41 S9 Cu5 106.08(14) . . ? C41 S9 Cu2 110.72(14) . . ? Cu5 S9 Cu2 127.67(5) . . ? C41 S9 Cu3 99.30(14) . . ? Cu5 S9 Cu3 67.21(3) . . ? Cu2 S9 Cu3 71.16(3) . . ? P5 S10 Cu5 93.65(5) . . ? C51 S11 Cu6 108.16(14) . . ? C51 S11 Cu5 110.97(14) . . ? Cu6 S11 Cu5 127.61(5) . . ? C51 S11 Cu4 100.63(13) . . ? Cu6 S11 Cu4 68.15(3) . . ? Cu5 S11 Cu4 71.52(3) . . ? P6 S12 Cu6 93.12(5) . . ? C61 S13 Cu7 108.41(14) . . ? C61 S13 Cu1 111.25(14) . . ? Cu7 S13 Cu1 127.65(5) . . ? C61 S13 Cu8 101.32(14) . . ? Cu7 S13 Cu8 70.19(3) . . ? Cu1 S13 Cu8 69.69(3) . . ? P7 S14 Cu7 93.20(6) . . ? C71 S15 Cu8 106.42(14) . . ? C71 S15 Cu6 111.10(13) . . ? Cu8 S15 Cu6 127.71(5) . . ? C71 S15 Cu7 99.88(13) . . ? Cu8 S15 Cu7 69.63(3) . . ? Cu6 S15 Cu7 69.15(3) . . ? P8 S16 Cu8 92.56(5) . . ? C1 N1 P1 130.7(3) . . ? C1 N2 C2 124.2(4) . . ? C11 N3 P2 132.2(3) . . ? C11 N4 C12 125.0(4) . . ? C21 N5 P3 130.6(3) . . ? C21 N6 C22 124.6(4) . . ? C31 N7 P4 131.6(3) . . ? C31 N8 C32 123.4(3) . . ? C41 N9 P5 131.9(3) . . ? C41 N10 C42 123.6(4) . . ? C51 N11 P6 131.2(3) . . ? C51 N12 C52 124.0(3) . . ? C61 N13 P7 131.6(3) . . ? C61 N14 C62 124.0(4) . . ? C71 N15 P8 131.7(3) . . ? C71 N16 C72 124.1(3) . . ? O2 P1 O1 101.32(17) . . ? O2 P1 N1 105.06(18) . . ? O1 P1 N1 110.46(18) . . ? O2 P1 S2 109.44(14) . . ? O1 P1 S2 108.12(13) . . ? N1 P1 S2 120.69(14) . . ? O3 P2 O4 101.10(17) . . ? O3 P2 N3 112.52(18) . . ? O4 P2 N3 104.50(18) . . ? O3 P2 S4 108.51(13) . . ? O4 P2 S4 110.10(13) . . ? N3 P2 S4 118.61(14) . . ? O5 P3 O6 101.68(17) . . ? O5 P3 N5 111.94(18) . . ? O6 P3 N5 104.06(17) . . ? O5 P3 S6 107.79(13) . . ? O6 P3 S6 109.93(13) . . ? N5 P3 S6 119.87(14) . . ? O7 P4 O8 101.34(17) . . ? O7 P4 N7 112.48(18) . . ? O8 P4 N7 103.63(17) . . ? O7 P4 S8 107.84(12) . . ? O8 P4 S8 110.69(13) . . ? N7 P4 S8 119.32(14) . . ? O9 P5 O10 101.63(17) . . ? O9 P5 N9 112.57(18) . . ? O10 P5 N9 103.71(17) . . ? O9 P5 S10 107.90(12) . . ? O10 P5 S10 110.45(14) . . ? N9 P5 S10 119.12(14) . . ? O11 P6 O12 102.66(17) . . ? O11 P6 N11 110.92(18) . . ? O12 P6 N11 103.99(17) . . ? O11 P6 S12 107.32(12) . . ? O12 P6 S12 109.93(13) . . ? N11 P6 S12 120.56(14) . . ? O14 P7 O13 102.87(17) . . ? O14 P7 N13 110.87(19) . . ? O13 P7 N13 103.96(18) . . ? O14 P7 S14 107.89(13) . . ? O13 P7 S14 109.39(14) . . ? N13 P7 S14 120.42(14) . . ? O16 P8 O15 100.61(17) . . ? O16 P8 N15 112.17(18) . . ? O15 P8 N15 104.86(17) . . ? O16 P8 S16 108.98(13) . . ? O15 P8 S16 110.07(13) . . ? N15 P8 S16 118.56(14) . . ? C5 O1 P1 122.2(3) . . ? C8 O2 P1 126.6(3) . . ? C18 O3 P2 124.1(3) . . ? C15 O4 P2 122.4(3) . . ? C25 O5 P3 123.9(3) . . ? C28 O6 P3 122.6(3) . . ? C35 O7 P4 123.5(3) . . ? C38 O8 P4 121.2(3) . . ? C45 O9 P5 123.6(3) . . ? C48 O10 P5 121.1(3) . . ? C55 O11 P6 123.2(3) . . ? C58 O12 P6 123.9(3) . . ? C65 O13 P7 123.9(3) . . ? C68 O14 P7 123.4(3) . . ? C75 O15 P8 121.3(3) . . ? C78 O16 P8 123.9(3) . . ? N1 C1 N2 118.8(4) . . ? N1 C1 S1 126.3(3) . . ? N2 C1 S1 114.8(3) . . ? N2 C2 C3 108.2(4) . . ? N2 C2 C4 109.5(4) . . ? C3 C2 C4 111.9(4) . . ? O1 C5 C6 106.3(4) . . ? O1 C5 C7 108.9(4) . . ? C6 C5 C7 114.1(5) . . ? O2 C8 C9 119.8(6) . . ? O2 C8 C10 104.2(4) . . ? C9 C8 C10 114.6(7) . . ? N3 C11 N4 118.7(4) . . ? N3 C11 S3 125.6(3) . . ? N4 C11 S3 115.6(3) . . ? C13 C12 N4 109.4(4) . . ? C13 C12 C14 109.8(6) . . ? N4 C12 C14 109.4(5) . . ? O4 C15 C17 109.6(5) . . ? O4 C15 C16 108.9(9) . . ? C17 C15 C16 108.4(6) . . ? O3 C18 C20 106.6(4) . . ? O3 C18 C19 108.0(5) . . ? C20 C18 C19 111.8(6) . . ? N5 C21 N6 118.7(4) . . ? N5 C21 S5 126.0(3) . . ? N6 C21 S5 115.2(3) . . ? N6 C22 C24 110.5(4) . . ? N6 C22 C23 108.1(4) . . ? C24 C22 C23 113.6(5) . . ? O5 C25 C26 106.0(4) . . ? O5 C25 C27 107.9(4) . . ? C26 C25 C27 114.2(5) . . ? C29 C28 C30 113.0(8) . . ? C29 C28 O6 113.2(6) . . ? C30 C28 O6 108.5(5) . . ? N7 C31 N8 118.9(4) . . ? N7 C31 S7 125.2(3) . . ? N8 C31 S7 115.8(3) . . ? N8 C32 C33 110.4(4) . . ? N8 C32 C34 108.0(4) . . ? C33 C32 C34 112.1(4) . . ? O7 C35 C37 107.8(5) . . ? O7 C35 C36 106.8(4) . . ? C37 C35 C36 113.1(5) . . ? C39 C38 C40 110.2(7) . . ? C39 C38 O8 108.6(5) . . ? C40 C38 O8 106.5(5) . . ? N9 C41 N10 117.9(4) . . ? N9 C41 S9 125.9(3) . . ? N10 C41 S9 116.1(3) . . ? C44 C42 N10 110.5(5) . . ? C44 C42 C43 113.8(7) . . ? N10 C42 C43 108.7(4) . . ? O9 C45 C47 106.7(4) . . ? O9 C45 C46 108.2(4) . . ? C47 C45 C46 113.8(5) . . ? C50 C48 O10 111.5(5) . . ? C50 C48 C49 112.3(6) . . ? O10 C48 C49 105.3(5) . . ? N11 C51 N12 118.3(4) . . ? N11 C51 S11 125.9(3) . . ? N12 C51 S11 115.6(3) . . ? N12 C52 C54 111.3(4) . . ? N12 C52 C53 107.6(4) . . ? C54 C52 C53 111.1(4) . . ? O11 C55 C56 106.4(4) . . ? O11 C55 C57 108.5(4) . . ? C56 C55 C57 113.3(4) . . ? C59 C58 C60 108.9(10) . . ? C59 C58 O12 112.4(6) . . ? C60 C58 O12 106.3(6) . . ? N13 C61 N14 118.7(4) . . ? N13 C61 S13 126.0(3) . . ? N14 C61 S13 115.3(3) . . ? N14 C62 C64 109.9(4) . . ? N14 C62 C63 107.6(4) . . ? C64 C62 C63 111.5(4) . . ? O13 C65 C66 116.8(5) . . ? O13 C65 C67 104.3(5) . . ? C66 C65 C67 111.8(6) . . ? O14 C68 C70 110.0(5) . . ? O14 C68 C69 105.5(4) . . ? C70 C68 C69 114.3(5) . . ? N15 C71 N16 118.8(4) . . ? N15 C71 S15 125.6(3) . . ? N16 C71 S15 115.5(3) . . ? N16 C72 C74 108.8(4) . . ? N16 C72 C73 110.7(4) . . ? C74 C72 C73 111.5(4) . . ? O15 C75 C76 107.1(5) . . ? O15 C75 C77 107.1(5) . . ? C76 C75 C77 111.6(5) . . ? O16 C78 C80 112.0(4) . . ? O16 C78 C79 106.3(4) . . ? C80 C78 C79 113.5(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.732 _refine_diff_density_min -1.101 _refine_diff_density_rms 0.106 # Attachment '- [Cu3LIV3].cif' data_safin48 #TrackingRef '- C0CE00337A_ccdc_684171_739994_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 739993' #TrackingRef '- [Cu3LIV3].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H78 Cu3 N6 O6 P3 S6' _chemical_formula_weight 1311.05 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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.1333(4) _cell_length_b 28.4411(9) _cell_length_c 24.4109(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.382(3) _cell_angle_gamma 90.00 _cell_volume 6339.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28861 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 26.3 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 1.317 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7342 _exptl_absorpt_correction_T_max 0.7515 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _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 '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 49505 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.0698 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.94 _reflns_number_total 12302 _reflns_number_gt 8412 _reflns_threshold_expression >2sigma(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 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material ? _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^)+(0.0322P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12302 _refine_ls_number_parameters 669 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0751 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 0.863 _refine_ls_restrained_S_all 0.867 _refine_ls_shift/su_max 0.002 _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 0.91188(4) 0.644622(12) 0.322866(13) 0.03132(9) Uani 1 1 d . . . Cu2 Cu 0.64601(4) 0.580494(12) 0.238287(13) 0.03449(9) Uani 1 1 d . . . Cu3 Cu 0.70060(4) 0.700087(12) 0.204624(13) 0.03440(9) Uani 1 1 d . . . P1 P 1.07996(8) 0.72765(2) 0.37571(3) 0.02711(16) Uani 1 1 d . . . P2 P 0.62113(8) 0.48283(3) 0.28110(3) 0.02760(16) Uani 1 1 d . . . P3 P 0.47968(9) 0.72488(3) 0.11146(3) 0.03155(17) Uani 1 1 d . . . S1 S 0.98768(9) 0.66990(3) 0.40566(3) 0.03569(17) Uani 1 1 d . . . S2 S 0.46737(9) 0.53002(3) 0.26181(3) 0.03688(17) Uani 1 1 d . . . S3 S 0.55089(10) 0.75865(3) 0.17849(3) 0.0460(2) Uani 1 1 d . . . S4 S 0.85486(9) 0.57434(2) 0.28815(3) 0.03231(16) Uani 1 1 d . . . S5 S 0.64379(8) 0.63057(2) 0.16879(3) 0.03158(16) Uani 1 1 d . . . S6 S 0.89858(8) 0.70144(2) 0.25858(3) 0.03174(16) Uani 1 1 d . . . N1 N 0.9835(3) 0.76357(8) 0.33917(9) 0.0303(5) Uani 1 1 d . . . N2 N 0.7292(3) 0.49571(8) 0.33145(8) 0.0287(5) Uani 1 1 d . . . N3 N 0.4077(3) 0.67368(8) 0.11776(9) 0.0312(5) Uani 1 1 d . . . N4 N 0.8428(3) 0.79205(8) 0.26837(10) 0.0374(6) Uani 1 1 d D . . H4 H 0.795(3) 0.7856(11) 0.2364(7) 0.040(9) Uiso 1 1 d D . . N5 N 0.8734(3) 0.53991(8) 0.38888(9) 0.0315(5) Uani 1 1 d D . . H5 H 0.923(3) 0.5674(7) 0.3931(13) 0.052(10) Uiso 1 1 d D . . N6 N 0.3881(3) 0.59554(8) 0.13702(9) 0.0324(5) Uani 1 1 d D . . H6 H 0.428(4) 0.5712(9) 0.1555(12) 0.059(11) Uiso 1 1 d D . . O1 O 1.2189(2) 0.71778(7) 0.34022(7) 0.0338(5) Uani 1 1 d D A . O2 O 1.1324(2) 0.75676(7) 0.42761(7) 0.0320(4) Uani 1 1 d . . . O3 O 0.5501(2) 0.43437(7) 0.29631(7) 0.0333(4) Uani 1 1 d . . . O4 O 0.7162(2) 0.46822(7) 0.23064(7) 0.0326(4) Uani 1 1 d . . . O5 O 0.3602(2) 0.75595(7) 0.08120(7) 0.0353(5) Uani 1 1 d . . . O6 O 0.5976(2) 0.71836(7) 0.06603(8) 0.0392(5) Uani 1 1 d . . . C1 C 0.9121(3) 0.75565(9) 0.29312(10) 0.0286(6) Uani 1 1 d . . . C2 C 0.8113(3) 0.53279(9) 0.33900(10) 0.0276(6) Uani 1 1 d . . . C3 C 0.4652(3) 0.63602(9) 0.13898(10) 0.0280(6) Uani 1 1 d . . . C4 C 1.3260(4) 0.68063(11) 0.35019(13) 0.0430(8) Uani 1 1 d D . . H4A H 1.2712 0.6506 0.3551 0.052 Uiso 0.535(6) 1 calc PR A 1 H4B H 1.3031 0.6653 0.3858 0.052 Uiso 0.465(6) 1 calc PR A 2 C5 C 1.4173(8) 0.6877(3) 0.3981(3) 0.062(2) Uiso 0.535(6) 1 d PD A 1 H5A H 1.3563 0.6891 0.4305 0.094 Uiso 0.535(6) 1 calc PR A 1 H5B H 1.4713 0.7173 0.3946 0.094 Uiso 0.535(6) 1 calc PR A 1 H5C H 1.4867 0.6616 0.4019 0.094 Uiso 0.535(6) 1 calc PR A 1 C6 C 1.4073(8) 0.6772(3) 0.2964(3) 0.065(2) Uiso 0.535(6) 1 d PD A 1 H6A H 1.3367 0.6723 0.2661 0.098 Uiso 0.535(6) 1 calc PR A 1 H6B H 1.4759 0.6507 0.2982 0.098 Uiso 0.535(6) 1 calc PR A 1 H6C H 1.4616 0.7064 0.2904 0.098 Uiso 0.535(6) 1 calc PR A 1 C5' C 1.4767(9) 0.7048(3) 0.3568(4) 0.072(3) Uiso 0.465(6) 1 d PD A 2 H5'1 H 1.4729 0.7284 0.3860 0.109 Uiso 0.465(6) 1 calc PR A 2 H5'2 H 1.5016 0.7202 0.3223 0.109 Uiso 0.465(6) 1 calc PR A 2 H5'3 H 1.5513 0.6812 0.3663 0.109 Uiso 0.465(6) 1 calc PR A 2 C6' C 1.3244(10) 0.6448(3) 0.3083(3) 0.066(3) Uiso 0.465(6) 1 d PD A 2 H6'1 H 1.2271 0.6303 0.3059 0.099 Uiso 0.465(6) 1 calc PR A 2 H6'2 H 1.3977 0.6207 0.3177 0.099 Uiso 0.465(6) 1 calc PR A 2 H6'3 H 1.3475 0.6590 0.2730 0.099 Uiso 0.465(6) 1 calc PR A 2 C7 C 1.1955(3) 0.80434(10) 0.42114(11) 0.0345(7) Uani 1 1 d . . . H7 H 1.2354 0.8076 0.3835 0.041 Uiso 1 1 calc R . . C8 C 1.0782(4) 0.84044(12) 0.42911(13) 0.0477(8) Uani 1 1 d . . . H8A H 1.0008 0.8363 0.4010 0.072 Uiso 1 1 calc R . . H8B H 1.1204 0.8720 0.4260 0.072 Uiso 1 1 calc R . . H8C H 1.0369 0.8366 0.4655 0.072 Uiso 1 1 calc R . . C9 C 1.3189(4) 0.80857(13) 0.46311(13) 0.0507(9) Uani 1 1 d . . . H9A H 1.3923 0.7843 0.4564 0.076 Uiso 1 1 calc R . . H9B H 1.2802 0.8045 0.4999 0.076 Uiso 1 1 calc R . . H9C H 1.3642 0.8397 0.4603 0.076 Uiso 1 1 calc R . . C10 C 0.4650(4) 0.42884(11) 0.34618(11) 0.0389(7) Uani 1 1 d . . . H10 H 0.4443 0.4604 0.3623 0.047 Uiso 1 1 calc R . . C11 C 0.3247(4) 0.40542(17) 0.32950(18) 0.0725(12) Uani 1 1 d . . . H11A H 0.2700 0.4257 0.3039 0.109 Uiso 1 1 calc R . . H11B H 0.2663 0.3998 0.3620 0.109 Uiso 1 1 calc R . . H11C H 0.3459 0.3754 0.3117 0.109 Uiso 1 1 calc R . . C12 C 0.5544(5) 0.40012(15) 0.38625(15) 0.0627(11) Uani 1 1 d . . . H12A H 0.6449 0.4170 0.3960 0.094 Uiso 1 1 calc R . . H12B H 0.5788 0.3698 0.3696 0.094 Uiso 1 1 calc R . . H12C H 0.4981 0.3947 0.4193 0.094 Uiso 1 1 calc R . . C13 C 0.6471(4) 0.45478(13) 0.17799(12) 0.0487(9) Uani 1 1 d . . . H13 H 0.5407 0.4630 0.1782 0.058 Uiso 1 1 calc R . . C14 C 0.6638(5) 0.40262(14) 0.17099(16) 0.0668(12) Uani 1 1 d . . . H14A H 0.6128 0.3863 0.2003 0.100 Uiso 1 1 calc R . . H14B H 0.7680 0.3944 0.1727 0.100 Uiso 1 1 calc R . . H14C H 0.6215 0.3932 0.1354 0.100 Uiso 1 1 calc R . . C15 C 0.7216(5) 0.48338(17) 0.13435(13) 0.0761(13) Uani 1 1 d . . . H15A H 0.7059 0.5169 0.1412 0.114 Uiso 1 1 calc R . . H15B H 0.6802 0.4751 0.0982 0.114 Uiso 1 1 calc R . . H15C H 0.8268 0.4766 0.1354 0.114 Uiso 1 1 calc R . . C16 C 0.2357(4) 0.77842(12) 0.10653(13) 0.0458(8) Uani 1 1 d . . . H16 H 0.2734 0.7986 0.1373 0.055 Uiso 1 1 calc R . . C17 C 0.1696(5) 0.81021(13) 0.06252(15) 0.0593(10) Uani 1 1 d . . . H17A H 0.2441 0.8324 0.0502 0.089 Uiso 1 1 calc R . . H17B H 0.0872 0.8277 0.0775 0.089 Uiso 1 1 calc R . . H17C H 0.1349 0.7911 0.0314 0.089 Uiso 1 1 calc R . . C18 C 0.1311(5) 0.74380(16) 0.12929(18) 0.0707(12) Uani 1 1 d . . . H18A H 0.1812 0.7248 0.1575 0.106 Uiso 1 1 calc R . . H18B H 0.0943 0.7232 0.0999 0.106 Uiso 1 1 calc R . . H18C H 0.0489 0.7606 0.1455 0.106 Uiso 1 1 calc R . . C19 C 0.7206(4) 0.74934(13) 0.05449(15) 0.0548(9) Uani 1 1 d . . . H19 H 0.7741 0.7572 0.0895 0.066 Uiso 1 1 calc R . . C20 C 0.8186(5) 0.72024(17) 0.01875(19) 0.0781(13) Uani 1 1 d . . . H20A H 0.8513 0.6922 0.0389 0.117 Uiso 1 1 calc R . . H20B H 0.9039 0.7389 0.0087 0.117 Uiso 1 1 calc R . . H20C H 0.7640 0.7107 -0.0145 0.117 Uiso 1 1 calc R . . C21 C 0.6693(6) 0.79328(17) 0.0277(2) 0.1036(19) Uani 1 1 d . . . H21A H 0.6066 0.8106 0.0526 0.155 Uiso 1 1 calc R . . H21B H 0.6135 0.7856 -0.0059 0.155 Uiso 1 1 calc R . . H21C H 0.7540 0.8127 0.0185 0.155 Uiso 1 1 calc R . . C41 C 0.8449(4) 0.83924(10) 0.28920(12) 0.0373(7) Uani 1 1 d . . . C42 C 0.7476(4) 0.85153(12) 0.32956(14) 0.0483(8) Uani 1 1 d . . . C43 C 0.7485(5) 0.89836(15) 0.34695(16) 0.0614(11) Uani 1 1 d . . . H43 H 0.6826 0.9076 0.3744 0.074 Uiso 1 1 calc R . . C44 C 0.8413(5) 0.93159(12) 0.32583(18) 0.0638(12) Uani 1 1 d . . . C45 C 0.9366(5) 0.91757(13) 0.28639(16) 0.0589(10) Uani 1 1 d . . . H45 H 1.0009 0.9402 0.2714 0.071 Uiso 1 1 calc R . . C46 C 0.9427(4) 0.87143(11) 0.26745(13) 0.0455(8) Uani 1 1 d . . . C47 C 0.6459(5) 0.81524(16) 0.35320(18) 0.0731(12) Uani 1 1 d . . . H47A H 0.5754 0.8049 0.3248 0.110 Uiso 1 1 calc R . . H47B H 0.5933 0.8291 0.3838 0.110 Uiso 1 1 calc R . . H47C H 0.7031 0.7882 0.3664 0.110 Uiso 1 1 calc R . . C48 C 0.8337(6) 0.98211(15) 0.3443(2) 0.103(2) Uani 1 1 d . . . H48A H 0.8628 0.9842 0.3832 0.154 Uiso 1 1 calc R . . H48B H 0.7332 0.9937 0.3393 0.154 Uiso 1 1 calc R . . H48C H 0.9000 1.0012 0.3226 0.154 Uiso 1 1 calc R . . C49 C 1.0493(5) 0.85695(15) 0.22463(16) 0.0690(11) Uani 1 1 d . . . H49A H 0.9955 0.8479 0.1910 0.104 Uiso 1 1 calc R . . H49B H 1.1073 0.8302 0.2381 0.104 Uiso 1 1 calc R . . H49C H 1.1146 0.8833 0.2168 0.104 Uiso 1 1 calc R . . C51 C 0.8317(3) 0.51363(10) 0.43680(10) 0.0310(6) Uani 1 1 d . . . C52 C 0.7364(4) 0.53524(11) 0.47251(12) 0.0432(8) Uani 1 1 d . . . C53 C 0.6975(4) 0.51028(13) 0.51906(13) 0.0529(9) Uani 1 1 d . . . H53 H 0.6297 0.5240 0.5432 0.063 Uiso 1 1 calc R . . C54 C 0.7535(4) 0.46647(12) 0.53143(13) 0.0493(9) Uani 1 1 d . . . C55 C 0.8467(4) 0.44592(11) 0.49474(12) 0.0403(7) Uani 1 1 d . . . H55 H 0.8839 0.4153 0.5020 0.048 Uiso 1 1 calc R . . C56 C 0.8877(3) 0.46928(11) 0.44701(11) 0.0356(7) Uani 1 1 d . . . C57 C 0.6772(5) 0.58379(13) 0.46070(17) 0.0677(12) Uani 1 1 d . . . H57A H 0.7539 0.6072 0.4683 0.102 Uiso 1 1 calc R . . H57B H 0.5934 0.5899 0.4840 0.102 Uiso 1 1 calc R . . H57C H 0.6459 0.5858 0.4221 0.102 Uiso 1 1 calc R . . C58 C 0.7163(5) 0.44160(16) 0.58418(16) 0.0750(13) Uani 1 1 d . . . H58A H 0.7357 0.4079 0.5805 0.112 Uiso 1 1 calc R . . H58B H 0.6125 0.4464 0.5918 0.112 Uiso 1 1 calc R . . H58C H 0.7766 0.4544 0.6144 0.112 Uiso 1 1 calc R . . C59 C 0.9895(4) 0.44544(12) 0.40738(13) 0.0509(9) Uani 1 1 d . . . H59A H 0.9324 0.4336 0.3758 0.076 Uiso 1 1 calc R . . H59B H 1.0395 0.4192 0.4259 0.076 Uiso 1 1 calc R . . H59C H 1.0622 0.4682 0.3949 0.076 Uiso 1 1 calc R . . C61 C 0.2564(3) 0.58937(9) 0.10419(10) 0.0287(6) Uani 1 1 d . . . C62 C 0.1211(4) 0.59954(11) 0.12648(12) 0.0394(7) Uani 1 1 d . . . C63 C -0.0043(4) 0.59215(11) 0.09287(15) 0.0466(8) Uani 1 1 d . . . H63 H -0.0977 0.5994 0.1070 0.056 Uiso 1 1 calc R . . C64 C 0.0032(4) 0.57474(11) 0.03995(13) 0.0432(8) Uani 1 1 d . . . C65 C 0.1394(4) 0.56490(11) 0.02031(12) 0.0404(7) Uani 1 1 d . . . H65 H 0.1466 0.5526 -0.0157 0.048 Uiso 1 1 calc R . . C66 C 0.2675(3) 0.57227(10) 0.05126(11) 0.0328(6) Uani 1 1 d . . . C67 C 0.1089(5) 0.61659(14) 0.18449(14) 0.0585(10) Uani 1 1 d . . . H67A H 0.1411 0.5917 0.2098 0.088 Uiso 1 1 calc R . . H67B H 0.0068 0.6248 0.1915 0.088 Uiso 1 1 calc R . . H67C H 0.1708 0.6444 0.1900 0.088 Uiso 1 1 calc R . . C68 C -0.1347(4) 0.56799(15) 0.00576(17) 0.0673(11) Uani 1 1 d . . . H68A H -0.1463 0.5943 -0.0199 0.101 Uiso 1 1 calc R . . H68B H -0.2192 0.5668 0.0297 0.101 Uiso 1 1 calc R . . H68C H -0.1284 0.5385 -0.0148 0.101 Uiso 1 1 calc R . . C69 C 0.4157(4) 0.56195(14) 0.02781(13) 0.0540(10) Uani 1 1 d . . . H69A H 0.4759 0.5905 0.0291 0.081 Uiso 1 1 calc R . . H69B H 0.4032 0.5516 -0.0103 0.081 Uiso 1 1 calc R . . H69C H 0.4641 0.5371 0.0494 0.081 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 0.0367(2) 0.02181(18) 0.03532(17) -0.00080(13) -0.00122(15) -0.00377(15) Cu2 0.0465(2) 0.02635(19) 0.03034(17) 0.00090(14) -0.00374(15) 0.00560(17) Cu3 0.0439(2) 0.0282(2) 0.03060(17) -0.00074(14) -0.00958(15) -0.00254(16) P1 0.0328(4) 0.0218(4) 0.0265(3) -0.0007(3) -0.0028(3) -0.0007(3) P2 0.0310(4) 0.0247(4) 0.0269(3) -0.0034(3) -0.0031(3) -0.0009(3) P3 0.0371(4) 0.0238(4) 0.0333(4) 0.0042(3) -0.0079(3) -0.0018(3) S1 0.0489(5) 0.0279(4) 0.0303(3) 0.0013(3) 0.0009(3) -0.0086(3) S2 0.0340(4) 0.0373(4) 0.0393(4) 0.0024(3) -0.0005(3) 0.0060(3) S3 0.0607(6) 0.0278(4) 0.0482(4) -0.0068(3) -0.0223(4) 0.0040(4) S4 0.0450(5) 0.0229(4) 0.0288(3) 0.0015(3) -0.0044(3) -0.0062(3) S5 0.0372(4) 0.0250(4) 0.0321(3) 0.0016(3) -0.0062(3) -0.0001(3) S6 0.0411(4) 0.0213(4) 0.0324(3) -0.0021(3) -0.0079(3) -0.0005(3) N1 0.0359(14) 0.0200(12) 0.0346(12) 0.0004(9) -0.0084(10) 0.0000(10) N2 0.0370(14) 0.0213(12) 0.0275(11) -0.0014(9) -0.0053(10) -0.0026(10) N3 0.0380(14) 0.0244(13) 0.0308(11) 0.0024(9) -0.0046(10) -0.0028(11) N4 0.0466(16) 0.0209(13) 0.0437(14) -0.0025(10) -0.0205(12) 0.0006(11) N5 0.0402(15) 0.0244(13) 0.0294(11) -0.0011(9) -0.0076(10) -0.0110(11) N6 0.0399(15) 0.0218(13) 0.0352(12) 0.0049(10) -0.0076(11) -0.0025(11) O1 0.0364(12) 0.0284(11) 0.0366(10) 0.0050(8) 0.0031(9) 0.0029(9) O2 0.0428(12) 0.0253(11) 0.0276(9) 0.0000(7) -0.0061(8) -0.0050(9) O3 0.0358(12) 0.0289(11) 0.0351(10) -0.0038(8) -0.0005(8) -0.0069(9) O4 0.0317(12) 0.0385(12) 0.0273(9) -0.0083(8) -0.0035(8) 0.0012(9) O5 0.0399(12) 0.0274(11) 0.0383(10) 0.0055(8) -0.0077(9) 0.0023(9) O6 0.0383(13) 0.0360(12) 0.0434(11) 0.0050(9) 0.0014(9) -0.0059(10) C1 0.0316(16) 0.0206(14) 0.0336(14) -0.0009(10) -0.0024(12) -0.0020(12) C2 0.0328(16) 0.0219(14) 0.0279(13) -0.0009(10) -0.0044(11) 0.0021(12) C3 0.0369(17) 0.0258(15) 0.0214(12) -0.0007(10) -0.0006(11) 0.0006(12) C4 0.043(2) 0.0314(17) 0.0552(19) 0.0022(14) 0.0102(15) 0.0086(15) C7 0.0470(19) 0.0269(16) 0.0296(13) -0.0015(11) -0.0013(13) -0.0108(14) C8 0.055(2) 0.0319(19) 0.0555(19) -0.0099(14) -0.0068(16) -0.0002(16) C9 0.053(2) 0.043(2) 0.0542(19) -0.0051(15) -0.0197(16) -0.0119(17) C10 0.0431(19) 0.0344(18) 0.0394(15) -0.0035(13) 0.0051(14) -0.0039(14) C11 0.036(2) 0.099(4) 0.082(3) 0.016(2) 0.002(2) -0.015(2) C12 0.065(3) 0.065(3) 0.057(2) 0.0197(18) -0.0090(19) -0.011(2) C13 0.041(2) 0.066(2) 0.0391(16) -0.0245(16) -0.0092(14) 0.0075(17) C14 0.058(3) 0.067(3) 0.074(2) -0.041(2) -0.003(2) -0.006(2) C15 0.106(4) 0.091(3) 0.0307(17) -0.0033(18) 0.000(2) 0.015(3) C16 0.046(2) 0.041(2) 0.0500(18) 0.0027(14) -0.0051(15) 0.0097(16) C17 0.066(3) 0.047(2) 0.063(2) 0.0037(17) -0.0187(19) 0.0194(19) C18 0.050(3) 0.067(3) 0.095(3) 0.024(2) 0.007(2) 0.008(2) C19 0.053(2) 0.051(2) 0.061(2) 0.0032(17) 0.0056(17) -0.0188(18) C20 0.062(3) 0.080(3) 0.093(3) -0.008(2) 0.023(2) -0.011(2) C21 0.096(4) 0.062(3) 0.155(5) 0.048(3) 0.038(4) -0.002(3) C41 0.0435(19) 0.0192(15) 0.0484(16) -0.0019(12) -0.0184(14) 0.0054(13) C42 0.041(2) 0.041(2) 0.062(2) -0.0013(16) -0.0120(16) 0.0092(16) C43 0.054(2) 0.059(3) 0.070(2) -0.0212(19) -0.0181(19) 0.029(2) C44 0.071(3) 0.0257(19) 0.093(3) -0.0164(18) -0.052(2) 0.0159(19) C45 0.065(3) 0.0299(19) 0.079(2) 0.0030(17) -0.037(2) -0.0040(18) C46 0.053(2) 0.0278(17) 0.0551(18) 0.0049(14) -0.0183(16) -0.0044(15) C47 0.053(3) 0.070(3) 0.097(3) 0.005(2) 0.012(2) 0.011(2) C48 0.120(4) 0.036(2) 0.147(4) -0.037(3) -0.083(3) 0.029(3) C49 0.079(3) 0.063(3) 0.066(2) 0.014(2) 0.005(2) -0.012(2) C51 0.0384(17) 0.0276(16) 0.0264(13) 0.0027(11) -0.0099(12) -0.0072(13) C52 0.052(2) 0.0350(18) 0.0423(16) 0.0043(13) 0.0060(15) 0.0008(16) C53 0.065(3) 0.049(2) 0.0452(18) 0.0074(15) 0.0182(17) 0.0022(19) C54 0.066(2) 0.042(2) 0.0397(16) 0.0094(14) 0.0007(16) -0.0091(18) C55 0.052(2) 0.0261(17) 0.0421(16) 0.0059(12) -0.0144(14) -0.0057(14) C56 0.0425(19) 0.0306(17) 0.0334(14) -0.0034(12) -0.0079(13) -0.0055(13) C57 0.089(3) 0.043(2) 0.073(2) 0.0158(18) 0.030(2) 0.019(2) C58 0.099(4) 0.066(3) 0.060(2) 0.025(2) 0.015(2) -0.007(3) C59 0.063(2) 0.036(2) 0.0528(19) 0.0007(15) -0.0033(17) 0.0096(17) C61 0.0293(16) 0.0228(15) 0.0339(14) 0.0039(11) -0.0030(12) -0.0021(12) C62 0.047(2) 0.0246(16) 0.0474(17) 0.0004(12) 0.0110(15) -0.0028(14) C63 0.0284(18) 0.0317(18) 0.080(2) 0.0069(16) 0.0121(17) -0.0007(14) C64 0.044(2) 0.0277(17) 0.0569(19) 0.0071(14) -0.0110(15) -0.0071(15) C65 0.054(2) 0.0304(17) 0.0360(15) 0.0019(12) -0.0084(14) -0.0005(15) C66 0.0386(18) 0.0263(16) 0.0334(14) 0.0013(11) -0.0022(12) 0.0019(13) C67 0.069(3) 0.055(2) 0.052(2) -0.0109(17) 0.0234(19) -0.006(2) C68 0.052(2) 0.055(3) 0.094(3) 0.016(2) -0.029(2) -0.0138(19) C69 0.047(2) 0.073(3) 0.0416(17) -0.0061(16) 0.0060(15) 0.0175(19) _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 S4 2.2280(8) . ? Cu1 S1 2.2391(8) . ? Cu1 S6 2.2538(8) . ? Cu2 S5 2.2148(8) . ? Cu2 S4 2.2447(9) . ? Cu2 S2 2.2577(9) . ? Cu3 S6 2.2116(8) . ? Cu3 S5 2.2185(8) . ? Cu3 S3 2.2380(9) . ? P1 O2 1.5781(19) . ? P1 O1 1.579(2) . ? P1 N1 1.605(2) . ? P1 S1 1.9931(10) . ? P2 O3 1.572(2) . ? P2 O4 1.5793(19) . ? P2 N2 1.600(2) . ? P2 S2 1.9910(11) . ? P3 O5 1.574(2) . ? P3 O6 1.575(2) . ? P3 N3 1.607(2) . ? P3 S3 1.9931(11) . ? S4 C2 1.766(3) . ? S5 C3 1.776(3) . ? S6 C1 1.760(3) . ? N1 C1 1.306(3) . ? N2 C2 1.305(4) . ? N3 C3 1.296(3) . ? N4 C1 1.348(4) . ? N4 C41 1.435(4) . ? N4 H4 0.904(10) . ? N5 C2 1.346(3) . ? N5 C51 1.447(3) . ? N5 H5 0.908(10) . ? N6 C3 1.350(4) . ? N6 C61 1.440(4) . ? N6 H6 0.900(10) . ? O1 C4 1.456(4) . ? O2 C7 1.481(3) . ? O3 C10 1.468(3) . ? O4 C13 1.469(3) . ? O5 C16 1.456(4) . ? O6 C19 1.460(4) . ? C4 C5 1.434(7) . ? C4 C6' 1.443(7) . ? C4 C6 1.527(6) . ? C4 C5' 1.544(8) . ? C4 H4A 1.0000 . ? C4 H4B 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C5' H5'1 0.9800 . ? C5' H5'2 0.9800 . ? C5' H5'3 0.9800 . ? C6' H6'1 0.9800 . ? C6' H6'2 0.9800 . ? C6' H6'3 0.9800 . ? C7 C8 1.500(5) . ? C7 C9 1.509(4) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.492(5) . ? C10 C12 1.501(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.501(5) . ? C13 C15 1.515(5) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.489(5) . ? C16 C17 1.518(4) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C21 1.482(6) . ? C19 C20 1.511(5) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C41 C42 1.387(5) . ? C41 C46 1.393(5) . ? C42 C43 1.398(5) . ? C42 C47 1.512(5) . ? C43 C44 1.377(6) . ? C43 H43 0.9500 . ? C44 C45 1.373(6) . ? C44 C48 1.508(5) . ? C45 C46 1.393(5) . ? C45 H45 0.9500 . ? C46 C49 1.503(5) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C51 C56 1.381(4) . ? C51 C52 1.390(4) . ? C52 C53 1.393(4) . ? C52 C57 1.508(5) . ? C53 C54 1.378(5) . ? C53 H53 0.9500 . ? C54 C55 1.381(5) . ? C54 C58 1.515(4) . ? C55 C56 1.400(4) . ? C55 H55 0.9500 . ? C56 C59 1.518(4) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C61 C66 1.387(4) . ? C61 C62 1.392(4) . ? C62 C63 1.409(5) . ? C62 C67 1.503(4) . ? C63 C64 1.387(5) . ? C63 H63 0.9500 . ? C64 C65 1.373(5) . ? C64 C68 1.506(5) . ? C65 C66 1.393(4) . ? C65 H65 0.9500 . ? C66 C69 1.511(4) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 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 S4 Cu1 S1 134.09(3) . . ? S4 Cu1 S6 111.73(3) . . ? S1 Cu1 S6 114.12(3) . . ? S5 Cu2 S4 117.23(3) . . ? S5 Cu2 S2 127.61(3) . . ? S4 Cu2 S2 114.99(3) . . ? S6 Cu3 S5 115.49(3) . . ? S6 Cu3 S3 129.94(3) . . ? S5 Cu3 S3 114.54(3) . . ? O2 P1 O1 107.52(11) . . ? O2 P1 N1 105.32(11) . . ? O1 P1 N1 104.22(11) . . ? O2 P1 S1 105.11(8) . . ? O1 P1 S1 114.03(8) . . ? N1 P1 S1 119.81(10) . . ? O3 P2 O4 101.04(10) . . ? O3 P2 N2 105.65(11) . . ? O4 P2 N2 108.59(12) . . ? O3 P2 S2 110.74(9) . . ? O4 P2 S2 112.99(8) . . ? N2 P2 S2 116.48(9) . . ? O5 P3 O6 102.34(11) . . ? O5 P3 N3 105.84(12) . . ? O6 P3 N3 104.43(12) . . ? O5 P3 S3 108.87(9) . . ? O6 P3 S3 114.80(9) . . ? N3 P3 S3 118.98(9) . . ? P1 S1 Cu1 93.31(3) . . ? P2 S2 Cu2 88.79(4) . . ? P3 S3 Cu3 93.46(4) . . ? C2 S4 Cu1 112.80(9) . . ? C2 S4 Cu2 103.33(10) . . ? Cu1 S4 Cu2 108.91(3) . . ? C3 S5 Cu2 111.18(9) . . ? C3 S5 Cu3 106.71(9) . . ? Cu2 S5 Cu3 105.86(3) . . ? C1 S6 Cu3 110.32(10) . . ? C1 S6 Cu1 107.01(9) . . ? Cu3 S6 Cu1 115.58(3) . . ? C1 N1 P1 128.7(2) . . ? C2 N2 P2 129.45(19) . . ? C3 N3 P3 128.6(2) . . ? C1 N4 C41 123.9(2) . . ? C1 N4 H4 116(2) . . ? C41 N4 H4 120(2) . . ? C2 N5 C51 122.7(2) . . ? C2 N5 H5 115(2) . . ? C51 N5 H5 120(2) . . ? C3 N6 C61 123.5(2) . . ? C3 N6 H6 116(2) . . ? C61 N6 H6 121(2) . . ? C4 O1 P1 125.65(17) . . ? C7 O2 P1 120.35(15) . . ? C10 O3 P2 121.31(17) . . ? C13 O4 P2 121.24(19) . . ? C16 O5 P3 125.95(17) . . ? C19 O6 P3 127.4(2) . . ? N1 C1 N4 118.2(2) . . ? N1 C1 S6 126.2(2) . . ? N4 C1 S6 115.5(2) . . ? N2 C2 N5 118.5(2) . . ? N2 C2 S4 125.4(2) . . ? N5 C2 S4 116.0(2) . . ? N3 C3 N6 119.0(3) . . ? N3 C3 S5 126.6(2) . . ? N6 C3 S5 114.4(2) . . ? C5 C4 C6' 132.2(5) . . ? C5 C4 O1 114.2(4) . . ? C6' C4 O1 113.5(4) . . ? C5 C4 C6 115.1(5) . . ? C6' C4 C6 49.0(4) . . ? O1 C4 C6 104.0(4) . . ? C5 C4 C5' 49.7(4) . . ? C6' C4 C5' 112.5(5) . . ? O1 C4 C5' 106.7(4) . . ? C6 C4 C5' 70.5(5) . . ? C5 C4 H4A 107.7 . . ? C6' C4 H4A 59.0 . . ? O1 C4 H4A 107.7 . . ? C6 C4 H4A 107.7 . . ? C5' C4 H4A 144.7 . . ? C5 C4 H4B 58.8 . . ? C6' C4 H4B 108.0 . . ? O1 C4 H4B 108.0 . . ? C6 C4 H4B 146.8 . . ? C5' C4 H4B 108.0 . . ? H4A C4 H4B 53.5 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C5' H5'1 109.5 . . ? C4 C5' H5'2 109.5 . . ? H5'1 C5' H5'2 109.5 . . ? C4 C5' H5'3 109.5 . . ? H5'1 C5' H5'3 109.5 . . ? H5'2 C5' H5'3 109.5 . . ? C4 C6' H6'1 109.5 . . ? C4 C6' H6'2 109.5 . . ? H6'1 C6' H6'2 109.5 . . ? C4 C6' H6'3 109.5 . . ? H6'1 C6' H6'3 109.5 . . ? H6'2 C6' H6'3 109.5 . . ? O2 C7 C8 109.3(2) . . ? O2 C7 C9 106.6(2) . . ? C8 C7 C9 112.4(3) . . ? O2 C7 H7 109.5 . . ? C8 C7 H7 109.5 . . ? C9 C7 H7 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O3 C10 C11 106.8(3) . . ? O3 C10 C12 107.9(3) . . ? C11 C10 C12 112.6(3) . . ? O3 C10 H10 109.8 . . ? C11 C10 H10 109.8 . . ? C12 C10 H10 109.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O4 C13 C14 108.3(3) . . ? O4 C13 C15 106.6(3) . . ? C14 C13 C15 113.7(3) . . ? O4 C13 H13 109.4 . . ? C14 C13 H13 109.4 . . ? C15 C13 H13 109.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O5 C16 C18 112.5(3) . . ? O5 C16 C17 105.2(3) . . ? C18 C16 C17 114.2(3) . . ? O5 C16 H16 108.2 . . ? C18 C16 H16 108.2 . . ? C17 C16 H16 108.2 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O6 C19 C21 111.0(3) . . ? O6 C19 C20 104.5(3) . . ? C21 C19 C20 113.1(4) . . ? O6 C19 H19 109.4 . . ? C21 C19 H19 109.4 . . ? C20 C19 H19 109.4 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C42 C41 C46 122.2(3) . . ? C42 C41 N4 118.9(3) . . ? C46 C41 N4 118.9(3) . . ? C41 C42 C43 117.1(3) . . ? C41 C42 C47 120.6(3) . . ? C43 C42 C47 122.3(4) . . ? C44 C43 C42 122.6(4) . . ? C44 C43 H43 118.7 . . ? C42 C43 H43 118.7 . . ? C45 C44 C43 118.0(3) . . ? C45 C44 C48 121.4(5) . . ? C43 C44 C48 120.5(5) . . ? C44 C45 C46 122.5(4) . . ? C44 C45 H45 118.8 . . ? C46 C45 H45 118.8 . . ? C45 C46 C41 117.5(3) . . ? C45 C46 C49 121.4(3) . . ? C41 C46 C49 121.1(3) . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C56 C51 C52 121.7(3) . . ? C56 C51 N5 120.9(3) . . ? C52 C51 N5 117.4(3) . . ? C51 C52 C53 117.5(3) . . ? C51 C52 C57 120.8(3) . . ? C53 C52 C57 121.7(3) . . ? C54 C53 C52 122.6(3) . . ? C54 C53 H53 118.7 . . ? C52 C53 H53 118.7 . . ? C53 C54 C55 118.2(3) . . ? C53 C54 C58 121.3(3) . . ? C55 C54 C58 120.5(3) . . ? C54 C55 C56 121.4(3) . . ? C54 C55 H55 119.3 . . ? C56 C55 H55 119.3 . . ? C51 C56 C55 118.6(3) . . ? C51 C56 C59 121.5(3) . . ? C55 C56 C59 119.9(3) . . ? C52 C57 H57A 109.5 . . ? C52 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C52 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C54 C58 H58A 109.5 . . ? C54 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C54 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C56 C59 H59A 109.5 . . ? C56 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C56 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C66 C61 C62 121.5(3) . . ? C66 C61 N6 118.8(2) . . ? C62 C61 N6 119.6(2) . . ? C61 C62 C63 117.3(3) . . ? C61 C62 C67 121.4(3) . . ? C63 C62 C67 121.3(3) . . ? C64 C63 C62 122.6(3) . . ? C64 C63 H63 118.7 . . ? C62 C63 H63 118.7 . . ? C65 C64 C63 117.6(3) . . ? C65 C64 C68 122.2(3) . . ? C63 C64 C68 120.2(3) . . ? C64 C65 C66 122.4(3) . . ? C64 C65 H65 118.8 . . ? C66 C65 H65 118.8 . . ? C61 C66 C65 118.6(3) . . ? C61 C66 C69 120.5(3) . . ? C65 C66 C69 120.9(3) . . ? C62 C67 H67A 109.5 . . ? C62 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C62 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C64 C68 H68A 109.5 . . ? C64 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C64 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C66 C69 H69A 109.5 . . ? C66 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C66 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 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 Cu1 174.43(8) . . . . ? O1 P1 S1 Cu1 -68.06(9) . . . . ? N1 P1 S1 Cu1 56.38(10) . . . . ? S4 Cu1 S1 P1 156.32(4) . . . . ? S6 Cu1 S1 P1 -20.45(5) . . . . ? O3 P2 S2 Cu2 -174.19(8) . . . . ? O4 P2 S2 Cu2 -61.66(9) . . . . ? N2 P2 S2 Cu2 65.08(10) . . . . ? S5 Cu2 S2 P2 141.64(4) . . . . ? S4 Cu2 S2 P2 -33.32(4) . . . . ? O5 P3 S3 Cu3 177.74(9) . . . . ? O6 P3 S3 Cu3 -68.26(10) . . . . ? N3 P3 S3 Cu3 56.48(12) . . . . ? S6 Cu3 S3 P3 157.01(4) . . . . ? S5 Cu3 S3 P3 -21.12(5) . . . . ? S1 Cu1 S4 C2 20.74(12) . . . . ? S6 Cu1 S4 C2 -162.43(11) . . . . ? S1 Cu1 S4 Cu2 134.84(4) . . . . ? S6 Cu1 S4 Cu2 -48.33(4) . . . . ? S5 Cu2 S4 C2 178.91(9) . . . . ? S2 Cu2 S4 C2 -5.58(10) . . . . ? S5 Cu2 S4 Cu1 58.78(4) . . . . ? S2 Cu2 S4 Cu1 -125.71(3) . . . . ? S4 Cu2 S5 C3 -173.21(9) . . . . ? S2 Cu2 S5 C3 11.93(10) . . . . ? S4 Cu2 S5 Cu3 -57.71(4) . . . . ? S2 Cu2 S5 Cu3 127.43(4) . . . . ? S6 Cu3 S5 C3 168.79(9) . . . . ? S3 Cu3 S5 C3 -12.80(9) . . . . ? S6 Cu3 S5 Cu2 50.28(4) . . . . ? S3 Cu3 S5 Cu2 -131.31(4) . . . . ? S5 Cu3 S6 C1 -169.80(10) . . . . ? S3 Cu3 S6 C1 12.08(11) . . . . ? S5 Cu3 S6 Cu1 -48.25(4) . . . . ? S3 Cu3 S6 Cu1 133.63(4) . . . . ? S4 Cu1 S6 C1 169.29(10) . . . . ? S1 Cu1 S6 C1 -13.21(11) . . . . ? S4 Cu1 S6 Cu3 45.98(4) . . . . ? S1 Cu1 S6 Cu3 -136.51(4) . . . . ? O2 P1 N1 C1 -177.4(2) . . . . ? O1 P1 N1 C1 69.5(3) . . . . ? S1 P1 N1 C1 -59.5(3) . . . . ? O3 P2 N2 C2 -178.5(2) . . . . ? O4 P2 N2 C2 73.8(3) . . . . ? S2 P2 N2 C2 -55.1(3) . . . . ? O5 P3 N3 C3 178.4(2) . . . . ? O6 P3 N3 C3 70.8(2) . . . . ? S3 P3 N3 C3 -58.9(3) . . . . ? O2 P1 O1 C4 81.2(2) . . . . ? N1 P1 O1 C4 -167.4(2) . . . . ? S1 P1 O1 C4 -34.9(3) . . . . ? O1 P1 O2 C7 63.4(2) . . . . ? N1 P1 O2 C7 -47.3(2) . . . . ? S1 P1 O2 C7 -174.72(19) . . . . ? O4 P2 O3 C10 172.1(2) . . . . ? N2 P2 O3 C10 59.0(2) . . . . ? S2 P2 O3 C10 -67.9(2) . . . . ? O3 P2 O4 C13 69.7(2) . . . . ? N2 P2 O4 C13 -179.5(2) . . . . ? S2 P2 O4 C13 -48.7(2) . . . . ? O6 P3 O5 C16 -170.4(2) . . . . ? N3 P3 O5 C16 80.5(3) . . . . ? S3 P3 O5 C16 -48.5(3) . . . . ? O5 P3 O6 C19 87.7(3) . . . . ? N3 P3 O6 C19 -162.1(3) . . . . ? S3 P3 O6 C19 -30.1(3) . . . . ? P1 N1 C1 N4 -177.3(2) . . . . ? P1 N1 C1 S6 1.6(4) . . . . ? C41 N4 C1 N1 1.0(4) . . . . ? C41 N4 C1 S6 -178.0(2) . . . . ? Cu3 S6 C1 N1 156.8(2) . . . . ? Cu1 S6 C1 N1 30.3(3) . . . . ? Cu3 S6 C1 N4 -24.3(2) . . . . ? Cu1 S6 C1 N4 -150.8(2) . . . . ? P2 N2 C2 N5 168.3(2) . . . . ? P2 N2 C2 S4 -14.1(4) . . . . ? C51 N5 C2 N2 -12.0(4) . . . . ? C51 N5 C2 S4 170.2(2) . . . . ? Cu1 S4 C2 N2 155.4(2) . . . . ? Cu2 S4 C2 N2 37.9(3) . . . . ? Cu1 S4 C2 N5 -27.0(2) . . . . ? Cu2 S4 C2 N5 -144.4(2) . . . . ? P3 N3 C3 N6 -175.82(19) . . . . ? P3 N3 C3 S5 1.1(4) . . . . ? C61 N6 C3 N3 11.6(4) . . . . ? C61 N6 C3 S5 -165.6(2) . . . . ? Cu2 S5 C3 N3 145.7(2) . . . . ? Cu3 S5 C3 N3 30.7(2) . . . . ? Cu2 S5 C3 N6 -37.3(2) . . . . ? Cu3 S5 C3 N6 -152.28(17) . . . . ? P1 O1 C4 C5 -70.2(4) . . . . ? P1 O1 C4 C6' 112.7(4) . . . . ? P1 O1 C4 C6 163.6(4) . . . . ? P1 O1 C4 C5' -122.9(4) . . . . ? P1 O2 C7 C8 96.5(2) . . . . ? P1 O2 C7 C9 -141.8(2) . . . . ? P2 O3 C10 C11 130.7(3) . . . . ? P2 O3 C10 C12 -107.9(3) . . . . ? P2 O4 C13 C14 -107.6(3) . . . . ? P2 O4 C13 C15 129.7(3) . . . . ? P3 O5 C16 C18 -64.0(4) . . . . ? P3 O5 C16 C17 171.0(2) . . . . ? P3 O6 C19 C21 -72.8(4) . . . . ? P3 O6 C19 C20 165.0(3) . . . . ? C1 N4 C41 C42 -82.7(4) . . . . ? C1 N4 C41 C46 98.6(4) . . . . ? C46 C41 C42 C43 1.6(5) . . . . ? N4 C41 C42 C43 -177.1(3) . . . . ? C46 C41 C42 C47 -178.4(3) . . . . ? N4 C41 C42 C47 2.9(5) . . . . ? C41 C42 C43 C44 -0.3(5) . . . . ? C47 C42 C43 C44 179.7(4) . . . . ? C42 C43 C44 C45 -0.4(6) . . . . ? C42 C43 C44 C48 177.5(4) . . . . ? C43 C44 C45 C46 -0.2(5) . . . . ? C48 C44 C45 C46 -178.1(3) . . . . ? C44 C45 C46 C41 1.4(5) . . . . ? C44 C45 C46 C49 -179.4(4) . . . . ? C42 C41 C46 C45 -2.1(5) . . . . ? N4 C41 C46 C45 176.6(3) . . . . ? C42 C41 C46 C49 178.6(3) . . . . ? N4 C41 C46 C49 -2.6(5) . . . . ? C2 N5 C51 C56 81.5(4) . . . . ? C2 N5 C51 C52 -99.9(3) . . . . ? C56 C51 C52 C53 -0.7(5) . . . . ? N5 C51 C52 C53 -179.2(3) . . . . ? C56 C51 C52 C57 179.7(3) . . . . ? N5 C51 C52 C57 1.2(5) . . . . ? C51 C52 C53 C54 2.3(6) . . . . ? C57 C52 C53 C54 -178.1(4) . . . . ? C52 C53 C54 C55 -2.9(6) . . . . ? C52 C53 C54 C58 176.1(4) . . . . ? C53 C54 C55 C56 2.0(5) . . . . ? C58 C54 C55 C56 -177.0(3) . . . . ? C52 C51 C56 C55 -0.2(5) . . . . ? N5 C51 C56 C55 178.3(3) . . . . ? C52 C51 C56 C59 178.8(3) . . . . ? N5 C51 C56 C59 -2.7(4) . . . . ? C54 C55 C56 C51 -0.5(5) . . . . ? C54 C55 C56 C59 -179.5(3) . . . . ? C3 N6 C61 C66 91.2(3) . . . . ? C3 N6 C61 C62 -90.3(3) . . . . ? C66 C61 C62 C63 -0.5(4) . . . . ? N6 C61 C62 C63 -179.0(3) . . . . ? C66 C61 C62 C67 178.0(3) . . . . ? N6 C61 C62 C67 -0.4(4) . . . . ? C61 C62 C63 C64 1.1(5) . . . . ? C67 C62 C63 C64 -177.5(3) . . . . ? C62 C63 C64 C65 -0.5(5) . . . . ? C62 C63 C64 C68 -179.4(3) . . . . ? C63 C64 C65 C66 -0.7(5) . . . . ? C68 C64 C65 C66 178.2(3) . . . . ? C62 C61 C66 C65 -0.5(4) . . . . ? N6 C61 C66 C65 177.9(3) . . . . ? C62 C61 C66 C69 179.4(3) . . . . ? N6 C61 C66 C69 -2.1(4) . . . . ? C64 C65 C66 C61 1.2(4) . . . . ? C64 C65 C66 C69 -178.7(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4 S3 0.904(10) 2.721(17) 3.542(3) 152(2) . N5 H5 S1 0.908(10) 2.989(15) 3.861(2) 161(3) . N6 H6 S2 0.900(10) 2.86(2) 3.629(2) 144(3) . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.293 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.065 # Attachment '- [Cu3LIII3].cif' data_safin27 #TrackingRef '- C0CE00337A_ccdc_684171_739994_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 739994' #TrackingRef '- [Cu3LIII3].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H72 Cu3 N6 O6 P3 S6' _chemical_formula_sum 'C45 H72 Cu3 N6 O6 P3 S6' _chemical_formula_weight 1268.98 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 17.9577(7) _cell_length_b 17.9577(7) _cell_length_c 32.1945(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8991.1(7) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15044 _cell_measurement_theta_min 3.6 _cell_measurement_theta_max 26.0 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3960 _exptl_absorpt_coefficient_mu 1.391 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6646 _exptl_absorpt_correction_T_max 0.7052 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _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 '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 16656 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.61 _reflns_number_total 3745 _reflns_number_gt 3247 _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 in SHELXTL-Plus (Sheldrick, 1991)' _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^)+(0.0487P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3745 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.002 _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 0.468779(14) 0.772484(15) 0.425221(8) 0.02271(9) Uani 1 1 d . . . P1 P 0.64291(3) 0.78033(3) 0.430287(16) 0.01749(12) Uani 1 1 d . . . S1 S 0.60295(3) 0.85424(3) 0.403349(18) 0.02574(13) Uani 1 1 d . . . S2 S 0.43328(3) 0.63730(3) 0.439480(18) 0.02398(13) Uani 1 1 d . . . N1 N 0.59682(10) 0.68110(10) 0.41707(5) 0.0207(3) Uani 1 1 d . . . N2 N 0.49016(11) 0.54356(10) 0.40374(6) 0.0236(4) Uani 1 1 d . . . H2 H 0.4374(17) 0.5061(16) 0.4091(8) 0.034(7) Uiso 1 1 d . . . O1 O 0.74146(8) 0.81889(8) 0.42044(4) 0.0208(3) Uani 1 1 d . . . O2 O 0.64198(9) 0.78289(8) 0.47884(4) 0.0242(3) Uani 1 1 d . . . C1 C 0.51562(11) 0.62298(12) 0.41862(6) 0.0194(4) Uani 1 1 d . . . C2 C 0.77432(13) 0.83831(14) 0.37789(7) 0.0262(4) Uani 1 1 d . . . H2A H 0.7260 0.8255 0.3584 0.031 Uiso 1 1 calc R . . C3 C 0.81185(15) 0.78221(17) 0.36737(8) 0.0370(5) Uani 1 1 d . . . H3A H 0.7665 0.7217 0.3683 0.055 Uiso 1 1 calc R . . H3B H 0.8568 0.7921 0.3875 0.055 Uiso 1 1 calc R . . H3C H 0.8368 0.7963 0.3394 0.055 Uiso 1 1 calc R . . C4 C 0.83932(18) 0.93287(16) 0.37639(10) 0.0515(7) Uani 1 1 d . . . H4A H 0.8111 0.9660 0.3832 0.077 Uiso 1 1 calc R . . H4B H 0.8640 0.9482 0.3484 0.077 Uiso 1 1 calc R . . H4C H 0.8851 0.9459 0.3966 0.077 Uiso 1 1 calc R . . C5 C 0.68203(15) 0.86482(14) 0.50192(7) 0.0332(5) Uani 1 1 d . . . H5 H 0.7015 0.9134 0.4818 0.040 Uiso 1 1 calc R . . C6 C 0.75880(19) 0.8726(2) 0.52436(10) 0.0570(8) Uani 1 1 d . . . H6A H 0.8002 0.8739 0.5041 0.085 Uiso 1 1 calc R . . H6B H 0.7405 0.8231 0.5429 0.085 Uiso 1 1 calc R . . H6C H 0.7858 0.9257 0.5407 0.085 Uiso 1 1 calc R . . C7 C 0.6143(2) 0.8633(2) 0.52961(11) 0.0721(11) Uani 1 1 d . . . H7A H 0.5666 0.8581 0.5126 0.108 Uiso 1 1 calc R . . H7B H 0.6389 0.9168 0.5457 0.108 Uiso 1 1 calc R . . H7C H 0.5931 0.8142 0.5486 0.108 Uiso 1 1 calc R . . C11 C 0.54847(12) 0.51295(12) 0.39467(7) 0.0217(4) Uani 1 1 d . . . C12 C 0.54759(14) 0.45094(13) 0.42111(7) 0.0279(5) Uani 1 1 d . . . C13 C 0.60775(16) 0.42473(14) 0.41349(8) 0.0353(5) Uani 1 1 d . . . H13 H 0.6094 0.3831 0.4311 0.042 Uiso 1 1 calc R . . C14 C 0.66441(15) 0.45835(15) 0.38091(9) 0.0381(6) Uani 1 1 d . . . H14 H 0.7060 0.4411 0.3767 0.046 Uiso 1 1 calc R . . C15 C 0.66145(14) 0.51671(14) 0.35435(8) 0.0325(5) Uani 1 1 d . . . H15 H 0.7003 0.5384 0.3316 0.039 Uiso 1 1 calc R . . C16 C 0.60241(12) 0.54453(12) 0.36021(7) 0.0240(4) Uani 1 1 d . . . C17 C 0.48418(19) 0.41286(17) 0.45630(8) 0.0457(6) Uani 1 1 d . . . H17A H 0.4864 0.4592 0.4733 0.069 Uiso 1 1 calc R . . H17B H 0.4988 0.3770 0.4735 0.069 Uiso 1 1 calc R . . H17C H 0.4261 0.3776 0.4450 0.069 Uiso 1 1 calc R . . C18 C 0.59636(15) 0.60335(14) 0.32904(7) 0.0330(5) Uani 1 1 d . . . H18A H 0.6258 0.6623 0.3398 0.050 Uiso 1 1 calc R . . H18B H 0.5358 0.5849 0.3239 0.050 Uiso 1 1 calc R . . H18C H 0.6236 0.6013 0.3030 0.050 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 0.01762(13) 0.01978(14) 0.03429(16) -0.00094(10) -0.00125(10) 0.01201(10) P1 0.0134(2) 0.0144(2) 0.0241(3) -0.00126(18) -0.00005(18) 0.00642(19) S1 0.0207(2) 0.0215(2) 0.0379(3) 0.0079(2) 0.0048(2) 0.0127(2) S2 0.0137(2) 0.0156(2) 0.0427(3) -0.0024(2) 0.0010(2) 0.00738(18) N1 0.0153(8) 0.0169(8) 0.0309(9) -0.0048(7) -0.0032(7) 0.0089(6) N2 0.0140(8) 0.0146(8) 0.0414(11) -0.0040(7) -0.0009(7) 0.0065(7) O1 0.0134(6) 0.0205(6) 0.0257(8) 0.0006(5) -0.0007(5) 0.0063(5) O2 0.0250(7) 0.0187(7) 0.0243(8) -0.0029(6) 0.0003(6) 0.0075(6) C1 0.0166(9) 0.0184(9) 0.0266(11) -0.0009(8) -0.0034(7) 0.0113(8) C2 0.0202(10) 0.0322(11) 0.0276(11) 0.0054(9) 0.0036(8) 0.0143(9) C3 0.0354(12) 0.0559(15) 0.0327(13) -0.0044(11) 0.0001(10) 0.0325(12) C4 0.0416(15) 0.0337(13) 0.069(2) 0.0184(13) 0.0197(14) 0.0110(12) C5 0.0387(12) 0.0258(11) 0.0299(12) -0.0119(9) -0.0021(10) 0.0122(10) C6 0.0559(18) 0.0580(18) 0.0526(18) -0.0274(15) -0.0254(14) 0.0252(15) C7 0.063(2) 0.077(2) 0.075(2) -0.0397(19) 0.0095(17) 0.0335(18) C11 0.0188(9) 0.0144(9) 0.0340(12) -0.0080(8) -0.0064(8) 0.0098(7) C12 0.0308(11) 0.0193(10) 0.0337(12) -0.0066(8) -0.0080(9) 0.0126(9) C13 0.0436(13) 0.0266(11) 0.0463(15) -0.0077(10) -0.0160(11) 0.0254(11) C14 0.0313(12) 0.0328(12) 0.0610(17) -0.0136(11) -0.0108(11) 0.0241(10) C15 0.0224(10) 0.0287(11) 0.0464(15) -0.0096(10) 0.0007(9) 0.0129(9) C16 0.0183(9) 0.0161(9) 0.0351(12) -0.0051(8) -0.0045(8) 0.0068(8) C17 0.0647(18) 0.0381(14) 0.0375(15) 0.0050(11) 0.0037(12) 0.0280(13) C18 0.0326(12) 0.0275(11) 0.0360(13) 0.0019(9) -0.0003(10) 0.0129(10) _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 2.1957(5) 2_665 ? Cu1 S1 2.2180(5) . ? Cu1 S2 2.2277(5) . ? P1 O2 1.5642(15) . ? P1 O1 1.5768(13) . ? P1 N1 1.6021(16) . ? P1 S1 1.9952(7) . ? S2 C1 1.7560(19) . ? S2 Cu1 2.1958(5) 3_565 ? N1 C1 1.302(2) . ? N2 C1 1.349(3) . ? N2 C11 1.435(2) . ? N2 H2 0.86(3) . ? O1 C2 1.463(3) . ? O2 C5 1.475(2) . ? C2 C3 1.504(3) . ? C2 C4 1.505(3) . ? 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 1.498(4) . ? C5 C6 1.500(4) . ? 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 1.393(3) . ? C11 C12 1.395(3) . ? C12 C13 1.399(3) . ? C12 C17 1.506(3) . ? C13 C14 1.373(4) . ? C13 H13 0.9500 . ? C14 C15 1.374(4) . ? C14 H14 0.9500 . ? C15 C16 1.392(3) . ? C15 H15 0.9500 . ? C16 C18 1.500(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? 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 134.34(2) 2_665 . ? S2 Cu1 S2 111.30(2) 2_665 . ? S1 Cu1 S2 114.269(19) . . ? O2 P1 O1 102.36(8) . . ? O2 P1 N1 106.92(8) . . ? O1 P1 N1 106.09(8) . . ? O2 P1 S1 113.72(6) . . ? O1 P1 S1 108.57(6) . . ? N1 P1 S1 117.83(7) . . ? P1 S1 Cu1 93.13(2) . . ? C1 S2 Cu1 113.43(7) . 3_565 ? C1 S2 Cu1 106.12(7) . . ? Cu1 S2 Cu1 120.27(2) 3_565 . ? C1 N1 P1 129.04(14) . . ? C1 N2 C11 123.40(16) . . ? C1 N2 H2 114.4(17) . . ? C11 N2 H2 118.0(17) . . ? C2 O1 P1 121.55(12) . . ? C5 O2 P1 121.71(14) . . ? N1 C1 N2 119.03(17) . . ? N1 C1 S2 125.78(15) . . ? N2 C1 S2 115.18(13) . . ? O1 C2 C3 108.27(17) . . ? O1 C2 C4 106.95(19) . . ? C3 C2 C4 113.2(2) . . ? O1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? C4 C2 H2A 109.4 . . ? 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 107.2(2) . . ? O2 C5 C6 107.58(19) . . ? C7 C5 C6 114.6(3) . . ? O2 C5 H5 109.1 . . ? C7 C5 H5 109.1 . . ? C6 C5 H5 109.1 . . ? 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 122.59(18) . . ? C16 C11 N2 119.87(18) . . ? C12 C11 N2 117.54(19) . . ? C11 C12 C13 117.3(2) . . ? C11 C12 C17 121.7(2) . . ? C13 C12 C17 121.0(2) . . ? C14 C13 C12 120.9(2) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.5(2) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C14 C15 C16 121.1(2) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C11 117.4(2) . . ? C15 C16 C18 119.9(2) . . ? C11 C16 C18 122.61(18) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 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 O2 P1 S1 Cu1 -67.91(6) . . . . ? O1 P1 S1 Cu1 178.87(6) . . . . ? N1 P1 S1 Cu1 58.34(8) . . . . ? S2 Cu1 S1 P1 152.57(3) 2_665 . . . ? S2 Cu1 S1 P1 -23.50(3) . . . . ? S2 Cu1 S2 C1 170.26(7) 2_665 . . . ? S1 Cu1 S2 C1 -12.76(7) . . . . ? S2 Cu1 S2 Cu1 39.88(5) 2_665 . . 3_565 ? S1 Cu1 S2 Cu1 -143.14(3) . . . 3_565 ? O2 P1 N1 C1 72.6(2) . . . . ? O1 P1 N1 C1 -178.70(18) . . . . ? S1 P1 N1 C1 -56.9(2) . . . . ? O2 P1 O1 C2 -172.67(13) . . . . ? N1 P1 O1 C2 75.41(15) . . . . ? S1 P1 O1 C2 -52.14(14) . . . . ? O1 P1 O2 C5 66.62(16) . . . . ? N1 P1 O2 C5 177.92(15) . . . . ? S1 P1 O2 C5 -50.27(16) . . . . ? P1 N1 C1 N2 176.60(16) . . . . ? P1 N1 C1 S2 -4.4(3) . . . . ? C11 N2 C1 N1 14.4(3) . . . . ? C11 N2 C1 S2 -164.71(16) . . . . ? Cu1 S2 C1 N1 169.09(16) 3_565 . . . ? Cu1 S2 C1 N1 34.9(2) . . . . ? Cu1 S2 C1 N2 -11.91(18) 3_565 . . . ? Cu1 S2 C1 N2 -146.10(14) . . . . ? P1 O1 C2 C3 -117.00(17) . . . . ? P1 O1 C2 C4 120.70(17) . . . . ? P1 O2 C5 C7 124.4(2) . . . . ? P1 O2 C5 C6 -111.9(2) . . . . ? C1 N2 C11 C16 -72.3(3) . . . . ? C1 N2 C11 C12 108.5(2) . . . . ? C16 C11 C12 C13 4.2(3) . . . . ? N2 C11 C12 C13 -176.61(18) . . . . ? C16 C11 C12 C17 -175.3(2) . . . . ? N2 C11 C12 C17 3.9(3) . . . . ? C11 C12 C13 C14 -0.8(3) . . . . ? C17 C12 C13 C14 178.8(2) . . . . ? C12 C13 C14 C15 -1.9(4) . . . . ? C13 C14 C15 C16 1.3(3) . . . . ? C14 C15 C16 C11 1.9(3) . . . . ? C14 C15 C16 C18 -175.6(2) . . . . ? C12 C11 C16 C15 -4.7(3) . . . . ? N2 C11 C16 C15 176.06(18) . . . . ? C12 C11 C16 C18 172.7(2) . . . . ? N2 C11 C16 C18 -6.5(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 S1 0.86(3) 2.92(3) 3.7465(17) 163(2) 3_565 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.620 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.059