# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Sylvia M Draper' _publ_contact_author_email smdraper@tcd.ie _publ_section_title ; A dinuclear extension to constrained heteroleptic Cu(I) systems ; loop_ _publ_author_name B.Gil G.Cooke D.Nolan 'G.O Maille' L.Wang S.Varughese S.Draper data_bgi03 _database_code_depnum_ccdc_archive 'CCDC 768169' _audit_creation_date 2009-03-10T17:02:01-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C74 H60 Cu2 N8 O7 P4' _chemical_formula_weight 1424.26 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.570(4) _cell_length_b 19.092(5) _cell_length_c 28.652(7) _cell_angle_alpha 90 _cell_angle_beta 113.424(12) _cell_angle_gamma 90 _cell_volume 7313(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10108 _cell_measurement_theta_min 4.908 _cell_measurement_theta_max 46.362 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Blocks _exptl_crystal_colour Orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2936 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS; Sheldrick, 1997' _exptl_absorpt_correction_T_min 0.8684 _exptl_absorpt_correction_T_max 0.9244 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex CCD Area Detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_reflns_av_R_equivalents 0.1526 _diffrn_reflns_av_unetI/netI 0.0854 _diffrn_reflns_number 62172 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 23.44 _diffrn_reflns_theta_full 23.44 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 10616 _reflns_number_gt 7579 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection SMART _computing_cell_refinement SAINTPLUS _computing_data_reduction SAINTPLUS _computing_structure_solution 'SHELXTL (Sheldrick, 1990)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1462P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10616 _refine_ls_number_parameters 816 _refine_ls_number_restraints 258 _refine_ls_R_factor_all 0.0945 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.224 _refine_ls_wR_factor_gt 0.2105 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.498 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.109 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 C3 C 0.5646(4) 0.3925(3) 0.4730(2) 0.0431(13) Uani 1 1 d U . . H3A H 0.6353 0.3954 0.4974 0.052 Uiso 1 1 calc R . . H3B H 0.5297 0.4344 0.4781 0.052 Uiso 1 1 calc R . . C12 C 0.8420(4) 0.2803(3) 0.4680(2) 0.0360(12) Uani 1 1 d U . . C13 C 0.9190(4) 0.2424(3) 0.5071(2) 0.0403(12) Uani 1 1 d U . . C14 C 0.7899(4) 0.2078(3) 0.5348(2) 0.0376(12) Uani 1 1 d U . . C16 C 0.8910(4) 0.2065(3) 0.5417(2) 0.0423(13) Uani 1 1 d U . . C21 C 0.6001(5) 0.1469(3) 0.5773(2) 0.0489(14) Uani 1 1 d U . . H21A H 0.5297 0.1403 0.5619 0.059 Uiso 1 1 calc R . . C22 C 1.0215(4) 0.2337(3) 0.5079(2) 0.0483(14) Uani 1 1 d U . . C23 C 0.8569(4) 0.3327(3) 0.4325(2) 0.0388(12) Uani 1 1 d U . . C24 C 0.7476(4) 0.1790(3) 0.5699(2) 0.0404(12) Uani 1 1 d U . . C26 C 0.9660(5) 0.1611(4) 0.5818(2) 0.0533(15) Uani 1 1 d U . . C29 C 0.4014(4) 0.0901(3) 0.4106(2) 0.0401(12) Uani 1 1 d U . . C32 C 0.3917(5) 0.2239(3) 0.2395(2) 0.0478(14) Uani 1 1 d U . . H32A H 0.3747 0.1794 0.2486 0.057 Uiso 1 1 calc R . . C34 C 0.5710(5) -0.0055(3) 0.4060(2) 0.0518(15) Uani 1 1 d U . . H34A H 0.5025 -0.0175 0.3959 0.062 Uiso 1 1 calc R . . C35 C 0.9436(5) 0.3723(3) 0.4456(3) 0.0581(17) Uani 1 1 d U . . H35A H 0.999 0.3644 0.4769 0.07 Uiso 1 1 calc R . . C37 C 0.3278(5) 0.2561(4) 0.1957(3) 0.0649(18) Uani 1 1 d U . . H37A H 0.2663 0.2344 0.1752 0.078 Uiso 1 1 calc R . . C40 C 0.8014(5) 0.1662(4) 0.6214(2) 0.0576(17) Uani 1 1 d U . . H40A H 0.8718 0.1732 0.6365 0.069 Uiso 1 1 calc R . . C44 C 0.5392(5) 0.3229(3) 0.5557(2) 0.0473(14) Uani 1 1 d U . . C47 C 0.5997(6) 0.5067(3) 0.3582(3) 0.0690(19) Uani 1 1 d U . . H47 H 0.5384 0.4949 0.331 0.083 Uiso 1 1 calc R . . C50 C 0.6408(5) 0.1579(3) 0.3153(2) 0.0443(13) Uani 1 1 d U . . C51 C 0.7835(5) 0.3901(3) 0.3565(2) 0.0527(15) Uani 1 1 d U . . H51A H 0.7286 0.3959 0.3247 0.063 Uiso 1 1 calc R . . C59 C 0.6475(5) 0.1335(3) 0.6276(2) 0.0583(17) Uani 1 1 d U . . H59A H 0.6112 0.1181 0.6468 0.07 Uiso 1 1 calc R . . C62 C 0.4048(5) 0.0615(3) 0.4560(2) 0.0558(16) Uani 1 1 d U . . H62A H 0.4644 0.0652 0.4859 0.067 Uiso 1 1 calc R . . C64 C 0.4792(4) 0.2551(3) 0.2700(2) 0.0402(12) Uani 1 1 d U . . C66 C 0.7193(5) 0.4901(3) 0.4442(3) 0.0616(17) Uani 1 1 d U . . H66A H 0.7396 0.4668 0.476 0.074 Uiso 1 1 calc R . . C67 C 0.7010(5) 0.0794(3) 0.4297(2) 0.0505(15) Uani 1 1 d U . . H67A H 0.7231 0.1265 0.4369 0.061 Uiso 1 1 calc R . . C73 C 0.3732(4) 0.3260(3) 0.4567(2) 0.0482(14) Uani 1 1 d U . . C74 C 0.3249(5) 0.3856(4) 0.4631(3) 0.079(2) Uani 1 1 d U . . H74A H 0.3624 0.422 0.485 0.095 Uiso 1 1 calc R . . C81 C 0.3851(6) 0.4768(4) 0.3732(4) 0.084(2) Uani 1 1 d U . . H81A H 0.4238 0.5122 0.3958 0.101 Uiso 1 1 calc R . . C82 C 0.6377(5) 0.3333(3) 0.5888(2) 0.0562(16) Uani 1 1 d U . . H82A H 0.6873 0.342 0.5758 0.067 Uiso 1 1 calc R . . C85 C 0.7500(6) 0.1427(4) 0.6504(3) 0.073(2) Uani 1 1 d U . . H85A H 0.7852 0.1331 0.6856 0.088 Uiso 1 1 calc R . . C89 C 0.6413(6) -0.0566(3) 0.4109(3) 0.0629(17) Uani 1 1 d U . . H89A H 0.6213 -0.1043 0.4052 0.075 Uiso 1 1 calc R . . C90 C 0.6302(5) 0.4725(3) 0.4054(3) 0.0488(14) Uani 1 1 d U . . C91 C 0.6022(4) 0.0637(3) 0.4160(2) 0.0387(12) Uani 1 1 d U . . C93 C 0.4310(4) 0.4159(3) 0.3689(2) 0.0454(13) Uani 1 1 d U . . C94 C 0.3724(5) 0.3682(4) 0.3334(3) 0.0679(19) Uani 1 1 d U . . H94A H 0.4006 0.3252 0.3289 0.081 Uiso 1 1 calc R . . C96 C 0.6626(7) 0.5593(4) 0.3523(4) 0.086(2) Uani 1 1 d U . . H96A H 0.6432 0.5838 0.3209 0.103 Uiso 1 1 calc R . . C98 C 0.8675(5) 0.4310(4) 0.3670(3) 0.0642(18) Uani 1 1 d U . . H98A H 0.8698 0.4645 0.3429 0.077 Uiso 1 1 calc R . . C99 C 0.6069(6) 0.0928(3) 0.2922(3) 0.0653(19) Uani 1 1 d U . . H99A H 0.54 0.0786 0.2845 0.078 Uiso 1 1 calc R . . C100 C 1.1360(7) 0.1807(4) 0.4788(4) 0.086(2) Uani 1 1 d U . . H10A H 1.1467 0.1495 0.4556 0.103 Uiso 1 1 calc R . . C101 C 0.5064(5) 0.3187(3) 0.2551(2) 0.0553(16) Uani 1 1 d U . . H10B H 0.5685 0.3398 0.2755 0.066 Uiso 1 1 calc R . . C104 C 0.7396(6) -0.0392(3) 0.4241(3) 0.0641(18) Uani 1 1 d U . . H10C H 0.7871 -0.0747 0.4268 0.077 Uiso 1 1 calc R . . C107 C 1.0324(5) 0.1927(4) 0.6269(3) 0.075(2) Uani 1 1 d U . . H10D H 1.0327 0.2419 0.6319 0.09 Uiso 1 1 calc R . . C110 C 0.3228(6) 0.0279(4) 0.4578(3) 0.0682(19) Uani 1 1 d U . . H11A H 0.3257 0.0082 0.4888 0.082 Uiso 1 1 calc R . . C112 C 0.7689(5) 0.0274(3) 0.4331(3) 0.0605(17) Uani 1 1 d U . . H11B H 0.8372 0.0391 0.4419 0.073 Uiso 1 1 calc R . . C114 C 1.0992(7) 0.1473(6) 0.6649(4) 0.106(3) Uani 1 1 d U . . H11C H 1.1434 0.1672 0.6961 0.127 Uiso 1 1 calc R . . C115 C 0.3140(5) 0.0845(4) 0.3678(3) 0.0621(18) Uani 1 1 d U . . H11D H 0.3095 0.1046 0.3367 0.075 Uiso 1 1 calc R . . C116 C 1.1967(5) 0.2510(5) 0.5450(3) 0.079(2) Uani 1 1 d U . . H11E H 1.2529 0.2729 0.5705 0.095 Uiso 1 1 calc R . . C117 C 0.9687(5) 0.0911(4) 0.5749(3) 0.0654(18) Uani 1 1 d U . . H11F H 0.9248 0.0694 0.5443 0.078 Uiso 1 1 calc R . . C120 C 0.9477(5) 0.4228(4) 0.4126(3) 0.0668(19) Uani 1 1 d U . . H12A H 1.0051 0.4518 0.4211 0.08 Uiso 1 1 calc R . . C121 C 0.3156(5) 0.2739(4) 0.4257(3) 0.0590(16) Uani 1 1 d U . . H12B H 0.347 0.2317 0.4223 0.071 Uiso 1 1 calc R . . C124 C 1.0380(8) 0.0521(5) 0.6141(4) 0.095(3) Uani 1 1 d U . . H12C H 1.0401 0.003 0.6092 0.114 Uiso 1 1 calc R . . C130 C 0.2852(6) 0.4881(4) 0.3459(4) 0.099(3) Uani 1 1 d U . . H13A H 0.2542 0.5291 0.3517 0.119 Uiso 1 1 calc R . . C131 C 0.2362(6) 0.0231(4) 0.4142(3) 0.0692(19) Uani 1 1 d U . . H13B H 0.1789 0.0008 0.4154 0.083 Uiso 1 1 calc R . . C133 C 1.0369(6) 0.1919(4) 0.4731(3) 0.0649(18) Uani 1 1 d U . . H13C H 0.9825 0.1711 0.446 0.078 Uiso 1 1 calc R . . C134 C 0.7384(5) 0.1777(4) 0.3249(3) 0.069(2) Uani 1 1 d U . . H13D H 0.7634 0.2213 0.341 0.082 Uiso 1 1 calc R . . C135 C 0.4689(6) 0.3093(4) 0.5760(3) 0.076(2) Uani 1 1 d U . . H13E H 0.4011 0.3008 0.554 0.091 Uiso 1 1 calc R . . C136 C 1.1056(5) 0.2656(4) 0.5447(3) 0.0632(17) Uani 1 1 d U . . H13F H 1.0989 0.2968 0.569 0.076 Uiso 1 1 calc R . . C141 C 0.2330(6) 0.0499(4) 0.3700(3) 0.079(2) Uani 1 1 d U . . H14A H 0.1739 0.0449 0.3399 0.094 Uiso 1 1 calc R . . C142 C 0.7639(7) 0.0713(5) 0.2897(4) 0.092(3) Uani 1 1 d U . . H14B H 0.8069 0.0416 0.281 0.11 Uiso 1 1 calc R . . C143 C 0.7980(7) 0.1351(5) 0.3114(4) 0.097(3) Uani 1 1 d U . . H14C H 0.864 0.1496 0.317 0.117 Uiso 1 1 calc R . . C144 C 0.2238(6) 0.3922(5) 0.4380(4) 0.097(3) Uani 1 1 d U . . H14D H 0.1919 0.4334 0.4428 0.116 Uiso 1 1 calc R . . C146 C 0.6640(6) 0.3308(4) 0.6407(3) 0.0724(19) Uani 1 1 d U . . H14E H 0.7318 0.3377 0.6631 0.087 Uiso 1 1 calc R . . C147 C 0.2316(6) 0.4419(5) 0.3113(4) 0.086(2) Uani 1 1 d U . . H14F H 0.1631 0.4509 0.2911 0.104 Uiso 1 1 calc R . . C151 C 0.3529(6) 0.3198(4) 0.1817(3) 0.0697(19) Uani 1 1 d U . . H15A H 0.308 0.3425 0.1518 0.084 Uiso 1 1 calc R . . C155 C 0.4432(6) 0.3509(4) 0.2109(3) 0.071(2) Uani 1 1 d U . . H15B H 0.4616 0.3941 0.2006 0.085 Uiso 1 1 calc R . . C157 C 0.2740(6) 0.3824(5) 0.3047(3) 0.092(3) Uani 1 1 d U . . H15C H 0.235 0.3496 0.2798 0.111 Uiso 1 1 calc R . . C159 C 0.2143(6) 0.2809(5) 0.3997(3) 0.083(2) Uani 1 1 d U . . H15D H 0.1764 0.245 0.3774 0.099 Uiso 1 1 calc R . . C163 C 0.4719(4) 0.1655(3) 0.3461(2) 0.0385(12) Uani 1 1 d U . . H16A H 0.4101 0.1933 0.3378 0.046 Uiso 1 1 calc R . . H16B H 0.4545 0.1241 0.3234 0.046 Uiso 1 1 calc R . . C168 C 0.7790(7) 0.5408(4) 0.4373(4) 0.092(3) Uani 1 1 d U . . H16C H 0.8403 0.5527 0.4644 0.11 Uiso 1 1 calc R . . C186 C 0.6700(7) 0.0498(4) 0.2807(3) 0.081(2) Uani 1 1 d U . . H18A H 0.6478 0.0049 0.2663 0.098 Uiso 1 1 calc R . . C190 C 0.7504(7) 0.5748(4) 0.3911(4) 0.087(2) Uani 1 1 d U . . H19A H 0.7929 0.6095 0.3865 0.104 Uiso 1 1 calc R . . C196 C 0.5941(8) 0.3186(4) 0.6602(3) 0.084(2) Uani 1 1 d U . . H19B H 0.6122 0.3175 0.6959 0.101 Uiso 1 1 calc R . . C202 C 0.4971(8) 0.3080(5) 0.6271(4) 0.096(3) Uani 1 1 d U . . H20A H 0.4479 0.2995 0.6404 0.116 Uiso 1 1 calc R . . C246 C 0.1678(6) 0.3416(5) 0.4064(3) 0.088(2) Uani 1 1 d U . . H24A H 0.0975 0.3473 0.3891 0.105 Uiso 1 1 calc R . . Cu1 Cu 0.57409(5) 0.21339(3) 0.47456(2) 0.0362(2) Uani 1 1 d U . . Cu3 Cu 0.63953(5) 0.30194(3) 0.38988(2) 0.0363(2) Uani 1 1 d U . . N1 N 0.7764(3) 0.3429(2) 0.38922(17) 0.0400(10) Uani 1 1 d U . . N2 N 0.7474(3) 0.2716(2) 0.45984(16) 0.0364(10) Uani 1 1 d U . . N3 N 0.7210(3) 0.2354(2) 0.49290(16) 0.0346(10) Uani 1 1 d U . . N4 N 0.6461(3) 0.1690(2) 0.54782(17) 0.0408(10) Uani 1 1 d U . . N5 N 1.2141(5) 0.2095(4) 0.5133(3) 0.085(2) Uani 1 1 d U . . N6 N 1.1026(6) 0.0794(5) 0.6586(4) 0.115(3) Uani 1 1 d U . . N97 N 0.3203(6) 0.0004(4) 0.2625(3) 0.0845(19) Uiso 1 1 d U . . N98 N 0.9031(7) 0.3899(5) 0.5787(4) 0.103(2) Uiso 1 1 d U . . O96 O 1.1192(5) 0.3093(3) 0.7497(3) 0.108(2) Uiso 1 1 d . . . O97A O 0.4063(9) -0.0071(5) 0.2860(4) 0.184(4) Uiso 1 1 d U . . O97B O 0.2600(8) -0.0400(5) 0.2563(4) 0.166(3) Uiso 1 1 d U . . O97C O 0.2992(6) 0.0613(4) 0.2529(3) 0.093(3) Uiso 0.763(12) 1 d PU . . O98A O 0.8921(10) 0.3382(8) 0.6091(5) 0.236(5) Uiso 1 1 d U . . O98B O 0.9875(9) 0.3765(6) 0.5897(5) 0.191(4) Uiso 1 1 d U . . O98C O 0.8215(8) 0.3827(5) 0.5475(4) 0.170(3) Uiso 1 1 d U . . O98D O 0.8995(17) 0.4544(12) 0.5945(9) 0.081(9) Uiso 0.237(12) 1 d PU . . P5 P 0.56296(11) 0.21902(7) 0.33190(5) 0.0355(4) Uani 1 1 d U . . P7 P 0.51382(11) 0.13481(7) 0.41224(5) 0.0360(4) Uani 1 1 d U . . P10 P 0.50775(11) 0.31390(7) 0.48772(6) 0.0396(4) Uani 1 1 d U . . P12 P 0.55995(11) 0.39403(7) 0.40758(6) 0.0398(4) Uani 1 1 d U . . 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 C3 0.049(3) 0.037(3) 0.047(3) -0.004(3) 0.023(3) -0.004(2) C12 0.036(3) 0.031(3) 0.044(3) 0.001(2) 0.019(2) -0.002(2) C13 0.041(3) 0.038(3) 0.044(3) 0.001(2) 0.018(3) -0.003(2) C14 0.046(3) 0.030(3) 0.038(3) 0.001(2) 0.018(3) -0.002(2) C16 0.046(3) 0.037(3) 0.043(3) 0.004(2) 0.017(3) 0.000(2) C21 0.062(4) 0.046(3) 0.051(3) -0.003(3) 0.035(3) -0.012(3) C22 0.047(3) 0.046(3) 0.054(4) 0.018(3) 0.021(3) 0.007(3) C23 0.038(3) 0.038(3) 0.043(3) 0.007(2) 0.019(3) 0.003(2) C24 0.046(3) 0.042(3) 0.034(3) -0.001(2) 0.016(2) -0.002(2) C26 0.044(3) 0.067(4) 0.052(4) 0.020(3) 0.022(3) 0.002(3) C29 0.056(3) 0.029(3) 0.040(3) -0.003(2) 0.024(3) -0.003(2) C32 0.062(4) 0.038(3) 0.044(3) 0.007(3) 0.022(3) 0.001(3) C34 0.069(4) 0.039(3) 0.056(4) -0.009(3) 0.034(3) -0.003(3) C35 0.050(4) 0.048(4) 0.076(5) 0.017(3) 0.025(3) -0.004(3) C37 0.068(4) 0.077(5) 0.043(4) 0.004(3) 0.015(3) -0.009(3) C40 0.051(4) 0.083(5) 0.041(3) 0.014(3) 0.020(3) 0.001(3) C44 0.060(4) 0.044(3) 0.048(3) -0.010(3) 0.031(3) -0.001(3) C47 0.090(5) 0.047(4) 0.073(4) 0.008(3) 0.036(4) -0.007(3) C50 0.066(4) 0.039(3) 0.034(3) 0.004(2) 0.026(3) 0.005(3) C51 0.057(4) 0.052(4) 0.053(4) 0.013(3) 0.025(3) 0.000(3) C59 0.076(4) 0.060(4) 0.048(4) 0.005(3) 0.035(3) -0.013(3) C62 0.065(4) 0.060(4) 0.045(4) 0.009(3) 0.025(3) -0.010(3) C64 0.059(3) 0.033(3) 0.032(3) 0.001(2) 0.022(2) 0.006(2) C66 0.074(4) 0.051(4) 0.063(4) -0.007(3) 0.031(3) -0.018(3) C67 0.056(4) 0.042(3) 0.056(4) -0.006(3) 0.025(3) -0.002(3) C73 0.043(3) 0.059(4) 0.052(4) 0.002(3) 0.028(3) 0.002(2) C74 0.053(4) 0.066(4) 0.118(7) -0.018(4) 0.032(4) 0.012(3) C81 0.067(4) 0.049(4) 0.121(7) -0.007(4) 0.022(4) 0.015(3) C82 0.069(4) 0.054(4) 0.055(4) -0.010(3) 0.034(3) -0.014(3) C85 0.094(5) 0.086(5) 0.044(4) 0.016(4) 0.031(4) -0.002(4) C89 0.090(5) 0.040(3) 0.069(5) -0.004(3) 0.043(4) 0.006(3) C90 0.064(4) 0.027(3) 0.064(4) 0.003(3) 0.034(3) 0.000(3) C91 0.056(3) 0.035(3) 0.025(3) -0.002(2) 0.016(3) -0.001(2) C93 0.047(3) 0.036(3) 0.050(3) 0.004(3) 0.016(3) 0.002(2) C94 0.061(4) 0.075(5) 0.056(4) -0.012(3) 0.010(3) 0.008(3) C96 0.130(7) 0.045(4) 0.107(6) 0.013(4) 0.073(5) -0.010(4) C98 0.061(4) 0.062(4) 0.082(5) 0.028(4) 0.040(4) -0.001(3) C99 0.096(5) 0.052(4) 0.068(5) -0.012(3) 0.054(4) -0.004(3) C100 0.092(6) 0.076(5) 0.119(7) 0.005(5) 0.073(5) 0.013(4) C101 0.075(4) 0.045(3) 0.049(4) 0.005(3) 0.027(3) -0.010(3) C104 0.087(5) 0.050(4) 0.070(5) 0.000(3) 0.047(4) 0.021(3) C107 0.055(4) 0.091(5) 0.062(4) 0.027(4) 0.005(3) -0.012(4) C110 0.085(5) 0.070(5) 0.063(4) 0.006(4) 0.044(4) -0.018(4) C112 0.055(4) 0.055(4) 0.070(5) -0.013(3) 0.024(4) 0.005(3) C114 0.080(6) 0.132(7) 0.078(6) 0.044(5) 0.001(4) -0.014(5) C115 0.060(4) 0.083(5) 0.046(4) 0.003(3) 0.024(3) -0.022(3) C116 0.045(4) 0.099(6) 0.090(6) 0.025(4) 0.025(4) -0.001(4) C117 0.073(5) 0.054(4) 0.082(5) 0.024(3) 0.044(4) 0.017(3) C120 0.049(4) 0.061(4) 0.097(5) 0.020(4) 0.036(4) -0.010(3) C121 0.053(4) 0.061(4) 0.063(4) -0.007(3) 0.024(3) -0.001(3) C124 0.111(7) 0.075(5) 0.113(7) 0.043(5) 0.059(5) 0.032(5) C130 0.067(5) 0.055(5) 0.157(9) 0.023(5) 0.025(5) 0.024(4) C131 0.069(4) 0.070(5) 0.082(5) -0.003(4) 0.044(4) -0.021(4) C133 0.067(4) 0.066(4) 0.073(5) 0.001(3) 0.039(4) 0.001(3) C134 0.066(4) 0.064(4) 0.092(6) -0.015(4) 0.050(4) -0.002(3) C135 0.071(5) 0.113(6) 0.059(4) -0.001(4) 0.042(4) -0.002(4) C136 0.042(3) 0.079(5) 0.068(5) 0.005(4) 0.021(3) 0.000(3) C141 0.061(4) 0.100(6) 0.072(5) 0.004(4) 0.025(4) -0.025(4) C142 0.114(6) 0.083(5) 0.101(7) -0.005(5) 0.066(6) 0.036(5) C143 0.076(5) 0.100(6) 0.137(8) -0.023(6) 0.065(6) 0.007(4) C144 0.058(5) 0.096(6) 0.135(8) -0.006(5) 0.036(5) 0.027(4) C146 0.095(5) 0.059(4) 0.052(4) -0.009(4) 0.017(4) -0.003(4) C147 0.056(5) 0.089(6) 0.098(6) 0.031(5) 0.014(4) 0.012(4) C151 0.080(5) 0.069(4) 0.058(4) 0.024(4) 0.025(4) 0.005(4) C155 0.091(5) 0.053(4) 0.062(5) 0.024(3) 0.024(4) -0.006(3) C157 0.061(5) 0.124(7) 0.067(5) -0.021(5) -0.001(4) 0.003(4) C159 0.048(4) 0.111(6) 0.082(6) -0.016(5) 0.019(4) -0.008(4) C163 0.045(3) 0.037(3) 0.033(3) 0.000(2) 0.015(3) -0.005(2) C168 0.100(6) 0.082(6) 0.101(6) -0.030(5) 0.048(5) -0.048(5) C186 0.123(6) 0.049(4) 0.091(6) -0.004(4) 0.063(6) 0.016(4) C190 0.122(7) 0.047(4) 0.119(7) -0.013(4) 0.077(6) -0.030(4) C196 0.137(7) 0.079(5) 0.049(4) -0.003(4) 0.048(4) 0.011(5) C202 0.114(6) 0.132(8) 0.074(5) 0.002(5) 0.071(5) 0.002(6) C246 0.047(4) 0.127(7) 0.083(6) 0.019(5) 0.019(4) 0.013(4) Cu1 0.0405(4) 0.0353(4) 0.0358(4) -0.0027(3) 0.0184(3) -0.0038(3) Cu3 0.0410(4) 0.0329(4) 0.0362(4) 0.0013(3) 0.0166(3) -0.0018(3) N1 0.051(3) 0.037(2) 0.042(3) 0.004(2) 0.028(2) -0.005(2) N2 0.044(3) 0.035(2) 0.035(2) 0.0020(19) 0.020(2) -0.0014(19) N3 0.039(2) 0.035(2) 0.032(2) 0.0031(19) 0.017(2) -0.0025(19) N4 0.051(3) 0.038(3) 0.038(2) 0.001(2) 0.023(2) -0.003(2) N5 0.063(4) 0.088(5) 0.121(6) 0.037(4) 0.054(4) 0.021(3) N6 0.079(5) 0.128(6) 0.129(7) 0.065(6) 0.031(4) 0.032(5) P5 0.0457(9) 0.0308(7) 0.0330(8) 0.0013(6) 0.0188(7) -0.0010(6) P7 0.0467(9) 0.0303(7) 0.0335(8) -0.0005(6) 0.0186(7) -0.0039(6) P10 0.0420(9) 0.0387(8) 0.0440(9) -0.0057(7) 0.0232(7) -0.0021(6) P12 0.0477(9) 0.0293(8) 0.0433(9) -0.0001(6) 0.0190(7) -0.0008(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C3 P10 1.842(5) . ? C3 P12 1.849(6) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C12 N2 1.313(7) . ? C12 C13 1.427(8) . ? C12 C23 1.504(7) . ? C13 C16 1.393(8) . ? C13 C22 1.494(8) . ? C14 N3 1.329(7) . ? C14 C16 1.406(8) . ? C14 C24 1.481(7) . ? C16 C26 1.505(8) . ? C21 N4 1.337(7) . ? C21 C59 1.353(9) . ? C21 H21A 0.95 . ? C22 C133 1.364(9) . ? C22 C136 1.399(9) . ? C23 N1 1.340(7) . ? C23 C35 1.389(8) . ? C24 N4 1.371(7) . ? C24 C40 1.389(8) . ? C26 C117 1.354(9) . ? C26 C107 1.406(10) . ? C29 C115 1.376(9) . ? C29 C62 1.394(8) . ? C29 P7 1.830(6) . ? C32 C64 1.363(8) . ? C32 C37 1.374(9) . ? C32 H32A 0.95 . ? C34 C89 1.380(9) . ? C34 C91 1.389(8) . ? C34 H34A 0.95 . ? C35 C120 1.369(9) . ? C35 H35A 0.95 . ? C37 C151 1.376(9) . ? C37 H37A 0.95 . ? C40 C85 1.396(9) . ? C40 H40A 0.95 . ? C44 C82 1.384(9) . ? C44 C135 1.388(9) . ? C44 P10 1.824(6) . ? C47 C90 1.405(9) . ? C47 C96 1.415(10) . ? C47 H47 0.95 . ? C50 C134 1.389(9) . ? C50 C99 1.402(9) . ? C50 P5 1.817(6) . ? C51 N1 1.336(7) . ? C51 C98 1.380(9) . ? C51 H51A 0.95 . ? C59 C85 1.383(10) . ? C59 H59A 0.95 . ? C62 C110 1.375(9) . ? C62 H62A 0.95 . ? C64 C101 1.395(8) . ? C64 P5 1.841(6) . ? C66 C168 1.368(10) . ? C66 C90 1.373(9) . ? C66 H66A 0.95 . ? C67 C91 1.367(8) . ? C67 C112 1.376(8) . ? C67 H67A 0.95 . ? C73 C121 1.375(9) . ? C73 C74 1.388(9) . ? C73 P10 1.817(6) . ? C74 C144 1.364(11) . ? C74 H74A 0.95 . ? C81 C130 1.369(11) . ? C81 C93 1.370(9) . ? C81 H81A 0.95 . ? C82 C146 1.381(9) . ? C82 H82A 0.95 . ? C85 H85A 0.95 . ? C89 C104 1.370(10) . ? C89 H89A 0.95 . ? C90 P12 1.830(6) . ? C91 P7 1.845(6) . ? C93 C94 1.379(9) . ? C93 P12 1.811(6) . ? C94 C157 1.366(10) . ? C94 H94A 0.95 . ? C96 C190 1.353(13) . ? C96 H96A 0.95 . ? C98 C120 1.372(10) . ? C98 H98A 0.95 . ? C99 C186 1.368(10) . ? C99 H99A 0.95 . ? C100 N5 1.296(11) . ? C100 C133 1.403(11) . ? C100 H10A 0.95 . ? C101 C155 1.381(9) . ? C101 H10B 0.95 . ? C104 C112 1.334(9) . ? C104 H10C 0.95 . ? C107 C114 1.428(11) . ? C107 H10D 0.95 . ? C110 C131 1.380(10) . ? C110 H11A 0.95 . ? C112 H11B 0.95 . ? C114 N6 1.313(13) . ? C114 H11C 0.95 . ? C115 C141 1.375(9) . ? C115 H11D 0.95 . ? C116 N5 1.304(11) . ? C116 C136 1.353(9) . ? C116 H11E 0.95 . ? C117 C124 1.390(11) . ? C117 H11F 0.95 . ? C120 H12A 0.95 . ? C121 C159 1.370(10) . ? C121 H12B 0.95 . ? C124 N6 1.352(13) . ? C124 H12C 0.95 . ? C130 C147 1.324(12) . ? C130 H13A 0.95 . ? C131 C141 1.350(10) . ? C131 H13B 0.95 . ? C133 H13C 0.95 . ? C134 C143 1.355(10) . ? C134 H13D 0.95 . ? C135 C202 1.354(11) . ? C135 H13E 0.95 . ? C136 H13F 0.95 . ? C141 H14A 0.95 . ? C142 C186 1.351(12) . ? C142 C143 1.368(12) . ? C142 H14B 0.95 . ? C143 H14C 0.95 . ? C144 C246 1.353(12) . ? C144 H14D 0.95 . ? C146 C196 1.362(11) . ? C146 H14E 0.95 . ? C147 C157 1.342(11) . ? C147 H14F 0.95 . ? C151 C155 1.381(10) . ? C151 H15A 0.95 . ? C155 H15B 0.95 . ? C157 H15C 0.95 . ? C159 C246 1.393(12) . ? C159 H15D 0.95 . ? C163 P7 1.840(5) . ? C163 P5 1.844(5) . ? C163 H16A 0.99 . ? C163 H16B 0.99 . ? C168 C190 1.382(12) . ? C168 H16C 0.95 . ? C186 H18A 0.95 . ? C190 H19A 0.95 . ? C196 C202 1.368(12) . ? C196 H19B 0.95 . ? C202 H20A 0.95 . ? C246 H24A 0.95 . ? Cu1 N3 2.035(4) . ? Cu1 N4 2.115(5) . ? Cu1 P7 2.2280(16) . ? Cu1 P10 2.2470(16) . ? Cu3 N2 2.079(5) . ? Cu3 N1 2.149(4) . ? Cu3 P5 2.2442(16) . ? Cu3 P12 2.2717(16) . ? N2 N3 1.346(6) . ? N97 O97B 1.129(10) . ? N97 O97A 1.172(11) . ? N97 O97C 1.206(9) . ? N98 O98B 1.171(12) . ? N98 O98C 1.177(11) . ? N98 O98D 1.32(2) . ? N98 O98A 1.368(14) . ? 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 P10 C3 P12 114.0(3) . . ? P10 C3 H3A 108.8 . . ? P12 C3 H3A 108.8 . . ? P10 C3 H3B 108.8 . . ? P12 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? N2 C12 C13 121.1(5) . . ? N2 C12 C23 112.8(5) . . ? C13 C12 C23 126.1(5) . . ? C16 C13 C12 116.6(5) . . ? C16 C13 C22 120.5(5) . . ? C12 C13 C22 122.5(5) . . ? N3 C14 C16 120.5(5) . . ? N3 C14 C24 113.1(5) . . ? C16 C14 C24 126.4(5) . . ? C13 C16 C14 118.4(5) . . ? C13 C16 C26 119.9(5) . . ? C14 C16 C26 121.3(5) . . ? N4 C21 C59 124.1(6) . . ? N4 C21 H21A 118 . . ? C59 C21 H21A 118 . . ? C133 C22 C136 117.1(6) . . ? C133 C22 C13 120.5(6) . . ? C136 C22 C13 122.3(6) . . ? N1 C23 C35 122.6(5) . . ? N1 C23 C12 114.4(5) . . ? C35 C23 C12 122.6(5) . . ? N4 C24 C40 121.1(5) . . ? N4 C24 C14 113.7(5) . . ? C40 C24 C14 125.1(5) . . ? C117 C26 C107 120.6(6) . . ? C117 C26 C16 120.7(6) . . ? C107 C26 C16 118.7(6) . . ? C115 C29 C62 118.5(5) . . ? C115 C29 P7 124.2(4) . . ? C62 C29 P7 117.3(5) . . ? C64 C32 C37 120.7(6) . . ? C64 C32 H32A 119.7 . . ? C37 C32 H32A 119.7 . . ? C89 C34 C91 118.9(6) . . ? C89 C34 H34A 120.6 . . ? C91 C34 H34A 120.6 . . ? C120 C35 C23 118.7(6) . . ? C120 C35 H35A 120.6 . . ? C23 C35 H35A 120.6 . . ? C32 C37 C151 120.1(7) . . ? C32 C37 H37A 120 . . ? C151 C37 H37A 120 . . ? C24 C40 C85 118.6(6) . . ? C24 C40 H40A 120.7 . . ? C85 C40 H40A 120.7 . . ? C82 C44 C135 118.5(6) . . ? C82 C44 P10 119.8(4) . . ? C135 C44 P10 121.0(5) . . ? C90 C47 C96 118.2(8) . . ? C90 C47 H47 120.9 . . ? C96 C47 H47 120.9 . . ? C134 C50 C99 118.4(6) . . ? C134 C50 P5 118.0(5) . . ? C99 C50 P5 123.6(5) . . ? N1 C51 C98 122.6(6) . . ? N1 C51 H51A 118.7 . . ? C98 C51 H51A 118.7 . . ? C21 C59 C85 118.5(6) . . ? C21 C59 H59A 120.8 . . ? C85 C59 H59A 120.8 . . ? C110 C62 C29 120.6(6) . . ? C110 C62 H62A 119.7 . . ? C29 C62 H62A 119.7 . . ? C32 C64 C101 119.4(5) . . ? C32 C64 P5 123.2(4) . . ? C101 C64 P5 117.4(5) . . ? C168 C66 C90 120.4(7) . . ? C168 C66 H66A 119.8 . . ? C90 C66 H66A 119.8 . . ? C91 C67 C112 120.5(6) . . ? C91 C67 H67A 119.8 . . ? C112 C67 H67A 119.8 . . ? C121 C73 C74 117.9(6) . . ? C121 C73 P10 119.1(5) . . ? C74 C73 P10 123.0(5) . . ? C144 C74 C73 120.2(8) . . ? C144 C74 H74A 119.9 . . ? C73 C74 H74A 119.9 . . ? C130 C81 C93 121.9(8) . . ? C130 C81 H81A 119.1 . . ? C93 C81 H81A 119.1 . . ? C146 C82 C44 120.0(6) . . ? C146 C82 H82A 120 . . ? C44 C82 H82A 120 . . ? C59 C85 C40 119.6(6) . . ? C59 C85 H85A 120.2 . . ? C40 C85 H85A 120.2 . . ? C104 C89 C34 120.6(6) . . ? C104 C89 H89A 119.7 . . ? C34 C89 H89A 119.7 . . ? C66 C90 C47 120.1(6) . . ? C66 C90 P12 122.3(5) . . ? C47 C90 P12 116.5(5) . . ? C67 C91 C34 119.3(5) . . ? C67 C91 P7 119.1(4) . . ? C34 C91 P7 121.6(5) . . ? C81 C93 C94 116.5(6) . . ? C81 C93 P12 124.4(5) . . ? C94 C93 P12 119.1(5) . . ? C157 C94 C93 120.4(7) . . ? C157 C94 H94A 119.8 . . ? C93 C94 H94A 119.8 . . ? C190 C96 C47 120.2(8) . . ? C190 C96 H96A 119.9 . . ? C47 C96 H96A 119.9 . . ? C120 C98 C51 119.3(6) . . ? C120 C98 H98A 120.4 . . ? C51 C98 H98A 120.4 . . ? C186 C99 C50 120.1(7) . . ? C186 C99 H99A 119.9 . . ? C50 C99 H99A 119.9 . . ? N5 C100 C133 125.0(8) . . ? N5 C100 H10A 117.5 . . ? C133 C100 H10A 117.5 . . ? C155 C101 C64 120.1(6) . . ? C155 C101 H10B 119.9 . . ? C64 C101 H10B 119.9 . . ? C112 C104 C89 120.3(6) . . ? C112 C104 H10C 119.9 . . ? C89 C104 H10C 119.9 . . ? C26 C107 C114 116.9(8) . . ? C26 C107 H10D 121.6 . . ? C114 C107 H10D 121.6 . . ? C62 C110 C131 119.5(6) . . ? C62 C110 H11A 120.2 . . ? C131 C110 H11A 120.2 . . ? C104 C112 C67 120.5(7) . . ? C104 C112 H11B 119.7 . . ? C67 C112 H11B 119.7 . . ? N6 C114 C107 123.1(10) . . ? N6 C114 H11C 118.5 . . ? C107 C114 H11C 118.5 . . ? C141 C115 C29 120.4(6) . . ? C141 C115 H11D 119.8 . . ? C29 C115 H11D 119.8 . . ? N5 C116 C136 125.6(8) . . ? N5 C116 H11E 117.2 . . ? C136 C116 H11E 117.2 . . ? C26 C117 C124 117.7(8) . . ? C26 C117 H11F 121.2 . . ? C124 C117 H11F 121.2 . . ? C35 C120 C98 119.0(6) . . ? C35 C120 H12A 120.5 . . ? C98 C120 H12A 120.5 . . ? C159 C121 C73 121.9(7) . . ? C159 C121 H12B 119 . . ? C73 C121 H12B 119 . . ? N6 C124 C117 124.5(9) . . ? N6 C124 H12C 117.8 . . ? C117 C124 H12C 117.8 . . ? C147 C130 C81 120.0(8) . . ? C147 C130 H13A 120 . . ? C81 C130 H13A 120 . . ? C141 C131 C110 120.1(6) . . ? C141 C131 H13B 119.9 . . ? C110 C131 H13B 119.9 . . ? C22 C133 C100 117.7(8) . . ? C22 C133 H13C 121.1 . . ? C100 C133 H13C 121.1 . . ? C143 C134 C50 120.1(7) . . ? C143 C134 H13D 119.9 . . ? C50 C134 H13D 119.9 . . ? C202 C135 C44 119.9(8) . . ? C202 C135 H13E 120.1 . . ? C44 C135 H13E 120.1 . . ? C116 C136 C22 118.6(7) . . ? C116 C136 H13F 120.7 . . ? C22 C136 H13F 120.7 . . ? C131 C141 C115 120.9(7) . . ? C131 C141 H14A 119.6 . . ? C115 C141 H14A 119.6 . . ? C186 C142 C143 121.0(7) . . ? C186 C142 H14B 119.5 . . ? C143 C142 H14B 119.5 . . ? C134 C143 C142 120.4(8) . . ? C134 C143 H14C 119.8 . . ? C142 C143 H14C 119.8 . . ? C246 C144 C74 121.6(8) . . ? C246 C144 H14D 119.2 . . ? C74 C144 H14D 119.2 . . ? C196 C146 C82 121.0(8) . . ? C196 C146 H14E 119.5 . . ? C82 C146 H14E 119.5 . . ? C130 C147 C157 120.1(8) . . ? C130 C147 H14F 119.9 . . ? C157 C147 H14F 119.9 . . ? C37 C151 C155 120.1(7) . . ? C37 C151 H15A 119.9 . . ? C155 C151 H15A 119.9 . . ? C101 C155 C151 119.5(6) . . ? C101 C155 H15B 120.3 . . ? C151 C155 H15B 120.3 . . ? C147 C157 C94 121.0(8) . . ? C147 C157 H15C 119.5 . . ? C94 C157 H15C 119.5 . . ? C121 C159 C246 119.0(8) . . ? C121 C159 H15D 120.5 . . ? C246 C159 H15D 120.5 . . ? P7 C163 P5 115.5(3) . . ? P7 C163 H16A 108.4 . . ? P5 C163 H16A 108.4 . . ? P7 C163 H16B 108.4 . . ? P5 C163 H16B 108.4 . . ? H16A C163 H16B 107.5 . . ? C66 C168 C190 120.3(8) . . ? C66 C168 H16C 119.8 . . ? C190 C168 H16C 119.8 . . ? C142 C186 C99 119.9(8) . . ? C142 C186 H18A 120.1 . . ? C99 C186 H18A 120.1 . . ? C96 C190 C168 120.7(7) . . ? C96 C190 H19A 119.7 . . ? C168 C190 H19A 119.7 . . ? C146 C196 C202 118.4(7) . . ? C146 C196 H19B 120.8 . . ? C202 C196 H19B 120.8 . . ? C135 C202 C196 122.2(8) . . ? C135 C202 H20A 118.9 . . ? C196 C202 H20A 118.9 . . ? C144 C246 C159 119.2(7) . . ? C144 C246 H24A 120.4 . . ? C159 C246 H24A 120.4 . . ? N3 Cu1 N4 76.75(17) . . ? N3 Cu1 P7 112.65(12) . . ? N4 Cu1 P7 114.04(13) . . ? N3 Cu1 P10 105.00(13) . . ? N4 Cu1 P10 104.63(13) . . ? P7 Cu1 P10 130.60(6) . . ? N2 Cu3 N1 76.19(17) . . ? N2 Cu3 P5 118.67(13) . . ? N1 Cu3 P5 116.10(13) . . ? N2 Cu3 P12 104.96(12) . . ? N1 Cu3 P12 106.16(13) . . ? P5 Cu3 P12 124.30(6) . . ? C51 N1 C23 117.6(5) . . ? C51 N1 Cu3 125.7(4) . . ? C23 N1 Cu3 114.5(3) . . ? C12 N2 N3 120.8(4) . . ? C12 N2 Cu3 118.3(3) . . ? N3 N2 Cu3 120.2(3) . . ? C14 N3 N2 120.9(4) . . ? C14 N3 Cu1 119.4(3) . . ? N2 N3 Cu1 119.3(3) . . ? C21 N4 C24 118.2(5) . . ? C21 N4 Cu1 125.2(4) . . ? C24 N4 Cu1 114.9(3) . . ? C100 N5 C116 115.8(7) . . ? C114 N6 C124 117.4(8) . . ? O97B N97 O97A 126.5(11) . . ? O97B N97 O97C 120.7(10) . . ? O97A N97 O97C 111.5(10) . . ? O98B N98 O98C 144.6(12) . . ? O98B N98 O98D 107.0(14) . . ? O98C N98 O98D 101.7(13) . . ? O98B N98 O98A 92.6(10) . . ? O98C N98 O98A 93.5(10) . . ? O98D N98 O98A 115.2(13) . . ? C50 P5 C64 103.4(2) . . ? C50 P5 C163 106.3(3) . . ? C64 P5 C163 99.2(3) . . ? C50 P5 Cu3 117.9(2) . . ? C64 P5 Cu3 113.18(18) . . ? C163 P5 Cu3 114.65(18) . . ? C29 P7 C163 101.2(2) . . ? C29 P7 C91 104.8(2) . . ? C163 P7 C91 103.4(2) . . ? C29 P7 Cu1 113.48(17) . . ? C163 P7 Cu1 118.34(18) . . ? C91 P7 Cu1 113.92(18) . . ? C73 P10 C44 105.9(3) . . ? C73 P10 C3 106.3(3) . . ? C44 P10 C3 102.9(3) . . ? C73 P10 Cu1 118.6(2) . . ? C44 P10 Cu1 108.5(2) . . ? C3 P10 Cu1 113.26(18) . . ? C93 P12 C90 104.4(3) . . ? C93 P12 C3 103.6(3) . . ? C90 P12 C3 104.6(3) . . ? C93 P12 Cu3 122.6(2) . . ? C90 P12 Cu3 106.50(19) . . ? C3 P12 Cu3 113.45(19) . . ? # Attachment '- bgi02ls.CIF' data_a _database_code_depnum_ccdc_archive 'CCDC 768170' #TrackingRef '- bgi02ls.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C77 H64 Cl2 Cu2 N6 O6 P4' _chemical_formula_weight 1491.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.673(3) _cell_length_b 19.071(4) _cell_length_c 26.536(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.795(4) _cell_angle_gamma 90.00 _cell_volume 7374(3) _cell_formula_units_Z 4 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'deep orange' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 0.792 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8812 _exptl_absorpt_correction_T_max 0.9513 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 301(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40382 _diffrn_reflns_av_R_equivalents 0.1040 _diffrn_reflns_av_sigmaI/netI 0.1233 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12885 _reflns_number_gt 6513 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINTPLUS _computing_data_reduction SAINTPLUS _computing_structure_solution 'SHELXTL (Sheldrick, 1990)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0714P)^2^+35.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12885 _refine_ls_number_parameters 875 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1471 _refine_ls_R_factor_gt 0.1024 _refine_ls_wR_factor_ref 0.2649 _refine_ls_wR_factor_gt 0.2482 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.007 _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 0.74776(8) 0.69602(5) 0.11075(4) 0.0433(3) Uani 1 1 d . . . Cu2 Cu 0.59860(7) 0.78567(5) 0.02607(4) 0.0421(3) Uani 1 1 d . . . P1 P 0.72783(18) 0.77893(11) 0.16834(8) 0.0452(6) Uani 1 1 d . . . P2 P 0.65292(17) 0.60333(11) 0.09262(9) 0.0444(6) Uani 1 1 d . . . P3 P 0.51967(17) 0.68507(11) 0.01390(9) 0.0452(6) Uani 1 1 d . . . P4 P 0.60198(17) 0.86455(11) 0.08838(8) 0.0426(6) Uani 1 1 d . . . N1 N 0.8829(5) 0.6562(4) 0.1114(3) 0.051(2) Uani 1 1 d . . . N2 N 0.7853(4) 0.7268(3) 0.0409(2) 0.0361(16) Uani 1 1 d . . . N3 N 0.7253(5) 0.7633(3) 0.0086(2) 0.0365(16) Uani 1 1 d . . . N4 N 0.5967(6) 0.8305(3) -0.0473(3) 0.054(2) Uani 1 1 d . . . C1 C 0.9241(7) 0.6081(5) 0.1439(4) 0.063(3) Uani 1 1 d . . . H1A H 0.9015 0.6019 0.1749 0.075 Uiso 1 1 calc R . . C2 C 0.9972(7) 0.5678(5) 0.1338(4) 0.075(3) Uani 1 1 d . . . H2A H 1.0222 0.5343 0.1569 0.089 Uiso 1 1 calc R . . C3 C 1.0328(8) 0.5783(5) 0.0885(5) 0.080(4) Uani 1 1 d . . . H3A H 1.0824 0.5520 0.0804 0.096 Uiso 1 1 calc R . . C4 C 0.9933(7) 0.6282(5) 0.0559(4) 0.067(3) Uani 1 1 d . . . H4A H 1.0155 0.6350 0.0248 0.081 Uiso 1 1 calc R . . C5 C 0.9222(6) 0.6680(4) 0.0681(3) 0.045(2) Uani 1 1 d . . . C6 C 0.8700(6) 0.7194(4) 0.0331(3) 0.040(2) Uani 1 1 d . . . C7 C 0.9080(6) 0.7593(4) -0.0045(3) 0.048(2) Uani 1 1 d . . . C8 C 0.8483(6) 0.7955(4) -0.0389(3) 0.041(2) Uani 1 1 d . . . C9 C 0.7531(7) 0.7928(4) -0.0341(3) 0.051(3) Uani 1 1 d . . . C10 C 0.6756(6) 0.8223(4) -0.0677(3) 0.044(2) Uani 1 1 d . . . C11 C 0.6774(8) 0.8347(5) -0.1187(3) 0.065(3) Uani 1 1 d . . . H11A H 0.7316 0.8269 -0.1329 0.078 Uiso 1 1 calc R . . C12 C 0.6031(8) 0.8577(6) -0.1486(4) 0.070(3) Uani 1 1 d . . . H12A H 0.6061 0.8672 -0.1827 0.084 Uiso 1 1 calc R . . C13 C 0.5212(8) 0.8672(5) -0.1274(4) 0.068(3) Uani 1 1 d . . . H13A H 0.4674 0.8819 -0.1466 0.081 Uiso 1 1 calc R . . C14 C 0.5252(7) 0.8534(4) -0.0763(4) 0.053(2) Uani 1 1 d . . . H14A H 0.4721 0.8611 -0.0612 0.063 Uiso 1 1 calc R . . C15 C 1.0081(7) 0.7700(4) -0.0032(4) 0.050(2) Uani 1 1 d . . . C16 C 1.0551(8) 0.8117(6) 0.0354(5) 0.073(3) Uani 1 1 d . . . H16A H 1.0242 0.8298 0.0611 0.088 Uiso 1 1 calc R . . C17 C 1.1469(9) 0.8255(7) 0.0347(6) 0.095(4) Uani 1 1 d . . . H17A H 1.1759 0.8546 0.0598 0.115 Uiso 1 1 calc R . . C18 C 1.1969(8) 0.7996(8) 0.0001(6) 0.096(5) Uani 1 1 d . . . H18A H 1.2594 0.8087 0.0012 0.115 Uiso 1 1 calc R . . C19 C 1.1499(9) 0.7582(7) -0.0378(6) 0.092(4) Uani 1 1 d . . . H19A H 1.1816 0.7402 -0.0633 0.111 Uiso 1 1 calc R . . C20 C 1.0623(7) 0.7438(6) -0.0387(4) 0.071(3) Uani 1 1 d . . . H20A H 1.0350 0.7146 -0.0643 0.085 Uiso 1 1 calc R . . C21 C 0.8830(7) 0.8413(5) -0.0782(4) 0.059(3) Uani 1 1 d . . . C22 C 0.9067(9) 0.8116(7) -0.1232(4) 0.089(4) Uani 1 1 d . . . H22A H 0.9013 0.7637 -0.1291 0.107 Uiso 1 1 calc R . . C23 C 0.9387(11) 0.8566(11) -0.1587(6) 0.132(7) Uani 1 1 d . . . H23A H 0.9536 0.8384 -0.1892 0.158 Uiso 1 1 calc R . . C24 C 0.9487(10) 0.9273(11) -0.1493(7) 0.129(7) Uani 1 1 d . . . H24A H 0.9719 0.9561 -0.1731 0.154 Uiso 1 1 calc R . . C25 C 0.9251(10) 0.9550(8) -0.1061(7) 0.119(6) Uani 1 1 d . . . H25A H 0.9303 1.0031 -0.1008 0.143 Uiso 1 1 calc R . . C26 C 0.8929(7) 0.9126(6) -0.0692(5) 0.075(3) Uani 1 1 d . . . H26A H 0.8782 0.9320 -0.0390 0.090 Uiso 1 1 calc R . . C27 C 0.5915(6) 0.6057(4) 0.0282(3) 0.049(2) Uani 1 1 d . . . H27A H 0.5525 0.5646 0.0234 0.059 Uiso 1 1 calc R . . H27B H 0.6360 0.6029 0.0040 0.059 Uiso 1 1 calc R . . C28 C 0.6270(6) 0.8340(4) 0.1537(3) 0.045(2) Uani 1 1 d . . . H28A H 0.6340 0.8748 0.1757 0.054 Uiso 1 1 calc R . . H28B H 0.5741 0.8081 0.1623 0.054 Uiso 1 1 calc R . . C101 C 0.7064(6) 0.7433(4) 0.2302(3) 0.048(2) Uani 1 1 d . . . C102 C 0.7482(8) 0.6799(5) 0.2448(4) 0.071(3) Uani 1 1 d . . . H10A H 0.7874 0.6584 0.2245 0.085 Uiso 1 1 calc R . . C103 C 0.7306(9) 0.6487(6) 0.2905(4) 0.089(4) Uani 1 1 d . . . H10B H 0.7592 0.6068 0.3011 0.107 Uiso 1 1 calc R . . C104 C 0.6709(8) 0.6805(6) 0.3197(4) 0.074(3) Uani 1 1 d . . . H10C H 0.6575 0.6588 0.3493 0.088 Uiso 1 1 calc R . . C105 C 0.6305(8) 0.7437(5) 0.3057(4) 0.067(3) Uani 1 1 d . . . H10D H 0.5905 0.7648 0.3257 0.080 Uiso 1 1 calc R . . C106 C 0.6505(8) 0.7761(5) 0.2608(3) 0.063(3) Uani 1 1 d . . . H10E H 0.6257 0.8198 0.2517 0.076 Uiso 1 1 calc R . . C111 C 0.8218(8) 0.8385(4) 0.1857(3) 0.055(3) Uani 1 1 d . . . C112 C 0.9101(7) 0.8175(5) 0.1790(4) 0.069(3) Uani 1 1 d . . . H11B H 0.9183 0.7752 0.1627 0.082 Uiso 1 1 calc R . . C113 C 0.9858(9) 0.8571(7) 0.1955(5) 0.094(4) Uani 1 1 d . . . H11C H 1.0440 0.8414 0.1904 0.113 Uiso 1 1 calc R . . C114 C 0.9760(10) 0.9191(7) 0.2195(5) 0.087(4) Uani 1 1 d . . . H11D H 1.0276 0.9458 0.2306 0.104 Uiso 1 1 calc R . . C115 C 0.8935(11) 0.9419(6) 0.2271(4) 0.083(4) Uani 1 1 d . . . H11E H 0.8884 0.9842 0.2440 0.099 Uiso 1 1 calc R . . C116 C 0.8142(8) 0.9043(5) 0.2105(4) 0.064(3) Uani 1 1 d . . . H11F H 0.7568 0.9219 0.2156 0.077 Uiso 1 1 calc R . . C201 C 0.7237(7) 0.5254(4) 0.0934(4) 0.052(2) Uani 1 1 d . . . C202 C 0.7446(8) 0.4891(5) 0.1389(4) 0.079(3) Uani 1 1 d . . . H20B H 0.7134 0.4995 0.1665 0.095 Uiso 1 1 calc R . . C203 C 0.8118(9) 0.4378(6) 0.1432(5) 0.090(4) Uani 1 1 d . . . H20C H 0.8237 0.4128 0.1733 0.108 Uiso 1 1 calc R . . C204 C 0.8609(8) 0.4232(6) 0.1037(6) 0.087(4) Uani 1 1 d . . . H20D H 0.9085 0.3908 0.1076 0.104 Uiso 1 1 calc R . . C205 C 0.8391(9) 0.4568(7) 0.0589(5) 0.095(4) Uani 1 1 d . . . H20E H 0.8694 0.4453 0.0311 0.114 Uiso 1 1 calc R . . C206 C 0.7716(7) 0.5082(5) 0.0544(4) 0.063(3) Uani 1 1 d . . . H20F H 0.7588 0.5317 0.0236 0.076 Uiso 1 1 calc R . . C211 C 0.5639(6) 0.5796(4) 0.1320(3) 0.050(2) Uani 1 1 d . . . C212 C 0.5366(8) 0.6279(5) 0.1669(4) 0.070(3) Uani 1 1 d . . . H21A H 0.5670 0.6707 0.1709 0.084 Uiso 1 1 calc R . . C213 C 0.4689(9) 0.6148(7) 0.1945(4) 0.085(4) Uani 1 1 d . . . H21B H 0.4547 0.6470 0.2187 0.101 Uiso 1 1 calc R . . C214 C 0.4196(10) 0.5536(7) 0.1871(5) 0.099(5) Uani 1 1 d . . . H21C H 0.3703 0.5451 0.2053 0.119 Uiso 1 1 calc R . . C215 C 0.4432(10) 0.5053(6) 0.1529(5) 0.101(5) Uani 1 1 d . . . H21D H 0.4107 0.4634 0.1484 0.121 Uiso 1 1 calc R . . C216 C 0.5137(8) 0.5181(5) 0.1258(4) 0.075(3) Uani 1 1 d . . . H21E H 0.5289 0.4849 0.1026 0.091 Uiso 1 1 calc R . . C301 C 0.4801(8) 0.6768(4) -0.0534(4) 0.060(3) Uani 1 1 d . . . C302 C 0.3920(9) 0.6865(5) -0.0732(5) 0.078(3) Uani 1 1 d . . . H30A H 0.3476 0.6900 -0.0511 0.093 Uiso 1 1 calc R . . C303 C 0.3640(10) 0.6917(6) -0.1254(5) 0.090(4) Uani 1 1 d . . . H30B H 0.3027 0.6985 -0.1379 0.108 Uiso 1 1 calc R . . C304 C 0.4317(13) 0.6861(6) -0.1577(5) 0.095(4) Uani 1 1 d . . . H30C H 0.4158 0.6902 -0.1926 0.113 Uiso 1 1 calc R . . C305 C 0.5182(10) 0.6751(5) -0.1396(4) 0.074(3) Uani 1 1 d . . . H30D H 0.5621 0.6707 -0.1620 0.089 Uiso 1 1 calc R . . C306 C 0.5455(7) 0.6699(4) -0.0871(4) 0.054(2) Uani 1 1 d . . . H30E H 0.6067 0.6619 -0.0750 0.064 Uiso 1 1 calc R . . C311 C 0.4196(8) 0.6720(5) 0.0454(4) 0.062(3) Uani 1 1 d . . . C312 C 0.3606(8) 0.6131(6) 0.0396(5) 0.079(3) Uani 1 1 d . . . H31A H 0.3726 0.5777 0.0172 0.095 Uiso 1 1 calc R . . C313 C 0.2860(9) 0.6066(7) 0.0664(5) 0.096(4) Uani 1 1 d . . . H31B H 0.2512 0.5657 0.0638 0.115 Uiso 1 1 calc R . . C314 C 0.2633(9) 0.6601(8) 0.0966(5) 0.091(4) Uani 1 1 d . . . H31C H 0.2110 0.6568 0.1131 0.109 Uiso 1 1 calc R . . C315 C 0.3170(9) 0.7181(7) 0.1027(5) 0.090(4) Uani 1 1 d . . . H31D H 0.3032 0.7534 0.1247 0.108 Uiso 1 1 calc R . . C316 C 0.3914(8) 0.7248(5) 0.0765(4) 0.067(3) Uani 1 1 d . . . H31E H 0.4248 0.7663 0.0796 0.080 Uiso 1 1 calc R . . C401 C 0.4927(7) 0.9091(4) 0.0892(3) 0.047(2) Uani 1 1 d . . . C402 C 0.4480(7) 0.9157(5) 0.1321(4) 0.065(3) Uani 1 1 d . . . H40A H 0.4751 0.8982 0.1630 0.078 Uiso 1 1 calc R . . C403 C 0.3623(8) 0.9486(6) 0.1291(5) 0.081(3) Uani 1 1 d . . . H40B H 0.3324 0.9520 0.1580 0.097 Uiso 1 1 calc R . . C404 C 0.3221(8) 0.9757(5) 0.0844(5) 0.074(3) Uani 1 1 d . . . H40C H 0.2649 0.9971 0.0825 0.089 Uiso 1 1 calc R . . C405 C 0.3685(7) 0.9707(5) 0.0415(4) 0.066(3) Uani 1 1 d . . . H40D H 0.3431 0.9906 0.0111 0.079 Uiso 1 1 calc R . . C406 C 0.4495(8) 0.9372(5) 0.0439(4) 0.062(3) Uani 1 1 d . . . H40E H 0.4777 0.9326 0.0145 0.074 Uiso 1 1 calc R . . C411 C 0.6832(6) 0.9349(4) 0.0848(3) 0.045(2) Uani 1 1 d . . . C412 C 0.7698(6) 0.9204(5) 0.0718(3) 0.050(2) Uani 1 1 d . . . H41A H 0.7836 0.8743 0.0642 0.060 Uiso 1 1 calc R . . C413 C 0.8378(8) 0.9712(5) 0.0693(4) 0.068(3) Uani 1 1 d . . . H41B H 0.8963 0.9593 0.0621 0.082 Uiso 1 1 calc R . . C414 C 0.8141(9) 1.0403(5) 0.0781(4) 0.073(3) Uani 1 1 d . . . H41C H 0.8561 1.0761 0.0751 0.088 Uiso 1 1 calc R . . C415 C 0.7273(8) 1.0560(5) 0.0915(4) 0.068(3) Uani 1 1 d . . . H41D H 0.7118 1.1023 0.0974 0.082 Uiso 1 1 calc R . . C416 C 0.6657(7) 1.0049(4) 0.0959(3) 0.054(2) Uani 1 1 d . . . H41E H 0.6096 1.0164 0.1067 0.065 Uiso 1 1 calc R . . C1S C 0.346(2) 0.8846(14) 0.2788(9) 0.262(16) Uani 1 1 d . . . H1SA H 0.3936 0.9189 0.2748 0.315 Uiso 1 1 calc R . . H1SB H 0.3452 0.8768 0.3148 0.315 Uiso 1 1 calc R . . Cl1 Cl 0.3728(9) 0.8107(5) 0.2523(4) 0.309(6) Uani 1 1 d . . . Cl2 Cl 0.2434(6) 0.9179(7) 0.2542(4) 0.335(6) Uani 1 1 d . . . N5 N 0.5616(11) 1.0028(7) 0.2363(4) 0.092(3) Uani 1 1 d . . . N6 N 0.8179(10) 0.6212(10) 0.9179(5) 0.226(7) Uani 1 1 d DU . . O1 O 0.6298(12) 1.0116(10) 0.2185(7) 0.247(10) Uani 1 1 d . . . O2 O 0.5528(11) 0.9415(7) 0.2464(4) 0.170(6) Uani 1 1 d . . . O3 O 0.5136(12) 1.0476(8) 0.2404(4) 0.227(10) Uani 1 1 d . . . O4 O 0.7797(13) 0.6576(11) 0.8883(5) 0.280(8) Uani 1 1 d DU . . O5 O 0.8945(10) 0.6187(11) 0.9197(6) 0.246(7) Uani 1 1 d DU . . O6 O 0.7830(11) 0.6110(9) 0.9525(5) 0.230(6) Uani 1 1 d DU . . 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 0.0538(7) 0.0358(6) 0.0432(6) 0.0018(4) 0.0181(5) 0.0019(5) Cu2 0.0493(7) 0.0379(6) 0.0416(6) -0.0026(4) 0.0156(5) 0.0017(5) P1 0.0665(17) 0.0319(11) 0.0399(12) 0.0005(9) 0.0183(12) 0.0000(11) P2 0.0561(16) 0.0325(11) 0.0470(13) 0.0006(10) 0.0160(12) 0.0012(10) P3 0.0504(15) 0.0394(12) 0.0483(13) -0.0040(10) 0.0163(12) 0.0003(11) P4 0.0589(16) 0.0332(11) 0.0380(12) -0.0002(9) 0.0152(12) 0.0021(11) N1 0.060(5) 0.043(4) 0.056(5) 0.008(4) 0.024(4) 0.010(4) N2 0.028(4) 0.043(4) 0.040(4) 0.004(3) 0.011(3) 0.012(3) N3 0.039(4) 0.035(4) 0.036(4) 0.000(3) 0.008(3) 0.005(3) N4 0.091(7) 0.033(4) 0.039(4) 0.000(3) 0.019(5) -0.002(4) C1 0.066(7) 0.064(6) 0.059(6) 0.018(5) 0.011(6) 0.007(6) C2 0.058(7) 0.071(7) 0.096(9) 0.036(6) 0.016(7) 0.027(6) C3 0.075(8) 0.063(7) 0.110(9) 0.032(6) 0.039(7) 0.040(6) C4 0.071(7) 0.056(6) 0.082(7) 0.017(5) 0.040(6) 0.021(5) C5 0.048(6) 0.037(5) 0.051(5) 0.010(4) 0.011(5) 0.008(4) C6 0.035(5) 0.041(5) 0.047(5) 0.001(4) 0.016(4) 0.002(4) C7 0.055(6) 0.038(5) 0.055(5) 0.005(4) 0.026(5) 0.006(4) C8 0.037(5) 0.046(5) 0.042(5) 0.003(4) 0.013(4) 0.004(4) C9 0.086(8) 0.028(4) 0.044(5) -0.005(4) 0.030(5) -0.012(4) C10 0.054(6) 0.040(5) 0.038(5) 0.005(4) 0.006(5) 0.008(4) C11 0.079(8) 0.079(7) 0.041(5) 0.014(5) 0.018(6) 0.017(6) C12 0.083(9) 0.087(8) 0.038(5) 0.010(5) 0.001(6) -0.004(7) C13 0.094(9) 0.055(6) 0.053(6) 0.007(5) 0.007(6) 0.021(6) C14 0.066(7) 0.043(5) 0.049(6) 0.002(4) 0.005(5) 0.014(5) C15 0.053(6) 0.045(5) 0.055(6) 0.013(4) 0.020(5) 0.003(4) C16 0.061(7) 0.071(7) 0.090(8) 0.016(6) 0.021(7) 0.011(6) C17 0.064(9) 0.092(9) 0.128(12) 0.001(8) 0.007(9) -0.021(7) C18 0.040(7) 0.107(10) 0.144(13) 0.066(10) 0.026(9) 0.001(7) C19 0.064(9) 0.119(11) 0.104(10) 0.038(9) 0.051(8) 0.014(8) C20 0.054(7) 0.089(8) 0.076(7) 0.012(6) 0.034(6) 0.007(6) C21 0.050(6) 0.068(7) 0.065(6) 0.021(5) 0.030(5) 0.009(5) C22 0.100(10) 0.108(9) 0.069(7) 0.026(7) 0.046(7) 0.015(8) C23 0.117(13) 0.199(18) 0.095(10) 0.076(12) 0.077(10) 0.064(13) C24 0.088(11) 0.152(15) 0.159(17) 0.090(14) 0.068(11) 0.022(11) C25 0.092(11) 0.097(10) 0.174(16) 0.073(11) 0.035(11) 0.009(8) C26 0.059(7) 0.069(7) 0.100(9) 0.031(6) 0.025(7) -0.005(6) C27 0.051(6) 0.037(5) 0.061(6) -0.006(4) 0.017(5) 0.001(4) C28 0.051(6) 0.043(5) 0.039(5) -0.003(4) 0.000(4) -0.009(4) C101 0.064(6) 0.041(5) 0.044(5) 0.005(4) 0.021(5) -0.009(4) C102 0.096(9) 0.060(6) 0.061(6) 0.021(5) 0.031(6) 0.037(6) C103 0.139(12) 0.066(7) 0.067(7) 0.030(6) 0.036(8) 0.031(7) C104 0.091(9) 0.073(7) 0.061(7) 0.020(6) 0.024(7) 0.005(6) C105 0.085(8) 0.071(7) 0.050(6) 0.008(5) 0.034(6) 0.010(6) C106 0.103(9) 0.047(5) 0.044(5) 0.004(4) 0.023(6) 0.004(5) C111 0.088(8) 0.040(5) 0.039(5) 0.010(4) 0.015(5) 0.000(5) C112 0.040(6) 0.065(6) 0.101(9) -0.024(6) 0.007(6) -0.018(5) C113 0.065(8) 0.086(9) 0.135(12) -0.015(8) 0.028(8) -0.018(7) C114 0.085(10) 0.086(9) 0.086(9) 0.008(7) -0.005(8) -0.038(8) C115 0.121(12) 0.052(7) 0.075(8) -0.009(6) 0.011(8) -0.026(8) C116 0.070(7) 0.055(6) 0.066(7) -0.002(5) 0.005(6) -0.010(5) C201 0.056(6) 0.036(5) 0.065(6) -0.002(4) 0.010(5) -0.006(4) C202 0.103(10) 0.052(6) 0.085(8) 0.014(6) 0.025(7) 0.016(6) C203 0.107(10) 0.057(7) 0.101(10) 0.030(7) -0.007(9) 0.022(7) C204 0.066(8) 0.068(8) 0.121(11) -0.020(8) -0.011(8) 0.029(6) C205 0.104(11) 0.090(9) 0.094(10) -0.023(8) 0.023(9) 0.041(8) C206 0.067(7) 0.061(6) 0.063(6) -0.004(5) 0.010(6) 0.016(5) C211 0.058(6) 0.041(5) 0.052(5) 0.003(4) 0.018(5) 0.000(4) C212 0.094(9) 0.064(7) 0.057(6) -0.008(5) 0.028(6) -0.014(6) C213 0.094(10) 0.091(9) 0.078(8) -0.007(7) 0.050(8) 0.003(7) C214 0.121(12) 0.096(10) 0.093(9) 0.041(8) 0.063(9) 0.021(9) C215 0.121(11) 0.061(7) 0.135(12) 0.012(7) 0.071(10) -0.014(7) C216 0.092(9) 0.047(6) 0.096(8) -0.003(6) 0.047(7) -0.010(6) C301 0.078(8) 0.036(5) 0.071(7) -0.010(5) 0.026(7) -0.011(5) C302 0.090(10) 0.071(7) 0.074(8) -0.010(6) 0.018(7) 0.011(7) C303 0.101(11) 0.088(9) 0.075(9) 0.000(7) -0.020(8) 0.000(8) C304 0.149(15) 0.077(8) 0.051(7) -0.006(6) -0.014(9) -0.024(9) C305 0.113(11) 0.057(7) 0.050(7) -0.014(5) 0.003(7) -0.008(7) C306 0.045(6) 0.047(5) 0.068(7) -0.005(5) 0.004(5) 0.000(4) C311 0.082(8) 0.050(6) 0.057(6) 0.001(5) 0.016(6) -0.010(5) C312 0.078(8) 0.070(7) 0.096(9) -0.006(6) 0.031(7) -0.020(6) C313 0.084(10) 0.092(10) 0.116(11) 0.028(8) 0.028(9) -0.028(8) C314 0.064(8) 0.129(12) 0.085(9) 0.019(9) 0.027(7) 0.002(8) C315 0.082(9) 0.114(10) 0.081(8) -0.008(7) 0.040(8) 0.004(8) C316 0.083(8) 0.058(6) 0.065(6) 0.002(5) 0.031(6) 0.006(6) C401 0.066(6) 0.033(4) 0.047(5) -0.003(4) 0.019(5) 0.003(4) C402 0.065(7) 0.074(7) 0.059(6) 0.007(5) 0.017(6) 0.030(6) C403 0.079(9) 0.092(8) 0.078(8) 0.009(7) 0.037(7) 0.028(7) C404 0.055(7) 0.066(7) 0.102(9) 0.009(6) 0.016(7) 0.020(6) C405 0.065(7) 0.065(7) 0.066(7) 0.002(5) -0.001(6) 0.014(6) C406 0.080(8) 0.058(6) 0.051(6) -0.001(5) 0.020(6) 0.012(6) C411 0.060(6) 0.039(5) 0.038(5) 0.009(4) 0.012(5) 0.013(4) C412 0.043(6) 0.044(5) 0.061(6) -0.012(4) 0.004(5) -0.012(4) C413 0.074(8) 0.065(7) 0.069(7) -0.006(5) 0.025(6) -0.010(6) C414 0.112(10) 0.050(6) 0.057(6) -0.003(5) 0.007(7) -0.022(6) C415 0.091(9) 0.034(5) 0.079(7) -0.011(5) 0.003(7) -0.014(6) C416 0.061(6) 0.044(5) 0.057(6) -0.008(4) 0.004(5) 0.005(5) C1S 0.39(5) 0.22(3) 0.19(2) 0.00(2) 0.05(3) 0.16(3) Cl1 0.474(17) 0.219(8) 0.259(9) 0.035(7) 0.143(11) 0.040(9) Cl2 0.208(8) 0.506(17) 0.308(11) 0.039(11) 0.099(8) 0.142(10) N5 0.139(12) 0.080(8) 0.055(6) 0.005(6) 0.003(7) -0.001(8) N6 0.268(16) 0.303(14) 0.095(10) 0.005(11) -0.021(11) 0.012(15) O1 0.170(14) 0.31(2) 0.27(2) 0.076(17) 0.091(15) -0.058(15) O2 0.275(18) 0.119(9) 0.109(8) 0.013(7) -0.006(10) -0.018(10) O3 0.34(2) 0.250(15) 0.084(7) -0.022(8) -0.009(10) 0.232(17) O4 0.350(18) 0.339(19) 0.144(12) 0.036(11) 0.002(13) 0.054(16) O5 0.261(17) 0.294(15) 0.180(12) -0.077(11) 0.008(12) 0.042(15) O6 0.283(15) 0.273(14) 0.124(10) 0.026(11) -0.014(10) -0.095(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 N2 2.079(6) . ? Cu1 N1 2.122(7) . ? Cu1 P1 2.242(2) . ? Cu1 P2 2.266(3) . ? Cu2 N3 2.014(6) . ? Cu2 N4 2.124(7) . ? Cu2 P4 2.232(2) . ? Cu2 P3 2.244(2) . ? P1 C111 1.803(10) . ? P1 C28 1.818(9) . ? P1 C101 1.838(8) . ? P2 C201 1.812(9) . ? P2 C211 1.824(9) . ? P2 C27 1.836(9) . ? P3 C311 1.790(10) . ? P3 C301 1.819(11) . ? P3 C27 1.858(8) . ? P4 C411 1.804(9) . ? P4 C401 1.817(9) . ? P4 C28 1.825(8) . ? N1 C1 1.351(11) . ? N1 C5 1.364(10) . ? N2 C6 1.292(9) . ? N2 N3 1.347(8) . ? N3 C9 1.371(9) . ? N4 C14 1.302(12) . ? N4 C10 1.343(11) . ? C1 C2 1.371(13) . ? C1 H1A 0.9300 . ? C2 C3 1.380(14) . ? C2 H2A 0.9300 . ? C3 C4 1.369(13) . ? C3 H3A 0.9300 . ? C4 C5 1.360(12) . ? C4 H4A 0.9300 . ? C5 C6 1.498(11) . ? C6 C7 1.419(11) . ? C7 C8 1.375(12) . ? C7 C15 1.480(13) . ? C8 C9 1.419(12) . ? C8 C21 1.493(11) . ? C9 C10 1.472(13) . ? C10 C11 1.376(11) . ? C11 C12 1.344(14) . ? C11 H11A 0.9300 . ? C12 C13 1.397(14) . ? C12 H12A 0.9300 . ? C13 C14 1.376(13) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C20 1.397(12) . ? C15 C16 1.409(14) . ? C16 C17 1.374(16) . ? C16 H16A 0.9300 . ? C17 C18 1.336(17) . ? C17 H17A 0.9300 . ? C18 C19 1.395(18) . ? C18 H18A 0.9300 . ? C19 C20 1.311(16) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C26 1.386(14) . ? C21 C22 1.402(14) . ? C22 C23 1.397(17) . ? C22 H22A 0.9300 . ? C23 C24 1.38(2) . ? C23 H23A 0.9300 . ? C24 C25 1.34(2) . ? C24 H24A 0.9300 . ? C25 C26 1.396(16) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C101 C106 1.372(12) . ? C101 C102 1.388(12) . ? C102 C103 1.403(13) . ? C102 H10A 0.9300 . ? C103 C104 1.376(14) . ? C103 H10B 0.9300 . ? C104 C105 1.375(13) . ? C104 H10C 0.9300 . ? C105 C106 1.403(12) . ? C105 H10D 0.9300 . ? C106 H10E 0.9300 . ? C111 C112 1.388(13) . ? C111 C116 1.429(12) . ? C112 C113 1.371(15) . ? C112 H11B 0.9300 . ? C113 C114 1.359(16) . ? C113 H11C 0.9300 . ? C114 C115 1.324(16) . ? C114 H11D 0.9300 . ? C115 C116 1.394(15) . ? C115 H11E 0.9300 . ? C116 H11F 0.9300 . ? C201 C206 1.358(12) . ? C201 C202 1.396(14) . ? C202 C203 1.384(15) . ? C202 H20B 0.9300 . ? C203 C204 1.368(16) . ? C203 H20C 0.9300 . ? C204 C205 1.355(17) . ? C204 H20D 0.9300 . ? C205 C206 1.389(15) . ? C205 H20E 0.9300 . ? C206 H20F 0.9300 . ? C211 C216 1.384(13) . ? C211 C212 1.398(12) . ? C212 C213 1.326(14) . ? C212 H21A 0.9300 . ? C213 C214 1.376(17) . ? C213 H21B 0.9300 . ? C214 C215 1.365(16) . ? C214 H21C 0.9300 . ? C215 C216 1.350(14) . ? C215 H21D 0.9300 . ? C216 H21E 0.9300 . ? C301 C302 1.349(15) . ? C301 C306 1.394(12) . ? C302 C303 1.399(16) . ? C302 H30A 0.9300 . ? C303 C304 1.392(18) . ? C303 H30B 0.9300 . ? C304 C305 1.320(17) . ? C304 H30C 0.9300 . ? C305 C306 1.407(14) . ? C305 H30D 0.9300 . ? C306 H30E 0.9300 . ? C311 C316 1.395(13) . ? C311 C312 1.415(13) . ? C312 C313 1.379(15) . ? C312 H31A 0.9300 . ? C313 C314 1.364(17) . ? C313 H31B 0.9300 . ? C314 C315 1.357(17) . ? C314 H31C 0.9300 . ? C315 C316 1.368(14) . ? C315 H31D 0.9300 . ? C316 H31E 0.9300 . ? C401 C402 1.385(11) . ? C401 C406 1.397(13) . ? C402 C403 1.400(14) . ? C402 H40A 0.9300 . ? C403 C404 1.362(15) . ? C403 H40B 0.9300 . ? C404 C405 1.397(14) . ? C404 H40C 0.9300 . ? C405 C406 1.345(13) . ? C405 H40D 0.9300 . ? C406 H40E 0.9300 . ? C411 C412 1.384(12) . ? C411 C416 1.398(11) . ? C412 C413 1.397(12) . ? C412 H41A 0.9300 . ? C413 C414 1.391(14) . ? C413 H41B 0.9300 . ? C414 C415 1.394(15) . ? C414 H41C 0.9300 . ? C415 C416 1.344(13) . ? C415 H41D 0.9300 . ? C416 H41E 0.9300 . ? C1S Cl1 1.64(2) . ? C1S Cl2 1.69(3) . ? C1S H1SA 0.9700 . ? C1S H1SB 0.9700 . ? N5 O3 1.119(14) . ? N5 O1 1.168(16) . ? N5 O2 1.211(13) . ? N6 O6 1.119(7) . ? N6 O5 1.122(7) . ? N6 O4 1.144(8) . ? 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 N2 Cu1 N1 76.3(3) . . ? N2 Cu1 P1 118.56(18) . . ? N1 Cu1 P1 116.3(2) . . ? N2 Cu1 P2 104.59(19) . . ? N1 Cu1 P2 105.8(2) . . ? P1 Cu1 P2 124.65(9) . . ? N3 Cu2 N4 77.7(3) . . ? N3 Cu2 P4 111.9(2) . . ? N4 Cu2 P4 113.90(19) . . ? N3 Cu2 P3 105.09(19) . . ? N4 Cu2 P3 105.2(2) . . ? P4 Cu2 P3 130.44(9) . . ? C111 P1 C28 105.6(4) . . ? C111 P1 C101 102.2(4) . . ? C28 P1 C101 100.6(4) . . ? C111 P1 Cu1 117.4(3) . . ? C28 P1 Cu1 115.5(3) . . ? C101 P1 Cu1 113.4(3) . . ? C201 P2 C211 103.8(4) . . ? C201 P2 C27 104.3(4) . . ? C211 P2 C27 103.5(4) . . ? C201 P2 Cu1 107.5(3) . . ? C211 P2 Cu1 122.4(3) . . ? C27 P2 Cu1 113.6(3) . . ? C311 P3 C301 105.1(5) . . ? C311 P3 C27 105.6(4) . . ? C301 P3 C27 103.7(4) . . ? C311 P3 Cu2 119.3(3) . . ? C301 P3 Cu2 108.4(3) . . ? C27 P3 Cu2 113.4(3) . . ? C411 P4 C401 104.0(4) . . ? C411 P4 C28 103.2(4) . . ? C401 P4 C28 102.5(4) . . ? C411 P4 Cu2 114.8(3) . . ? C401 P4 Cu2 112.4(3) . . ? C28 P4 Cu2 118.2(3) . . ? C1 N1 C5 116.6(7) . . ? C1 N1 Cu1 126.6(6) . . ? C5 N1 Cu1 114.9(6) . . ? C6 N2 N3 121.6(6) . . ? C6 N2 Cu1 118.3(6) . . ? N3 N2 Cu1 119.3(4) . . ? N2 N3 C9 120.1(7) . . ? N2 N3 Cu2 121.0(4) . . ? C9 N3 Cu2 118.4(6) . . ? C14 N4 C10 118.3(8) . . ? C14 N4 Cu2 126.8(7) . . ? C10 N4 Cu2 113.9(6) . . ? N1 C1 C2 123.9(9) . . ? N1 C1 H1A 118.0 . . ? C2 C1 H1A 118.0 . . ? C1 C2 C3 118.2(9) . . ? C1 C2 H2A 120.9 . . ? C3 C2 H2A 120.9 . . ? C4 C3 C2 118.5(9) . . ? C4 C3 H3A 120.7 . . ? C2 C3 H3A 120.7 . . ? C5 C4 C3 121.0(9) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 N1 121.5(8) . . ? C4 C5 C6 124.5(8) . . ? N1 C5 C6 113.2(7) . . ? N2 C6 C7 121.3(8) . . ? N2 C6 C5 113.8(7) . . ? C7 C6 C5 125.0(7) . . ? C8 C7 C6 117.7(8) . . ? C8 C7 C15 119.9(7) . . ? C6 C7 C15 121.9(8) . . ? C7 C8 C9 118.6(7) . . ? C7 C8 C21 120.9(8) . . ? C9 C8 C21 120.3(8) . . ? N3 C9 C8 118.8(9) . . ? N3 C9 C10 112.0(8) . . ? C8 C9 C10 129.0(7) . . ? N4 C10 C11 119.6(9) . . ? N4 C10 C9 116.1(7) . . ? C11 C10 C9 123.9(8) . . ? C12 C11 C10 121.8(10) . . ? C12 C11 H11A 119.1 . . ? C10 C11 H11A 119.1 . . ? C11 C12 C13 118.9(9) . . ? C11 C12 H12A 120.6 . . ? C13 C12 H12A 120.6 . . ? C14 C13 C12 115.6(10) . . ? C14 C13 H13A 122.2 . . ? C12 C13 H13A 122.2 . . ? N4 C14 C13 125.7(10) . . ? N4 C14 H14A 117.1 . . ? C13 C14 H14A 117.1 . . ? C20 C15 C16 115.0(9) . . ? C20 C15 C7 125.4(10) . . ? C16 C15 C7 119.6(8) . . ? C17 C16 C15 119.7(11) . . ? C17 C16 H16A 120.2 . . ? C15 C16 H16A 120.2 . . ? C18 C17 C16 123.8(14) . . ? C18 C17 H17A 118.1 . . ? C16 C17 H17A 118.1 . . ? C17 C18 C19 116.1(11) . . ? C17 C18 H18A 122.0 . . ? C19 C18 H18A 122.0 . . ? C20 C19 C18 122.1(12) . . ? C20 C19 H19A 118.9 . . ? C18 C19 H19A 118.9 . . ? C19 C20 C15 123.2(12) . . ? C19 C20 H20A 118.4 . . ? C15 C20 H20A 118.4 . . ? C26 C21 C22 120.7(9) . . ? C26 C21 C8 119.4(9) . . ? C22 C21 C8 119.9(9) . . ? C23 C22 C21 117.7(13) . . ? C23 C22 H22A 121.1 . . ? C21 C22 H22A 121.1 . . ? C24 C23 C22 121.1(15) . . ? C24 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? C25 C24 C23 120.5(13) . . ? C25 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? C24 C25 C26 120.9(15) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C21 C26 C25 119.0(13) . . ? C21 C26 H26A 120.5 . . ? C25 C26 H26A 120.5 . . ? P2 C27 P3 114.5(4) . . ? P2 C27 H27A 108.6 . . ? P3 C27 H27A 108.6 . . ? P2 C27 H27B 108.6 . . ? P3 C27 H27B 108.6 . . ? H27A C27 H27B 107.6 . . ? P1 C28 P4 117.0(5) . . ? P1 C28 H28A 108.0 . . ? P4 C28 H28A 108.0 . . ? P1 C28 H28B 108.0 . . ? P4 C28 H28B 108.0 . . ? H28A C28 H28B 107.3 . . ? C106 C101 C102 120.4(8) . . ? C106 C101 P1 122.5(7) . . ? C102 C101 P1 117.1(7) . . ? C101 C102 C103 119.4(9) . . ? C101 C102 H10A 120.3 . . ? C103 C102 H10A 120.3 . . ? C104 C103 C102 119.5(10) . . ? C104 C103 H10B 120.2 . . ? C102 C103 H10B 120.2 . . ? C103 C104 C105 121.1(9) . . ? C103 C104 H10C 119.4 . . ? C105 C104 H10C 119.4 . . ? C104 C105 C106 119.3(9) . . ? C104 C105 H10D 120.4 . . ? C106 C105 H10D 120.4 . . ? C101 C106 C105 120.1(9) . . ? C101 C106 H10E 120.0 . . ? C105 C106 H10E 120.0 . . ? C112 C111 C116 115.9(9) . . ? C112 C111 P1 118.9(7) . . ? C116 C111 P1 124.9(8) . . ? C113 C112 C111 122.2(10) . . ? C113 C112 H11B 118.9 . . ? C111 C112 H11B 118.9 . . ? C114 C113 C112 120.2(12) . . ? C114 C113 H11C 119.9 . . ? C112 C113 H11C 119.9 . . ? C115 C114 C113 120.4(12) . . ? C115 C114 H11D 119.8 . . ? C113 C114 H11D 119.8 . . ? C114 C115 C116 121.8(11) . . ? C114 C115 H11E 119.1 . . ? C116 C115 H11E 119.1 . . ? C115 C116 C111 119.3(11) . . ? C115 C116 H11F 120.3 . . ? C111 C116 H11F 120.3 . . ? C206 C201 C202 117.4(9) . . ? C206 C201 P2 122.5(7) . . ? C202 C201 P2 118.9(7) . . ? C203 C202 C201 120.2(11) . . ? C203 C202 H20B 119.9 . . ? C201 C202 H20B 119.9 . . ? C204 C203 C202 121.0(11) . . ? C204 C203 H20C 119.5 . . ? C202 C203 H20C 119.5 . . ? C205 C204 C203 119.0(11) . . ? C205 C204 H20D 120.5 . . ? C203 C204 H20D 120.5 . . ? C204 C205 C206 120.1(11) . . ? C204 C205 H20E 120.0 . . ? C206 C205 H20E 120.0 . . ? C201 C206 C205 122.1(11) . . ? C201 C206 H20F 118.9 . . ? C205 C206 H20F 118.9 . . ? C216 C211 C212 116.6(9) . . ? C216 C211 P2 123.3(7) . . ? C212 C211 P2 119.7(7) . . ? C213 C212 C211 122.2(10) . . ? C213 C212 H21A 118.9 . . ? C211 C212 H21A 118.9 . . ? C212 C213 C214 119.8(11) . . ? C212 C213 H21B 120.1 . . ? C214 C213 H21B 120.1 . . ? C215 C214 C213 119.8(11) . . ? C215 C214 H21C 120.1 . . ? C213 C214 H21C 120.1 . . ? C216 C215 C214 120.2(12) . . ? C216 C215 H21D 119.9 . . ? C214 C215 H21D 119.9 . . ? C215 C216 C211 121.3(10) . . ? C215 C216 H21E 119.3 . . ? C211 C216 H21E 119.3 . . ? C302 C301 C306 117.6(10) . . ? C302 C301 P3 123.4(8) . . ? C306 C301 P3 118.3(9) . . ? C301 C302 C303 123.5(12) . . ? C301 C302 H30A 118.3 . . ? C303 C302 H30A 118.3 . . ? C304 C303 C302 117.2(13) . . ? C304 C303 H30B 121.4 . . ? C302 C303 H30B 121.4 . . ? C305 C304 C303 120.9(12) . . ? C305 C304 H30C 119.5 . . ? C303 C304 H30C 119.5 . . ? C304 C305 C306 121.3(12) . . ? C304 C305 H30D 119.3 . . ? C306 C305 H30D 119.3 . . ? C301 C306 C305 119.5(10) . . ? C301 C306 H30E 120.3 . . ? C305 C306 H30E 120.3 . . ? C316 C311 C312 114.6(10) . . ? C316 C311 P3 119.5(8) . . ? C312 C311 P3 125.8(8) . . ? C313 C312 C311 121.9(11) . . ? C313 C312 H31A 119.0 . . ? C311 C312 H31A 119.0 . . ? C314 C313 C312 120.0(12) . . ? C314 C313 H31B 120.0 . . ? C312 C313 H31B 120.0 . . ? C315 C314 C313 120.1(12) . . ? C315 C314 H31C 120.0 . . ? C313 C314 H31C 120.0 . . ? C314 C315 C316 120.2(12) . . ? C314 C315 H31D 119.9 . . ? C316 C315 H31D 119.9 . . ? C315 C316 C311 122.9(11) . . ? C315 C316 H31E 118.5 . . ? C311 C316 H31E 118.5 . . ? C402 C401 C406 117.5(9) . . ? C402 C401 P4 123.8(7) . . ? C406 C401 P4 118.7(7) . . ? C401 C402 C403 120.3(10) . . ? C401 C402 H40A 119.9 . . ? C403 C402 H40A 119.9 . . ? C404 C403 C402 120.8(10) . . ? C404 C403 H40B 119.6 . . ? C402 C403 H40B 119.6 . . ? C403 C404 C405 118.8(10) . . ? C403 C404 H40C 120.6 . . ? C405 C404 H40C 120.6 . . ? C406 C405 C404 120.4(10) . . ? C406 C405 H40D 119.8 . . ? C404 C405 H40D 119.8 . . ? C405 C406 C401 122.1(9) . . ? C405 C406 H40E 118.9 . . ? C401 C406 H40E 118.9 . . ? C412 C411 C416 116.1(8) . . ? C412 C411 P4 119.8(6) . . ? C416 C411 P4 124.1(7) . . ? C411 C412 C413 123.8(9) . . ? C411 C412 H41A 118.1 . . ? C413 C412 H41A 118.1 . . ? C414 C413 C412 117.0(10) . . ? C414 C413 H41B 121.5 . . ? C412 C413 H41B 121.5 . . ? C413 C414 C415 120.0(10) . . ? C413 C414 H41C 120.0 . . ? C415 C414 H41C 120.0 . . ? C416 C415 C414 120.7(9) . . ? C416 C415 H41D 119.7 . . ? C414 C415 H41D 119.7 . . ? C415 C416 C411 122.2(9) . . ? C415 C416 H41E 118.9 . . ? C411 C416 H41E 118.9 . . ? Cl1 C1S Cl2 114(2) . . ? Cl1 C1S H1SA 108.8 . . ? Cl2 C1S H1SA 108.8 . . ? Cl1 C1S H1SB 108.8 . . ? Cl2 C1S H1SB 108.8 . . ? H1SA C1S H1SB 107.7 . . ? O3 N5 O1 120.6(18) . . ? O3 N5 O2 129(2) . . ? O1 N5 O2 110.3(17) . . ? O6 N6 O5 120.9(11) . . ? O6 N6 O4 115.7(11) . . ? O5 N6 O4 117.5(11) . . ? 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 N2 Cu1 P1 C111 -55.1(4) . . . . ? N1 Cu1 P1 C111 33.0(4) . . . . ? P2 Cu1 P1 C111 168.4(3) . . . . ? N2 Cu1 P1 C28 70.6(4) . . . . ? N1 Cu1 P1 C28 158.7(4) . . . . ? P2 Cu1 P1 C28 -65.9(3) . . . . ? N2 Cu1 P1 C101 -174.1(4) . . . . ? N1 Cu1 P1 C101 -86.0(4) . . . . ? P2 Cu1 P1 C101 49.4(4) . . . . ? N2 Cu1 P2 C201 87.1(4) . . . . ? N1 Cu1 P2 C201 7.5(4) . . . . ? P1 Cu1 P2 C201 -131.6(3) . . . . ? N2 Cu1 P2 C211 -153.1(4) . . . . ? N1 Cu1 P2 C211 127.3(4) . . . . ? P1 Cu1 P2 C211 -11.8(4) . . . . ? N2 Cu1 P2 C27 -27.8(3) . . . . ? N1 Cu1 P2 C27 -107.4(4) . . . . ? P1 Cu1 P2 C27 113.5(3) . . . . ? N3 Cu2 P3 C311 158.0(4) . . . . ? N4 Cu2 P3 C311 -121.0(5) . . . . ? P4 Cu2 P3 C311 20.5(4) . . . . ? N3 Cu2 P3 C301 -81.9(4) . . . . ? N4 Cu2 P3 C301 -0.8(5) . . . . ? P4 Cu2 P3 C301 140.6(4) . . . . ? N3 Cu2 P3 C27 32.7(4) . . . . ? N4 Cu2 P3 C27 113.7(4) . . . . ? P4 Cu2 P3 C27 -104.8(3) . . . . ? N3 Cu2 P4 C411 40.1(4) . . . . ? N4 Cu2 P4 C411 -45.7(4) . . . . ? P3 Cu2 P4 C411 175.5(3) . . . . ? N3 Cu2 P4 C401 158.8(3) . . . . ? N4 Cu2 P4 C401 73.0(4) . . . . ? P3 Cu2 P4 C401 -65.9(3) . . . . ? N3 Cu2 P4 C28 -82.0(4) . . . . ? N4 Cu2 P4 C28 -167.8(4) . . . . ? P3 Cu2 P4 C28 53.3(4) . . . . ? N2 Cu1 N1 C1 -165.4(8) . . . . ? P1 Cu1 N1 C1 79.2(8) . . . . ? P2 Cu1 N1 C1 -63.9(8) . . . . ? N2 Cu1 N1 C5 -2.0(6) . . . . ? P1 Cu1 N1 C5 -117.3(6) . . . . ? P2 Cu1 N1 C5 99.6(6) . . . . ? N1 Cu1 N2 C6 -10.4(6) . . . . ? P1 Cu1 N2 C6 102.3(6) . . . . ? P2 Cu1 N2 C6 -113.5(6) . . . . ? N1 Cu1 N2 N3 179.8(6) . . . . ? P1 Cu1 N2 N3 -67.5(6) . . . . ? P2 Cu1 N2 N3 76.7(5) . . . . ? C6 N2 N3 C9 1.0(11) . . . . ? Cu1 N2 N3 C9 170.5(5) . . . . ? C6 N2 N3 Cu2 -171.4(6) . . . . ? Cu1 N2 N3 Cu2 -2.0(7) . . . . ? N4 Cu2 N3 N2 -178.9(6) . . . . ? P4 Cu2 N3 N2 70.1(5) . . . . ? P3 Cu2 N3 N2 -76.2(5) . . . . ? N4 Cu2 N3 C9 8.6(6) . . . . ? P4 Cu2 N3 C9 -102.5(6) . . . . ? P3 Cu2 N3 C9 111.2(5) . . . . ? N3 Cu2 N4 C14 168.0(7) . . . . ? P4 Cu2 N4 C14 -83.3(7) . . . . ? P3 Cu2 N4 C14 65.5(7) . . . . ? N3 Cu2 N4 C10 0.0(6) . . . . ? P4 Cu2 N4 C10 108.7(5) . . . . ? P3 Cu2 N4 C10 -102.6(6) . . . . ? C5 N1 C1 C2 -5.1(15) . . . . ? Cu1 N1 C1 C2 158.1(9) . . . . ? N1 C1 C2 C3 1.9(18) . . . . ? C1 C2 C3 C4 -0.1(18) . . . . ? C2 C3 C4 C5 1.7(18) . . . . ? C3 C4 C5 N1 -5.2(17) . . . . ? C3 C4 C5 C6 -174.6(10) . . . . ? C1 N1 C5 C4 6.6(14) . . . . ? Cu1 N1 C5 C4 -158.6(8) . . . . ? C1 N1 C5 C6 177.2(8) . . . . ? Cu1 N1 C5 C6 12.0(9) . . . . ? N3 N2 C6 C7 11.4(12) . . . . ? Cu1 N2 C6 C7 -158.2(6) . . . . ? N3 N2 C6 C5 -170.7(7) . . . . ? Cu1 N2 C6 C5 19.8(9) . . . . ? C4 C5 C6 N2 149.6(9) . . . . ? N1 C5 C6 N2 -20.7(11) . . . . ? C4 C5 C6 C7 -32.6(14) . . . . ? N1 C5 C6 C7 157.2(8) . . . . ? N2 C6 C7 C8 -12.7(12) . . . . ? C5 C6 C7 C8 169.6(8) . . . . ? N2 C6 C7 C15 159.3(8) . . . . ? C5 C6 C7 C15 -18.4(13) . . . . ? C6 C7 C8 C9 1.9(12) . . . . ? C15 C7 C8 C9 -170.2(8) . . . . ? C6 C7 C8 C21 177.3(8) . . . . ? C15 C7 C8 C21 5.1(13) . . . . ? N2 N3 C9 C8 -11.5(11) . . . . ? Cu2 N3 C9 C8 161.1(6) . . . . ? N2 N3 C9 C10 172.5(6) . . . . ? Cu2 N3 C9 C10 -14.8(8) . . . . ? C7 C8 C9 N3 9.7(11) . . . . ? C21 C8 C9 N3 -165.7(8) . . . . ? C7 C8 C9 C10 -175.2(8) . . . . ? C21 C8 C9 C10 9.4(13) . . . . ? C14 N4 C10 C11 -3.4(12) . . . . ? Cu2 N4 C10 C11 165.7(7) . . . . ? C14 N4 C10 C9 -176.9(8) . . . . ? Cu2 N4 C10 C9 -7.8(9) . . . . ? N3 C9 C10 N4 14.5(10) . . . . ? C8 C9 C10 N4 -160.9(8) . . . . ? N3 C9 C10 C11 -158.7(8) . . . . ? C8 C9 C10 C11 25.9(14) . . . . ? N4 C10 C11 C12 2.9(15) . . . . ? C9 C10 C11 C12 175.9(9) . . . . ? C10 C11 C12 C13 -2.0(16) . . . . ? C11 C12 C13 C14 1.6(15) . . . . ? C10 N4 C14 C13 3.4(14) . . . . ? Cu2 N4 C14 C13 -164.2(7) . . . . ? C12 C13 C14 N4 -2.4(15) . . . . ? C8 C7 C15 C20 -74.5(12) . . . . ? C6 C7 C15 C20 113.7(10) . . . . ? C8 C7 C15 C16 103.2(10) . . . . ? C6 C7 C15 C16 -68.6(11) . . . . ? C20 C15 C16 C17 2.2(14) . . . . ? C7 C15 C16 C17 -175.7(10) . . . . ? C15 C16 C17 C18 -2.4(19) . . . . ? C16 C17 C18 C19 2(2) . . . . ? C17 C18 C19 C20 -1.9(19) . . . . ? C18 C19 C20 C15 2.1(19) . . . . ? C16 C15 C20 C19 -2.2(15) . . . . ? C7 C15 C20 C19 175.6(10) . . . . ? C7 C8 C21 C26 -96.2(11) . . . . ? C9 C8 C21 C26 79.0(12) . . . . ? C7 C8 C21 C22 82.7(13) . . . . ? C9 C8 C21 C22 -102.1(11) . . . . ? C26 C21 C22 C23 -1.2(18) . . . . ? C8 C21 C22 C23 179.9(11) . . . . ? C21 C22 C23 C24 1(2) . . . . ? C22 C23 C24 C25 -2(3) . . . . ? C23 C24 C25 C26 2(3) . . . . ? C22 C21 C26 C25 1.3(17) . . . . ? C8 C21 C26 C25 -179.8(10) . . . . ? C24 C25 C26 C21 -2(2) . . . . ? C201 P2 C27 P3 -175.1(5) . . . . ? C211 P2 C27 P3 76.6(5) . . . . ? Cu1 P2 C27 P3 -58.3(5) . . . . ? C311 P3 C27 P2 -76.2(6) . . . . ? C301 P3 C27 P2 173.5(5) . . . . ? Cu2 P3 C27 P2 56.2(5) . . . . ? C111 P1 C28 P4 88.7(5) . . . . ? C101 P1 C28 P4 -165.3(5) . . . . ? Cu1 P1 C28 P4 -42.8(6) . . . . ? C411 P4 C28 P1 -77.4(5) . . . . ? C401 P4 C28 P1 174.7(5) . . . . ? Cu2 P4 C28 P1 50.4(6) . . . . ? C111 P1 C101 C106 85.9(9) . . . . ? C28 P1 C101 C106 -22.8(9) . . . . ? Cu1 P1 C101 C106 -146.7(8) . . . . ? C111 P1 C101 C102 -95.4(9) . . . . ? C28 P1 C101 C102 156.0(8) . . . . ? Cu1 P1 C101 C102 32.0(9) . . . . ? C106 C101 C102 C103 1.8(17) . . . . ? P1 C101 C102 C103 -177.0(10) . . . . ? C101 C102 C103 C104 1.4(19) . . . . ? C102 C103 C104 C105 -2(2) . . . . ? C103 C104 C105 C106 0.3(18) . . . . ? C102 C101 C106 C105 -3.9(16) . . . . ? P1 C101 C106 C105 174.8(8) . . . . ? C104 C105 C106 C101 2.9(17) . . . . ? C28 P1 C111 C112 -154.0(8) . . . . ? C101 P1 C111 C112 101.2(8) . . . . ? Cu1 P1 C111 C112 -23.6(9) . . . . ? C28 P1 C111 C116 32.1(8) . . . . ? C101 P1 C111 C116 -72.7(8) . . . . ? Cu1 P1 C111 C116 162.5(7) . . . . ? C116 C111 C112 C113 0.6(16) . . . . ? P1 C111 C112 C113 -173.8(10) . . . . ? C111 C112 C113 C114 0(2) . . . . ? C112 C113 C114 C115 0(2) . . . . ? C113 C114 C115 C116 -1(2) . . . . ? C114 C115 C116 C111 1.6(17) . . . . ? C112 C111 C116 C115 -1.4(14) . . . . ? P1 C111 C116 C115 172.7(8) . . . . ? C211 P2 C201 C206 151.4(8) . . . . ? C27 P2 C201 C206 43.3(9) . . . . ? Cu1 P2 C201 C206 -77.6(9) . . . . ? C211 P2 C201 C202 -41.7(9) . . . . ? C27 P2 C201 C202 -149.8(8) . . . . ? Cu1 P2 C201 C202 89.3(8) . . . . ? C206 C201 C202 C203 -0.2(16) . . . . ? P2 C201 C202 C203 -167.8(9) . . . . ? C201 C202 C203 C204 2.2(19) . . . . ? C202 C203 C204 C205 -4(2) . . . . ? C203 C204 C205 C206 4(2) . . . . ? C202 C201 C206 C205 0.0(16) . . . . ? P2 C201 C206 C205 167.1(9) . . . . ? C204 C205 C206 C201 -1.9(19) . . . . ? C201 P2 C211 C216 -49.3(10) . . . . ? C27 P2 C211 C216 59.5(10) . . . . ? Cu1 P2 C211 C216 -170.8(8) . . . . ? C201 P2 C211 C212 137.7(8) . . . . ? C27 P2 C211 C212 -113.5(8) . . . . ? Cu1 P2 C211 C212 16.2(10) . . . . ? C216 C211 C212 C213 2.8(17) . . . . ? P2 C211 C212 C213 176.3(10) . . . . ? C211 C212 C213 C214 -4(2) . . . . ? C212 C213 C214 C215 3(2) . . . . ? C213 C214 C215 C216 -1(2) . . . . ? C214 C215 C216 C211 0(2) . . . . ? C212 C211 C216 C215 -1.1(17) . . . . ? P2 C211 C216 C215 -174.3(10) . . . . ? C311 P3 C301 C302 22.6(10) . . . . ? C27 P3 C301 C302 133.2(9) . . . . ? Cu2 P3 C301 C302 -106.0(8) . . . . ? C311 P3 C301 C306 -166.9(7) . . . . ? C27 P3 C301 C306 -56.2(8) . . . . ? Cu2 P3 C301 C306 64.5(7) . . . . ? C306 C301 C302 C303 -1.6(16) . . . . ? P3 C301 C302 C303 169.0(9) . . . . ? C301 C302 C303 C304 0.1(18) . . . . ? C302 C303 C304 C305 1.3(18) . . . . ? C303 C304 C305 C306 -1.2(18) . . . . ? C302 C301 C306 C305 1.6(13) . . . . ? P3 C301 C306 C305 -169.5(7) . . . . ? C304 C305 C306 C301 -0.3(15) . . . . ? C301 P3 C311 C316 -121.0(9) . . . . ? C27 P3 C311 C316 129.7(8) . . . . ? Cu2 P3 C311 C316 0.8(10) . . . . ? C301 P3 C311 C312 55.1(11) . . . . ? C27 P3 C311 C312 -54.2(11) . . . . ? Cu2 P3 C311 C312 176.9(9) . . . . ? C316 C311 C312 C313 -5.3(17) . . . . ? P3 C311 C312 C313 178.4(10) . . . . ? C311 C312 C313 C314 5(2) . . . . ? C312 C313 C314 C315 -4(2) . . . . ? C313 C314 C315 C316 3(2) . . . . ? C314 C315 C316 C311 -4.2(19) . . . . ? C312 C311 C316 C315 5.0(16) . . . . ? P3 C311 C316 C315 -178.5(9) . . . . ? C411 P4 C401 C402 -105.9(8) . . . . ? C28 P4 C401 C402 1.3(9) . . . . ? Cu2 P4 C401 C402 129.4(8) . . . . ? C411 P4 C401 C406 75.6(8) . . . . ? C28 P4 C401 C406 -177.2(7) . . . . ? Cu2 P4 C401 C406 -49.2(8) . . . . ? C406 C401 C402 C403 0.9(15) . . . . ? P4 C401 C402 C403 -177.7(8) . . . . ? C401 C402 C403 C404 -1.2(18) . . . . ? C402 C403 C404 C405 -0.6(18) . . . . ? C403 C404 C405 C406 2.7(17) . . . . ? C404 C405 C406 C401 -3.0(16) . . . . ? C402 C401 C406 C405 1.2(15) . . . . ? P4 C401 C406 C405 179.8(8) . . . . ? C401 P4 C411 C412 -165.1(7) . . . . ? C28 P4 C411 C412 88.2(8) . . . . ? Cu2 P4 C411 C412 -41.8(8) . . . . ? C401 P4 C411 C416 16.9(9) . . . . ? C28 P4 C411 C416 -89.9(8) . . . . ? Cu2 P4 C411 C416 140.1(7) . . . . ? C416 C411 C412 C413 -0.1(14) . . . . ? P4 C411 C412 C413 -178.3(8) . . . . ? C411 C412 C413 C414 -3.3(15) . . . . ? C412 C413 C414 C415 3.4(15) . . . . ? C413 C414 C415 C416 -0.1(17) . . . . ? C414 C415 C416 C411 -3.6(16) . . . . ? C412 C411 C416 C415 3.7(14) . . . . ? P4 C411 C416 C415 -178.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.109 _refine_diff_density_min -1.013 _refine_diff_density_rms 0.147 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.161 0.682 0.219 152 23 ' ' 2 -0.161 0.318 0.781 152 23 ' ' 3 0.339 0.182 0.281 152 23 ' ' 4 0.661 0.818 0.719 152 23 ' ' _platon_squeeze_details ; ; # Attachment '- bgi03ls.CIF' data_b _database_code_depnum_ccdc_archive 'CCDC 824325' #TrackingRef '- bgi03ls.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H62 Cl2 Cu2 N8 O6 P4' _chemical_formula_weight 1493.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.570(4) _cell_length_b 19.092(5) _cell_length_c 26.482(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.897(7) _cell_angle_gamma 90.00 _cell_volume 7313(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8565 _exptl_absorpt_correction_T_max 0.9172 _exptl_absorpt_process_details 'SADABS; Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker Apex CCD Area Detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62142 _diffrn_reflns_av_R_equivalents 0.1526 _diffrn_reflns_av_sigmaI/netI 0.0856 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 23.44 _reflns_number_total 10613 _reflns_number_gt 7567 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINTPLUS _computing_data_reduction SAINTPLUS _computing_structure_solution 'SHELXTL (Sheldrick, 1990)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0456P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10613 _refine_ls_number_parameters 911 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1283 _refine_ls_wR_factor_gt 0.1196 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_restrained_S_all 0.920 _refine_ls_shift/su_max 0.012 _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 0.24962(3) 0.80192(2) 0.110151(19) 0.03820(15) Uani 1 1 d . . . Cu2 Cu 0.09947(3) 0.71340(2) 0.025477(19) 0.03776(15) Uani 1 1 d . . . P1 P 0.23089(7) 0.71904(5) 0.16812(4) 0.0370(3) Uani 1 1 d . . . P2 P 0.15234(8) 0.89393(5) 0.09249(5) 0.0417(3) Uani 1 1 d . . . P3 P 0.10159(7) 0.63482(5) 0.08779(4) 0.0376(3) Uani 1 1 d . . . P4 P 0.01992(7) 0.81371(6) 0.01236(5) 0.0413(3) Uani 1 1 d . . . N1 N 0.3875(2) 0.84233(17) 0.11072(14) 0.0416(9) Uani 1 1 d . . . N2 N 0.2874(2) 0.77156(16) 0.04021(13) 0.0366(8) Uani 1 1 d . . . N3 N 0.2283(2) 0.73579(16) 0.00717(13) 0.0357(8) Uani 1 1 d . . . N4 N 0.0983(2) 0.66883(16) -0.04767(13) 0.0405(9) Uani 1 1 d . . . N5 N 0.7008(3) 0.7105(3) -0.0144(3) 0.0894(17) Uani 1 1 d . . . N6 N 0.4440(4) 0.5796(4) -0.1587(3) 0.114(2) Uani 1 1 d . . . C1 C 0.4273(3) 0.8898(2) 0.14363(19) 0.0550(13) Uani 1 1 d . . . H1A H 0.4046 0.8955 0.1747 0.066 Uiso 1 1 calc R . . C2 C 0.5006(3) 0.9303(3) 0.1330(2) 0.0661(15) Uani 1 1 d . . . H2A H 0.5264 0.9629 0.1566 0.079 Uiso 1 1 calc R . . C3 C 0.5355(3) 0.9227(3) 0.0876(2) 0.0699(16) Uani 1 1 d . . . H3A H 0.5836 0.9510 0.0794 0.084 Uiso 1 1 calc R . . C4 C 0.4975(3) 0.8719(2) 0.0543(2) 0.0604(13) Uani 1 1 d . . . H4A H 0.5208 0.8644 0.0235 0.073 Uiso 1 1 calc R . . C5 C 0.4242(3) 0.8321(2) 0.06731(17) 0.0414(10) Uani 1 1 d . . . C6 C 0.3742(3) 0.78029(19) 0.03187(16) 0.0369(10) Uani 1 1 d . . . C7 C 0.4119(3) 0.7424(2) -0.00655(17) 0.0416(10) Uani 1 1 d . . . C8 C 0.3494(3) 0.7060(2) -0.04160(17) 0.0414(10) Uani 1 1 d . . . C9 C 0.2557(3) 0.7077(2) -0.03447(16) 0.0388(10) Uani 1 1 d . . . C10 C 0.1766(3) 0.6785(2) -0.06933(17) 0.0424(11) Uani 1 1 d . . . C11 C 0.1789(3) 0.6669(3) -0.12117(18) 0.0592(13) Uani 1 1 d . . . H11A H 0.2327 0.6748 -0.1360 0.071 Uiso 1 1 calc R . . C12 C 0.0989(4) 0.6432(3) -0.1503(2) 0.0721(16) Uani 1 1 d . . . H12A H 0.0989 0.6342 -0.1848 0.087 Uiso 1 1 calc R . . C13 C 0.0205(4) 0.6333(2) -0.1277(2) 0.0595(14) Uani 1 1 d . . . H13A H -0.0334 0.6174 -0.1466 0.071 Uiso 1 1 calc R . . C14 C 0.0225(3) 0.6473(2) -0.07709(19) 0.0515(12) Uani 1 1 d . . . H14A H -0.0317 0.6415 -0.0623 0.062 Uiso 1 1 calc R . . C15 C 0.5131(3) 0.7340(2) -0.00823(19) 0.0503(12) Uani 1 1 d . . . C16 C 0.5637(4) 0.6917(3) 0.0268(2) 0.0679(15) Uani 1 1 d . . . H16A H 0.5366 0.6712 0.0532 0.082 Uiso 1 1 calc R . . C17 C 0.6564(4) 0.6802(3) 0.0216(3) 0.088(2) Uani 1 1 d . . . H17A H 0.6897 0.6499 0.0443 0.106 Uiso 1 1 calc R . . C18 C 0.6514(4) 0.7514(3) -0.0459(3) 0.0799(17) Uani 1 1 d . . . H18A H 0.6807 0.7731 -0.0710 0.096 Uiso 1 1 calc R . . C19 C 0.5603(3) 0.7651(3) -0.0450(2) 0.0639(14) Uani 1 1 d . . . H19A H 0.5295 0.7952 -0.0689 0.077 Uiso 1 1 calc R . . C20 C 0.3841(3) 0.6620(3) -0.08161(18) 0.0505(12) Uani 1 1 d . . . C21 C 0.3941(3) 0.5910(3) -0.0746(2) 0.0662(15) Uani 1 1 d . . . H21A H 0.3809 0.5696 -0.0447 0.079 Uiso 1 1 calc R . . C22 C 0.4253(4) 0.5515(4) -0.1145(3) 0.095(2) Uani 1 1 d . . . H22A H 0.4333 0.5035 -0.1099 0.114 Uiso 1 1 calc R . . C23 C 0.4351(5) 0.6473(5) -0.1635(3) 0.105(2) Uani 1 1 d . . . H23A H 0.4487 0.6676 -0.1937 0.127 Uiso 1 1 calc R . . C24 C 0.4064(4) 0.6910(3) -0.1263(2) 0.0757(16) Uani 1 1 d . . . H24A H 0.4023 0.7392 -0.1315 0.091 Uiso 1 1 calc R . . C25 C 0.0921(3) 0.8928(2) 0.02714(17) 0.0430(11) Uani 1 1 d . . . H25A H 0.1377 0.8955 0.0034 0.052 Uiso 1 1 calc R . . H25B H 0.0530 0.9339 0.0222 0.052 Uiso 1 1 calc R . . C26 C 0.1264(3) 0.6653(2) 0.15338(15) 0.0383(10) Uani 1 1 d . . . H26A H 0.1318 0.6247 0.1755 0.046 Uiso 1 1 calc R . . H26B H 0.0738 0.6923 0.1616 0.046 Uiso 1 1 calc R . . C101 C 0.3259(3) 0.6575(2) 0.18503(17) 0.0457(11) Uani 1 1 d . . . C102 C 0.4130(3) 0.6778(3) 0.1757(2) 0.0706(16) Uani 1 1 d . . . H10A H 0.4213 0.7208 0.1604 0.085 Uiso 1 1 calc R . . C103 C 0.4878(4) 0.6346(4) 0.1889(3) 0.094(2) Uani 1 1 d . . . H10B H 0.5467 0.6486 0.1829 0.113 Uiso 1 1 calc R . . C104 C 0.4752(5) 0.5718(4) 0.2107(3) 0.093(2) Uani 1 1 d . . . H10C H 0.5257 0.5425 0.2194 0.112 Uiso 1 1 calc R . . C105 C 0.3905(5) 0.5512(3) 0.2201(2) 0.0829(19) Uani 1 1 d . . . H10D H 0.3833 0.5080 0.2354 0.099 Uiso 1 1 calc R . . C106 C 0.3144(4) 0.5932(2) 0.2072(2) 0.0652(15) Uani 1 1 d . . . H10E H 0.2559 0.5784 0.2134 0.078 Uiso 1 1 calc R . . C111 C 0.2096(3) 0.7552(2) 0.22996(16) 0.0408(10) Uani 1 1 d . . . C112 C 0.2505(4) 0.8184(2) 0.24500(19) 0.0590(13) Uani 1 1 d . . . H11B H 0.2916 0.8392 0.2252 0.071 Uiso 1 1 calc R . . C113 C 0.2311(4) 0.8509(3) 0.2890(2) 0.0706(16) Uani 1 1 d . . . H11C H 0.2581 0.8937 0.2986 0.085 Uiso 1 1 calc R . . C114 C 0.1713(4) 0.8193(3) 0.3185(2) 0.0700(15) Uani 1 1 d . . . H11D H 0.1574 0.8410 0.3481 0.084 Uiso 1 1 calc R . . C115 C 0.1325(4) 0.7564(3) 0.30462(19) 0.0639(14) Uani 1 1 d . . . H11E H 0.0925 0.7351 0.3249 0.077 Uiso 1 1 calc R . . C116 C 0.1520(3) 0.7241(2) 0.26090(17) 0.0486(12) Uani 1 1 d . . . H11F H 0.1259 0.6807 0.2520 0.058 Uiso 1 1 calc R . . C201 C 0.2247(3) 0.9724(2) 0.09474(19) 0.0502(12) Uani 1 1 d . . . C202 C 0.2743(3) 0.9896(3) 0.0558(2) 0.0647(14) Uani 1 1 d . . . H20A H 0.2628 0.9667 0.0247 0.078 Uiso 1 1 calc R . . C203 C 0.3416(4) 1.0412(3) 0.0627(3) 0.090(2) Uani 1 1 d . . . H20B H 0.3747 1.0531 0.0360 0.108 Uiso 1 1 calc R . . C204 C 0.3598(5) 1.0748(3) 0.1089(3) 0.091(2) Uani 1 1 d . . . H20C H 0.4059 1.1087 0.1136 0.109 Uiso 1 1 calc R . . C205 C 0.3104(4) 1.0585(3) 0.1473(3) 0.087(2) Uani 1 1 d . . . H20D H 0.3222 1.0819 0.1782 0.104 Uiso 1 1 calc R . . C206 C 0.2426(4) 1.0075(2) 0.1413(2) 0.0691(15) Uani 1 1 d . . . H20E H 0.2091 0.9966 0.1680 0.083 Uiso 1 1 calc R . . C211 C 0.0627(3) 0.9158(2) 0.13154(18) 0.0478(11) Uani 1 1 d . . . C212 C 0.0396(4) 0.8681(3) 0.1667(2) 0.0676(15) Uani 1 1 d . . . H21B H 0.0725 0.8264 0.1714 0.081 Uiso 1 1 calc R . . C213 C -0.0315(5) 0.8815(4) 0.1950(2) 0.092(2) Uani 1 1 d . . . H21C H -0.0461 0.8484 0.2186 0.111 Uiso 1 1 calc R . . C214 C -0.0804(4) 0.9409(4) 0.1895(3) 0.0877(19) Uani 1 1 d . . . H21D H -0.1280 0.9493 0.2092 0.105 Uiso 1 1 calc R . . C215 C -0.0598(5) 0.9885(3) 0.1549(3) 0.103(2) Uani 1 1 d . . . H21E H -0.0942 1.0295 0.1503 0.124 Uiso 1 1 calc R . . C216 C 0.0116(4) 0.9767(3) 0.1265(3) 0.0844(19) Uani 1 1 d . . . H21F H 0.0259 1.0106 0.1035 0.101 Uiso 1 1 calc R . . C301 C 0.1858(3) 0.5638(2) 0.08412(15) 0.0400(10) Uani 1 1 d . . . C302 C 0.2712(3) 0.5797(2) 0.07046(18) 0.0519(12) Uani 1 1 d . . . H30A H 0.2853 0.6259 0.0636 0.062 Uiso 1 1 calc R . . C303 C 0.3369(3) 0.5281(3) 0.0667(2) 0.0617(14) Uani 1 1 d . . . H30B H 0.3950 0.5397 0.0581 0.074 Uiso 1 1 calc R . . C304 C 0.3152(4) 0.4598(3) 0.0760(2) 0.0658(15) Uani 1 1 d . . . H30C H 0.3585 0.4246 0.0733 0.079 Uiso 1 1 calc R . . C305 C 0.2299(4) 0.4432(2) 0.0893(2) 0.0649(15) Uani 1 1 d . . . H30D H 0.2155 0.3967 0.0951 0.078 Uiso 1 1 calc R . . C306 C 0.1649(3) 0.4946(2) 0.09410(18) 0.0527(12) Uani 1 1 d . . . H30E H 0.1077 0.4830 0.1039 0.063 Uiso 1 1 calc R . . C311 C -0.0090(3) 0.5901(2) 0.08938(17) 0.0405(10) Uani 1 1 d . . . C312 C -0.0510(3) 0.5617(2) 0.04447(18) 0.0566(13) Uani 1 1 d . . . H31A H -0.0223 0.5652 0.0150 0.068 Uiso 1 1 calc R . . C313 C -0.1349(4) 0.5282(3) 0.0430(2) 0.0685(16) Uani 1 1 d . . . H31B H -0.1622 0.5086 0.0127 0.082 Uiso 1 1 calc R . . C314 C -0.1784(4) 0.5236(3) 0.0860(2) 0.0701(16) Uani 1 1 d . . . H31C H -0.2356 0.5015 0.0848 0.084 Uiso 1 1 calc R . . C315 C -0.1379(4) 0.5513(3) 0.1300(2) 0.0779(17) Uani 1 1 d . . . H31D H -0.1673 0.5481 0.1592 0.094 Uiso 1 1 calc R . . C316 C -0.0534(3) 0.5843(3) 0.1319(2) 0.0647(14) Uani 1 1 d . . . H31E H -0.0261 0.6028 0.1626 0.078 Uiso 1 1 calc R . . C401 C -0.0836(3) 0.8260(2) 0.04332(18) 0.0476(11) Uani 1 1 d . . . C402 C -0.1378(4) 0.8856(3) 0.0373(3) 0.0790(17) Uani 1 1 d . . . H40A H -0.1225 0.9213 0.0159 0.095 Uiso 1 1 calc R . . C403 C -0.2143(4) 0.8923(4) 0.0629(3) 0.097(2) Uani 1 1 d . . . H40B H -0.2502 0.9326 0.0587 0.116 Uiso 1 1 calc R . . C404 C -0.2381(4) 0.8401(4) 0.0945(3) 0.0868(19) Uani 1 1 d . . . H40C H -0.2895 0.8453 0.1119 0.104 Uiso 1 1 calc R . . C405 C -0.1863(4) 0.7813(4) 0.1002(2) 0.0815(17) Uani 1 1 d . . . H40D H -0.2023 0.7455 0.1214 0.098 Uiso 1 1 calc R . . C406 C -0.1099(3) 0.7743(3) 0.0746(2) 0.0601(13) Uani 1 1 d . . . H40E H -0.0752 0.7334 0.0787 0.072 Uiso 1 1 calc R . . C411 C -0.0171(3) 0.8229(2) -0.05583(18) 0.0467(11) Uani 1 1 d . . . C412 C 0.0475(4) 0.8333(2) -0.0888(2) 0.0600(14) Uani 1 1 d . . . H41A H 0.1085 0.8423 -0.0758 0.072 Uiso 1 1 calc R . . C413 C 0.0240(4) 0.8306(3) -0.1406(2) 0.0724(16) Uani 1 1 d . . . H41B H 0.0689 0.8372 -0.1622 0.087 Uiso 1 1 calc R . . C414 C -0.0655(5) 0.8181(3) -0.1602(2) 0.0845(19) Uani 1 1 d . . . H41C H -0.0820 0.8165 -0.1952 0.101 Uiso 1 1 calc R . . C415 C -0.1305(5) 0.8079(4) -0.1279(3) 0.098(2) Uani 1 1 d . . . H41D H -0.1915 0.7995 -0.1411 0.118 Uiso 1 1 calc R . . C416 C -0.1067(4) 0.8100(3) -0.0758(2) 0.0756(17) Uani 1 1 d . . . H41E H -0.1517 0.8026 -0.0542 0.091 Uiso 1 1 calc R . . C1S C 0.8440(7) 0.6132(5) 0.2770(4) 0.161(4) Uani 1 1 d . . . H1SA H 0.8909 0.5801 0.2693 0.193 Uiso 1 1 calc R . . H1SB H 0.8494 0.6186 0.3136 0.193 Uiso 1 1 calc R . . Cl1 Cl 0.8643(4) 0.69116(19) 0.25046(18) 0.261(2) Uani 1 1 d . . . Cl2 Cl 0.7394(3) 0.5802(3) 0.2566(2) 0.311(3) Uani 1 1 d . . . N7 N 0.0562(5) 0.4983(3) 0.2371(2) 0.0811(15) Uani 1 1 d . . . O1 O 0.1217(5) 0.4901(5) 0.2156(4) 0.209(4) Uani 1 1 d . . . O2 O 0.0473(4) 0.5590(3) 0.2472(2) 0.143(2) Uani 1 1 d . . . O3 O 0.0079(6) 0.4553(4) 0.2428(2) 0.212(5) Uani 1 1 d . . . O4 O 0.2846(9) 0.8393(6) -0.1072(5) 0.137(5) Uani 0.588(14) 1 d PD A 1 O5 O 0.4004(10) 0.8968(9) -0.0830(8) 0.202(11) Uani 0.588(14) 1 d PD A 1 O6 O 0.2844(14) 0.9066(11) -0.0478(7) 0.215(12) Uani 0.588(14) 1 d PD A 1 N8 N 0.3232(10) 0.8812(10) -0.0797(7) 0.124(12) Uani 0.588(14) 1 d PD A 1 O4' O 0.3114(12) 0.9505(6) -0.0939(8) 0.171(10) Uani 0.412(14) 1 d PD A 2 O5' O 0.3868(15) 0.8582(10) -0.0918(8) 0.127(11) Uani 0.412(14) 1 d PD A 2 O6' O 0.2741(9) 0.8670(7) -0.0503(7) 0.080(5) Uani 0.412(14) 1 d PD A 2 N8' N 0.3267(8) 0.8925(6) -0.0767(6) 0.046(6) Uani 0.412(14) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0419(3) 0.0348(3) 0.0374(3) -0.0012(2) 0.0028(2) -0.0028(2) Cu2 0.0380(3) 0.0374(3) 0.0369(3) 0.0029(2) 0.0006(2) -0.0027(2) P1 0.0430(6) 0.0319(6) 0.0348(6) -0.0013(5) -0.0013(5) -0.0015(4) P2 0.0481(7) 0.0313(6) 0.0454(7) 0.0008(5) 0.0040(5) -0.0008(5) P3 0.0442(6) 0.0326(6) 0.0346(6) 0.0003(5) -0.0010(5) -0.0036(5) P4 0.0368(6) 0.0407(6) 0.0453(7) 0.0057(5) -0.0001(5) 0.0001(5) N1 0.038(2) 0.040(2) 0.045(2) -0.0059(17) -0.0055(17) -0.0074(15) N2 0.035(2) 0.0359(19) 0.037(2) -0.0030(16) -0.0008(16) -0.0035(14) N3 0.0382(19) 0.0352(18) 0.032(2) -0.0026(16) -0.0004(16) -0.0047(15) N4 0.044(2) 0.0367(19) 0.039(2) -0.0009(16) -0.0026(18) -0.0051(15) N5 0.055(3) 0.096(4) 0.116(5) -0.041(4) 0.009(3) -0.001(3) N6 0.098(4) 0.129(6) 0.122(6) -0.060(5) 0.035(4) 0.000(4) C1 0.053(3) 0.056(3) 0.054(3) -0.013(2) 0.000(2) -0.008(2) C2 0.049(3) 0.064(3) 0.084(4) -0.027(3) 0.000(3) -0.018(2) C3 0.046(3) 0.066(3) 0.100(5) -0.028(3) 0.019(3) -0.024(2) C4 0.056(3) 0.054(3) 0.073(4) -0.014(3) 0.018(3) -0.012(2) C5 0.039(2) 0.039(2) 0.046(3) -0.006(2) 0.003(2) -0.0008(19) C6 0.035(2) 0.033(2) 0.043(3) -0.0024(19) 0.0025(19) -0.0040(17) C7 0.042(2) 0.040(2) 0.043(3) 0.000(2) 0.008(2) -0.0037(19) C8 0.043(3) 0.039(2) 0.042(3) -0.002(2) 0.005(2) -0.0032(19) C9 0.045(3) 0.034(2) 0.036(3) -0.004(2) 0.000(2) -0.0043(18) C10 0.047(3) 0.040(2) 0.038(3) -0.001(2) -0.001(2) -0.0019(19) C11 0.056(3) 0.083(4) 0.039(3) -0.014(3) 0.004(2) -0.005(3) C12 0.080(4) 0.088(4) 0.044(3) -0.015(3) -0.011(3) -0.005(3) C13 0.064(3) 0.060(3) 0.050(3) -0.005(3) -0.013(3) -0.015(2) C14 0.050(3) 0.047(3) 0.054(3) 0.002(2) -0.008(2) -0.011(2) C15 0.049(3) 0.047(3) 0.054(3) -0.015(2) 0.002(2) 0.002(2) C16 0.057(3) 0.068(3) 0.077(4) -0.004(3) -0.001(3) 0.000(3) C17 0.065(4) 0.078(4) 0.116(6) -0.008(4) -0.013(4) 0.014(3) C18 0.051(4) 0.105(5) 0.086(5) -0.023(4) 0.016(3) -0.012(3) C19 0.044(3) 0.082(4) 0.068(4) -0.006(3) 0.014(3) -0.003(2) C20 0.042(3) 0.059(3) 0.050(3) -0.017(2) 0.007(2) -0.007(2) C21 0.059(3) 0.064(3) 0.074(4) -0.023(3) 0.002(3) 0.004(3) C22 0.079(4) 0.076(4) 0.126(7) -0.043(5) -0.003(5) 0.012(3) C23 0.106(5) 0.138(7) 0.079(5) -0.043(5) 0.040(4) -0.029(5) C24 0.086(4) 0.081(4) 0.065(4) -0.026(3) 0.028(3) -0.025(3) C25 0.043(2) 0.038(2) 0.047(3) 0.006(2) 0.002(2) -0.0017(18) C26 0.043(2) 0.037(2) 0.035(2) -0.0002(19) 0.0013(19) -0.0020(18) C101 0.054(3) 0.042(3) 0.038(3) -0.004(2) -0.007(2) 0.002(2) C102 0.052(3) 0.063(3) 0.094(5) 0.015(3) -0.002(3) 0.007(3) C103 0.058(4) 0.097(5) 0.127(6) 0.025(4) 0.006(4) 0.020(3) C104 0.079(5) 0.085(5) 0.110(6) 0.001(4) -0.016(4) 0.041(4) C105 0.098(5) 0.050(3) 0.094(5) 0.008(3) -0.016(4) 0.020(3) C106 0.071(3) 0.049(3) 0.070(4) 0.009(3) -0.014(3) 0.003(2) C111 0.047(3) 0.036(2) 0.037(3) 0.001(2) -0.004(2) 0.0017(19) C112 0.075(3) 0.051(3) 0.051(3) -0.007(2) 0.005(3) -0.017(2) C113 0.100(4) 0.052(3) 0.059(4) -0.023(3) 0.007(3) -0.021(3) C114 0.078(4) 0.076(4) 0.056(4) -0.024(3) 0.008(3) -0.002(3) C115 0.072(4) 0.074(4) 0.046(3) -0.007(3) 0.009(3) -0.015(3) C116 0.062(3) 0.042(3) 0.041(3) -0.005(2) 0.000(2) -0.005(2) C201 0.056(3) 0.030(2) 0.062(3) 0.001(2) -0.004(3) 0.000(2) C202 0.068(3) 0.058(3) 0.067(4) 0.008(3) 0.003(3) -0.018(3) C203 0.089(4) 0.086(4) 0.095(5) 0.030(4) 0.010(4) -0.030(4) C204 0.088(5) 0.055(4) 0.122(6) 0.010(4) -0.013(4) -0.027(3) C205 0.098(5) 0.049(3) 0.106(6) -0.015(3) -0.019(4) -0.016(3) C206 0.084(4) 0.047(3) 0.076(4) -0.011(3) 0.008(3) -0.009(3) C211 0.053(3) 0.043(3) 0.049(3) -0.004(2) 0.011(2) -0.002(2) C212 0.076(4) 0.074(4) 0.056(3) 0.009(3) 0.017(3) 0.014(3) C213 0.106(5) 0.116(6) 0.062(4) 0.011(4) 0.038(4) 0.010(4) C214 0.083(4) 0.092(5) 0.095(5) -0.030(4) 0.040(4) -0.004(4) C215 0.095(5) 0.063(4) 0.160(8) -0.021(4) 0.053(5) 0.025(3) C216 0.091(4) 0.049(3) 0.120(6) 0.013(3) 0.044(4) 0.019(3) C301 0.055(3) 0.035(2) 0.028(2) 0.0009(18) -0.004(2) -0.0006(19) C302 0.056(3) 0.042(3) 0.056(3) 0.007(2) 0.001(2) -0.001(2) C303 0.056(3) 0.061(3) 0.069(4) 0.011(3) 0.011(3) 0.009(3) C304 0.073(4) 0.053(3) 0.067(4) -0.002(3) -0.010(3) 0.022(3) C305 0.073(4) 0.042(3) 0.075(4) 0.004(3) -0.011(3) 0.009(3) C306 0.054(3) 0.046(3) 0.057(3) 0.010(2) -0.002(2) -0.002(2) C311 0.049(3) 0.029(2) 0.041(3) 0.0037(19) -0.001(2) -0.0016(18) C312 0.069(3) 0.058(3) 0.041(3) -0.004(2) 0.000(2) -0.014(2) C313 0.065(4) 0.069(3) 0.065(4) -0.003(3) -0.018(3) -0.023(3) C314 0.056(3) 0.074(4) 0.078(4) 0.007(3) -0.003(3) -0.022(3) C315 0.066(4) 0.103(5) 0.067(4) -0.006(3) 0.016(3) -0.031(3) C316 0.063(3) 0.085(4) 0.044(3) -0.005(3) -0.001(3) -0.027(3) C401 0.037(2) 0.056(3) 0.049(3) -0.003(2) 0.001(2) -0.002(2) C402 0.061(4) 0.070(4) 0.111(5) 0.021(3) 0.030(3) 0.020(3) C403 0.062(4) 0.098(5) 0.134(7) -0.003(5) 0.032(4) 0.032(3) C404 0.056(4) 0.127(6) 0.082(5) -0.015(4) 0.024(3) 0.004(4) C405 0.058(4) 0.109(5) 0.080(4) 0.016(4) 0.021(3) -0.002(3) C406 0.050(3) 0.068(3) 0.063(3) 0.008(3) 0.009(3) 0.005(2) C411 0.044(3) 0.043(3) 0.050(3) 0.009(2) -0.005(2) 0.0044(19) C412 0.062(3) 0.055(3) 0.060(4) 0.010(3) -0.006(3) -0.006(2) C413 0.099(5) 0.064(3) 0.053(4) 0.006(3) 0.007(3) -0.004(3) C414 0.112(6) 0.080(4) 0.054(4) 0.006(3) -0.022(4) 0.012(4) C415 0.070(4) 0.136(6) 0.078(5) -0.001(4) -0.033(4) 0.001(4) C416 0.055(3) 0.111(5) 0.057(4) 0.005(3) -0.008(3) -0.003(3) C1S 0.152(8) 0.197(10) 0.141(9) -0.021(8) 0.046(7) -0.055(7) Cl1 0.409(7) 0.160(3) 0.224(4) -0.011(3) 0.075(4) -0.018(3) Cl2 0.178(3) 0.485(8) 0.274(5) 0.002(5) 0.050(3) -0.128(4) N7 0.107(5) 0.073(4) 0.057(3) 0.002(3) -0.014(3) -0.007(3) O1 0.136(6) 0.273(10) 0.221(9) -0.050(7) 0.042(6) 0.028(6) O2 0.204(6) 0.104(4) 0.104(4) -0.013(3) -0.043(4) 0.016(4) O3 0.330(10) 0.212(7) 0.082(4) 0.031(4) -0.017(5) -0.202(8) O4 0.150(11) 0.109(8) 0.156(12) -0.001(8) 0.039(8) -0.014(7) O5 0.081(10) 0.179(16) 0.34(2) 0.121(15) -0.019(10) -0.045(11) O6 0.27(2) 0.25(3) 0.126(14) -0.080(18) 0.036(13) 0.107(18) N8 0.20(3) 0.067(11) 0.105(19) -0.018(11) 0.020(19) -0.037(14) O4' 0.211(19) 0.074(10) 0.24(2) 0.055(11) 0.069(15) 0.005(10) O5' 0.15(2) 0.117(15) 0.133(15) 0.064(12) 0.094(15) 0.067(14) O6' 0.061(7) 0.101(10) 0.086(12) 0.027(8) 0.035(6) 0.008(6) N8' 0.027(8) 0.049(11) 0.061(14) 0.013(8) 0.007(8) 0.007(6) _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 N2 2.077(4) . ? Cu1 N1 2.150(3) . ? Cu1 P1 2.2440(13) . ? Cu1 P2 2.2703(12) . ? Cu2 N3 2.040(3) . ? Cu2 N4 2.114(4) . ? Cu2 P3 2.2277(13) . ? Cu2 P4 2.2438(13) . ? P1 C101 1.830(4) . ? P1 C111 1.838(4) . ? P1 C26 1.838(4) . ? P2 C211 1.810(5) . ? P2 C201 1.829(4) . ? P2 C25 1.844(4) . ? P3 C26 1.826(4) . ? P3 C311 1.828(4) . ? P3 C301 1.839(4) . ? P4 C401 1.816(5) . ? P4 C411 1.830(5) . ? P4 C25 1.854(4) . ? N1 C5 1.339(5) . ? N1 C1 1.340(5) . ? N2 C6 1.319(5) . ? N2 N3 1.339(4) . ? N3 C9 1.330(5) . ? N4 C14 1.337(5) . ? N4 C10 1.350(5) . ? N5 C18 1.296(8) . ? N5 C17 1.344(9) . ? N6 C23 1.303(9) . ? N6 C22 1.344(9) . ? C1 C2 1.375(7) . ? C1 H1A 0.9300 . ? C2 C3 1.367(8) . ? C2 H2A 0.9300 . ? C3 C4 1.382(7) . ? C3 H3A 0.9300 . ? C4 C5 1.387(6) . ? C4 H4A 0.9300 . ? C5 C6 1.492(5) . ? C6 C7 1.413(6) . ? C7 C8 1.403(6) . ? C7 C15 1.489(6) . ? C8 C9 1.400(6) . ? C8 C20 1.489(6) . ? C9 C10 1.495(6) . ? C10 C11 1.395(6) . ? C11 C12 1.393(6) . ? C11 H11A 0.9300 . ? C12 C13 1.363(7) . ? C12 H12A 0.9300 . ? C13 C14 1.365(7) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C16 1.376(7) . ? C15 C19 1.390(7) . ? C16 C17 1.392(8) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C19 1.356(7) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.373(7) . ? C20 C24 1.380(7) . ? C21 C22 1.417(9) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.395(9) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C101 C102 1.377(7) . ? C101 C106 1.381(6) . ? C102 C103 1.379(7) . ? C102 H10A 0.9300 . ? C103 C104 1.353(9) . ? C103 H10B 0.9300 . ? C104 C105 1.347(9) . ? C104 H10C 0.9300 . ? C105 C106 1.378(7) . ? C105 H10D 0.9300 . ? C106 H10E 0.9300 . ? C111 C116 1.376(6) . ? C111 C112 1.384(6) . ? C112 C113 1.378(7) . ? C112 H11B 0.9300 . ? C113 C114 1.379(8) . ? C113 H11C 0.9300 . ? C114 C115 1.359(7) . ? C114 H11D 0.9300 . ? C115 C116 1.371(7) . ? C115 H11E 0.9300 . ? C116 H11F 0.9300 . ? C201 C202 1.368(7) . ? C201 C206 1.401(7) . ? C202 C203 1.386(7) . ? C202 H20A 0.9300 . ? C203 C204 1.380(9) . ? C203 H20B 0.9300 . ? C204 C205 1.351(9) . ? C204 H20C 0.9300 . ? C205 C206 1.383(7) . ? C205 H20D 0.9300 . ? C206 H20E 0.9300 . ? C211 C212 1.372(7) . ? C211 C216 1.378(6) . ? C212 C213 1.375(8) . ? C212 H21B 0.9300 . ? C213 C214 1.338(8) . ? C213 H21C 0.9300 . ? C214 C215 1.350(9) . ? C214 H21D 0.9300 . ? C215 C216 1.374(8) . ? C215 H21E 0.9300 . ? C216 H21F 0.9300 . ? C301 C302 1.372(6) . ? C301 C306 1.388(6) . ? C302 C303 1.385(6) . ? C302 H30A 0.9300 . ? C303 C304 1.372(7) . ? C303 H30B 0.9300 . ? C304 C305 1.368(7) . ? C304 H30C 0.9300 . ? C305 C306 1.380(7) . ? C305 H30D 0.9300 . ? C306 H30E 0.9300 . ? C311 C316 1.370(7) . ? C311 C312 1.382(6) . ? C312 C313 1.376(7) . ? C312 H31A 0.9300 . ? C313 C314 1.371(8) . ? C313 H31B 0.9300 . ? C314 C315 1.350(7) . ? C314 H31C 0.9300 . ? C315 C316 1.378(7) . ? C315 H31D 0.9300 . ? C316 H31E 0.9300 . ? C401 C406 1.373(7) . ? C401 C402 1.383(6) . ? C402 C403 1.378(8) . ? C402 H40A 0.9300 . ? C403 C404 1.373(9) . ? C403 H40B 0.9300 . ? C404 C405 1.352(8) . ? C404 H40C 0.9300 . ? C405 C406 1.377(7) . ? C405 H40D 0.9300 . ? C406 H40E 0.9300 . ? C411 C416 1.371(6) . ? C411 C412 1.373(7) . ? C412 C413 1.375(7) . ? C412 H41A 0.9300 . ? C413 C414 1.365(8) . ? C413 H41B 0.9300 . ? C414 C415 1.362(9) . ? C414 H41C 0.9300 . ? C415 C416 1.383(9) . ? C415 H41D 0.9300 . ? C416 H41E 0.9300 . ? C1S Cl2 1.677(9) . ? C1S Cl1 1.687(10) . ? C1S H1SA 0.9700 . ? C1S H1SB 0.9700 . ? N7 O3 1.102(7) . ? N7 O1 1.180(8) . ? N7 O2 1.200(6) . ? O4 N8 1.178(11) . ? O5 N8 1.176(11) . ? O6 N8 1.177(11) . ? O4' N8' 1.208(10) . ? O5' N8' 1.199(11) . ? O6' N8' 1.202(11) . ? 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 N2 Cu1 N1 76.04(13) . . ? N2 Cu1 P1 118.70(9) . . ? N1 Cu1 P1 116.01(10) . . ? N2 Cu1 P2 104.96(9) . . ? N1 Cu1 P2 106.47(9) . . ? P1 Cu1 P2 124.21(5) . . ? N3 Cu2 N4 76.89(13) . . ? N3 Cu2 P3 112.70(9) . . ? N4 Cu2 P3 113.92(10) . . ? N3 Cu2 P4 104.91(9) . . ? N4 Cu2 P4 104.74(9) . . ? P3 Cu2 P4 130.57(5) . . ? C101 P1 C111 103.12(19) . . ? C101 P1 C26 106.08(19) . . ? C111 P1 C26 100.04(19) . . ? C101 P1 Cu1 118.00(16) . . ? C111 P1 Cu1 113.09(14) . . ? C26 P1 Cu1 114.44(13) . . ? C211 P2 C201 104.2(2) . . ? C211 P2 C25 104.1(2) . . ? C201 P2 C25 104.4(2) . . ? C211 P2 Cu1 122.47(16) . . ? C201 P2 Cu1 106.50(14) . . ? C25 P2 Cu1 113.51(14) . . ? C26 P3 C311 101.61(19) . . ? C26 P3 C301 103.21(18) . . ? C311 P3 C301 104.63(19) . . ? C26 P3 Cu2 118.24(14) . . ? C311 P3 Cu2 113.41(13) . . ? C301 P3 Cu2 114.05(15) . . ? C401 P4 C411 105.7(2) . . ? C401 P4 C25 106.3(2) . . ? C411 P4 C25 102.9(2) . . ? C401 P4 Cu2 118.83(16) . . ? C411 P4 Cu2 108.68(15) . . ? C25 P4 Cu2 113.13(14) . . ? C5 N1 C1 118.1(4) . . ? C5 N1 Cu1 114.3(3) . . ? C1 N1 Cu1 125.3(3) . . ? C6 N2 N3 120.6(3) . . ? C6 N2 Cu1 118.4(3) . . ? N3 N2 Cu1 120.4(3) . . ? C9 N3 N2 120.9(3) . . ? C9 N3 Cu2 119.3(3) . . ? N2 N3 Cu2 119.3(3) . . ? C14 N4 C10 118.4(4) . . ? C14 N4 Cu2 125.0(3) . . ? C10 N4 Cu2 114.8(3) . . ? C18 N5 C17 115.9(6) . . ? C23 N6 C22 117.0(6) . . ? N1 C1 C2 122.2(5) . . ? N1 C1 H1A 118.9 . . ? C2 C1 H1A 118.9 . . ? C3 C2 C1 120.0(5) . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C2 C3 C4 118.2(5) . . ? C2 C3 H3A 120.9 . . ? C4 C3 H3A 120.9 . . ? C3 C4 C5 119.1(5) . . ? C3 C4 H4A 120.5 . . ? C5 C4 H4A 120.5 . . ? N1 C5 C4 122.2(4) . . ? N1 C5 C6 114.9(4) . . ? C4 C5 C6 122.6(4) . . ? N2 C6 C7 121.3(3) . . ? N2 C6 C5 112.6(4) . . ? C7 C6 C5 126.1(4) . . ? C8 C7 C6 116.9(4) . . ? C8 C7 C15 119.6(4) . . ? C6 C7 C15 123.3(4) . . ? C9 C8 C7 117.7(4) . . ? C9 C8 C20 121.9(4) . . ? C7 C8 C20 120.1(4) . . ? N3 C9 C8 121.0(4) . . ? N3 C9 C10 112.1(4) . . ? C8 C9 C10 126.9(4) . . ? N4 C10 C11 121.2(4) . . ? N4 C10 C9 114.7(4) . . ? C11 C10 C9 124.0(4) . . ? C12 C11 C10 118.6(5) . . ? C12 C11 H11A 120.7 . . ? C10 C11 H11A 120.7 . . ? C13 C12 C11 119.5(5) . . ? C13 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C12 C13 C14 118.9(4) . . ? C12 C13 H13A 120.6 . . ? C14 C13 H13A 120.6 . . ? N4 C14 C13 123.5(5) . . ? N4 C14 H14A 118.3 . . ? C13 C14 H14A 118.3 . . ? C16 C15 C19 116.9(5) . . ? C16 C15 C7 119.7(5) . . ? C19 C15 C7 123.4(4) . . ? C15 C16 C17 118.3(6) . . ? C15 C16 H16A 120.9 . . ? C17 C16 H16A 120.9 . . ? N5 C17 C16 123.9(6) . . ? N5 C17 H17A 118.0 . . ? C16 C17 H17A 118.0 . . ? N5 C18 C19 125.0(6) . . ? N5 C18 H18A 117.5 . . ? C19 C18 H18A 117.5 . . ? C18 C19 C15 119.9(6) . . ? C18 C19 H19A 120.1 . . ? C15 C19 H19A 120.1 . . ? C21 C20 C24 118.8(5) . . ? C21 C20 C8 120.1(5) . . ? C24 C20 C8 121.2(5) . . ? C20 C21 C22 117.5(6) . . ? C20 C21 H21A 121.2 . . ? C22 C21 H21A 121.2 . . ? N6 C22 C21 123.6(7) . . ? N6 C22 H22A 118.2 . . ? C21 C22 H22A 118.2 . . ? N6 C23 C24 123.9(7) . . ? N6 C23 H23A 118.0 . . ? C24 C23 H23A 118.0 . . ? C20 C24 C23 119.1(6) . . ? C20 C24 H24A 120.4 . . ? C23 C24 H24A 120.4 . . ? P2 C25 P4 113.7(2) . . ? P2 C25 H25A 108.8 . . ? P4 C25 H25A 108.8 . . ? P2 C25 H25B 108.8 . . ? P4 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? P3 C26 P1 116.4(2) . . ? P3 C26 H26A 108.2 . . ? P1 C26 H26A 108.2 . . ? P3 C26 H26B 108.2 . . ? P1 C26 H26B 108.2 . . ? H26A C26 H26B 107.3 . . ? C102 C101 C106 119.3(4) . . ? C102 C101 P1 117.5(3) . . ? C106 C101 P1 123.2(4) . . ? C103 C102 C101 120.2(5) . . ? C103 C102 H10A 119.9 . . ? C101 C102 H10A 119.9 . . ? C104 C103 C102 119.7(6) . . ? C104 C103 H10B 120.2 . . ? C102 C103 H10B 120.2 . . ? C105 C104 C103 120.8(5) . . ? C105 C104 H10C 119.6 . . ? C103 C104 H10C 119.6 . . ? C104 C105 C106 120.8(6) . . ? C104 C105 H10D 119.6 . . ? C106 C105 H10D 119.6 . . ? C105 C106 C101 119.2(5) . . ? C105 C106 H10E 120.4 . . ? C101 C106 H10E 120.4 . . ? C116 C111 C112 118.5(4) . . ? C116 C111 P1 123.3(3) . . ? C112 C111 P1 118.1(4) . . ? C113 C112 C111 120.7(5) . . ? C113 C112 H11B 119.7 . . ? C111 C112 H11B 119.7 . . ? C112 C113 C114 119.4(5) . . ? C112 C113 H11C 120.3 . . ? C114 C113 H11C 120.3 . . ? C115 C114 C113 120.3(5) . . ? C115 C114 H11D 119.9 . . ? C113 C114 H11D 119.9 . . ? C114 C115 C116 120.2(5) . . ? C114 C115 H11E 119.9 . . ? C116 C115 H11E 119.9 . . ? C115 C116 C111 120.9(4) . . ? C115 C116 H11F 119.6 . . ? C111 C116 H11F 119.6 . . ? C202 C201 C206 119.3(4) . . ? C202 C201 P2 121.8(4) . . ? C206 C201 P2 117.8(4) . . ? C201 C202 C203 120.1(6) . . ? C201 C202 H20A 120.0 . . ? C203 C202 H20A 120.0 . . ? C204 C203 C202 120.3(6) . . ? C204 C203 H20B 119.8 . . ? C202 C203 H20B 119.8 . . ? C205 C204 C203 119.9(6) . . ? C205 C204 H20C 120.1 . . ? C203 C204 H20C 120.1 . . ? C204 C205 C206 120.9(6) . . ? C204 C205 H20D 119.6 . . ? C206 C205 H20D 119.6 . . ? C205 C206 C201 119.5(6) . . ? C205 C206 H20E 120.2 . . ? C201 C206 H20E 120.2 . . ? C212 C211 C216 116.9(5) . . ? C212 C211 P2 119.1(4) . . ? C216 C211 P2 123.9(4) . . ? C211 C212 C213 120.6(5) . . ? C211 C212 H21B 119.7 . . ? C213 C212 H21B 119.7 . . ? C214 C213 C212 121.6(6) . . ? C214 C213 H21C 119.2 . . ? C212 C213 H21C 119.2 . . ? C213 C214 C215 119.1(6) . . ? C213 C214 H21D 120.4 . . ? C215 C214 H21D 120.4 . . ? C214 C215 C216 120.4(6) . . ? C214 C215 H21E 119.8 . . ? C216 C215 H21E 119.8 . . ? C215 C216 C211 121.4(6) . . ? C215 C216 H21F 119.3 . . ? C211 C216 H21F 119.3 . . ? C302 C301 C306 119.1(4) . . ? C302 C301 P3 118.9(3) . . ? C306 C301 P3 122.0(4) . . ? C301 C302 C303 121.3(4) . . ? C301 C302 H30A 119.4 . . ? C303 C302 H30A 119.4 . . ? C304 C303 C302 119.2(5) . . ? C304 C303 H30B 120.4 . . ? C302 C303 H30B 120.4 . . ? C305 C304 C303 120.1(5) . . ? C305 C304 H30C 119.9 . . ? C303 C304 H30C 119.9 . . ? C304 C305 C306 120.9(5) . . ? C304 C305 H30D 119.5 . . ? C306 C305 H30D 119.5 . . ? C305 C306 C301 119.4(5) . . ? C305 C306 H30E 120.3 . . ? C301 C306 H30E 120.3 . . ? C316 C311 C312 118.2(4) . . ? C316 C311 P3 124.2(3) . . ? C312 C311 P3 117.6(4) . . ? C313 C312 C311 120.5(5) . . ? C313 C312 H31A 119.7 . . ? C311 C312 H31A 119.7 . . ? C314 C313 C312 120.2(5) . . ? C314 C313 H31B 119.9 . . ? C312 C313 H31B 119.9 . . ? C315 C314 C313 119.6(5) . . ? C315 C314 H31C 120.2 . . ? C313 C314 H31C 120.2 . . ? C314 C315 C316 120.5(6) . . ? C314 C315 H31D 119.8 . . ? C316 C315 H31D 119.8 . . ? C311 C316 C315 121.0(5) . . ? C311 C316 H31E 119.5 . . ? C315 C316 H31E 119.5 . . ? C406 C401 C402 117.6(5) . . ? C406 C401 P4 119.2(4) . . ? C402 C401 P4 123.2(4) . . ? C403 C402 C401 120.2(6) . . ? C403 C402 H40A 119.9 . . ? C401 C402 H40A 119.9 . . ? C404 C403 C402 120.9(6) . . ? C404 C403 H40B 119.6 . . ? C402 C403 H40B 119.6 . . ? C405 C404 C403 119.4(6) . . ? C405 C404 H40C 120.3 . . ? C403 C404 H40C 120.3 . . ? C404 C405 C406 119.9(6) . . ? C404 C405 H40D 120.1 . . ? C406 C405 H40D 120.1 . . ? C401 C406 C405 122.0(5) . . ? C401 C406 H40E 119.0 . . ? C405 C406 H40E 119.0 . . ? C416 C411 C412 118.3(5) . . ? C416 C411 P4 121.2(4) . . ? C412 C411 P4 119.8(3) . . ? C411 C412 C413 121.4(5) . . ? C411 C412 H41A 119.3 . . ? C413 C412 H41A 119.3 . . ? C414 C413 C412 119.9(6) . . ? C414 C413 H41B 120.1 . . ? C412 C413 H41B 120.1 . . ? C415 C414 C413 119.3(6) . . ? C415 C414 H41C 120.3 . . ? C413 C414 H41C 120.3 . . ? C414 C415 C416 120.8(6) . . ? C414 C415 H41D 119.6 . . ? C416 C415 H41D 119.6 . . ? C411 C416 C415 120.2(6) . . ? C411 C416 H41E 119.9 . . ? C415 C416 H41E 119.9 . . ? Cl2 C1S Cl1 113.3(7) . . ? Cl2 C1S H1SA 108.9 . . ? Cl1 C1S H1SA 108.9 . . ? Cl2 C1S H1SB 108.9 . . ? Cl1 C1S H1SB 108.9 . . ? H1SA C1S H1SB 107.7 . . ? O3 N7 O1 122.2(9) . . ? O3 N7 O2 126.9(10) . . ? O1 N7 O2 110.6(8) . . ? O5 N8 O6 119.6(8) . . ? O5 N8 O4 121.1(8) . . ? O6 N8 O4 119.2(7) . . ? O5' N8' O6' 121.0(8) . . ? O5' N8' O4' 119.0(7) . . ? O6' N8' O4' 119.3(7) . . ? 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 N2 Cu1 P1 C101 53.54(18) . . . . ? N1 Cu1 P1 C101 -34.24(19) . . . . ? P2 Cu1 P1 C101 -169.73(15) . . . . ? N2 Cu1 P1 C111 173.95(17) . . . . ? N1 Cu1 P1 C111 86.17(18) . . . . ? P2 Cu1 P1 C111 -49.32(15) . . . . ? N2 Cu1 P1 C26 -72.35(18) . . . . ? N1 Cu1 P1 C26 -160.13(18) . . . . ? P2 Cu1 P1 C26 64.38(16) . . . . ? N2 Cu1 P2 C211 152.40(19) . . . . ? N1 Cu1 P2 C211 -128.1(2) . . . . ? P1 Cu1 P2 C211 10.88(18) . . . . ? N2 Cu1 P2 C201 -88.2(2) . . . . ? N1 Cu1 P2 C201 -8.6(2) . . . . ? P1 Cu1 P2 C201 130.30(18) . . . . ? N2 Cu1 P2 C25 26.08(18) . . . . ? N1 Cu1 P2 C25 105.63(18) . . . . ? P1 Cu1 P2 C25 -115.44(15) . . . . ? N3 Cu2 P3 C26 82.50(19) . . . . ? N4 Cu2 P3 C26 167.72(18) . . . . ? P4 Cu2 P3 C26 -54.01(17) . . . . ? N3 Cu2 P3 C311 -158.72(18) . . . . ? N4 Cu2 P3 C311 -73.50(19) . . . . ? P4 Cu2 P3 C311 64.77(16) . . . . ? N3 Cu2 P3 C301 -39.08(17) . . . . ? N4 Cu2 P3 C301 46.14(18) . . . . ? P4 Cu2 P3 C301 -175.59(14) . . . . ? N3 Cu2 P4 C401 -159.67(19) . . . . ? N4 Cu2 P4 C401 120.27(19) . . . . ? P3 Cu2 P4 C401 -20.74(18) . . . . ? N3 Cu2 P4 C411 79.54(19) . . . . ? N4 Cu2 P4 C411 -0.52(19) . . . . ? P3 Cu2 P4 C411 -141.54(16) . . . . ? N3 Cu2 P4 C25 -34.04(19) . . . . ? N4 Cu2 P4 C25 -114.10(19) . . . . ? P3 Cu2 P4 C25 104.88(17) . . . . ? N2 Cu1 N1 C5 3.6(3) . . . . ? P1 Cu1 N1 C5 119.1(3) . . . . ? P2 Cu1 N1 C5 -98.1(3) . . . . ? N2 Cu1 N1 C1 165.8(4) . . . . ? P1 Cu1 N1 C1 -78.7(4) . . . . ? P2 Cu1 N1 C1 64.1(4) . . . . ? N1 Cu1 N2 C6 9.3(3) . . . . ? P1 Cu1 N2 C6 -102.9(3) . . . . ? P2 Cu1 N2 C6 113.0(3) . . . . ? N1 Cu1 N2 N3 -179.2(3) . . . . ? P1 Cu1 N2 N3 68.5(3) . . . . ? P2 Cu1 N2 N3 -75.6(3) . . . . ? C6 N2 N3 C9 0.7(5) . . . . ? Cu1 N2 N3 C9 -170.6(3) . . . . ? C6 N2 N3 Cu2 172.7(3) . . . . ? Cu1 N2 N3 Cu2 1.5(4) . . . . ? N4 Cu2 N3 C9 -8.2(3) . . . . ? P3 Cu2 N3 C9 102.5(3) . . . . ? P4 Cu2 N3 C9 -110.2(3) . . . . ? N4 Cu2 N3 N2 179.7(3) . . . . ? P3 Cu2 N3 N2 -69.6(3) . . . . ? P4 Cu2 N3 N2 77.6(3) . . . . ? N3 Cu2 N4 C14 -166.1(3) . . . . ? P3 Cu2 N4 C14 84.6(3) . . . . ? P4 Cu2 N4 C14 -63.9(3) . . . . ? N3 Cu2 N4 C10 -1.9(3) . . . . ? P3 Cu2 N4 C10 -111.2(3) . . . . ? P4 Cu2 N4 C10 100.3(3) . . . . ? C5 N1 C1 C2 3.6(7) . . . . ? Cu1 N1 C1 C2 -158.0(4) . . . . ? N1 C1 C2 C3 -0.3(8) . . . . ? C1 C2 C3 C4 -2.4(8) . . . . ? C2 C3 C4 C5 1.8(8) . . . . ? C1 N1 C5 C4 -4.2(6) . . . . ? Cu1 N1 C5 C4 159.4(4) . . . . ? C1 N1 C5 C6 -178.0(4) . . . . ? Cu1 N1 C5 C6 -14.4(4) . . . . ? C3 C4 C5 N1 1.5(7) . . . . ? C3 C4 C5 C6 174.9(4) . . . . ? N3 N2 C6 C7 -11.5(6) . . . . ? Cu1 N2 C6 C7 159.9(3) . . . . ? N3 N2 C6 C5 169.3(3) . . . . ? Cu1 N2 C6 C5 -19.3(4) . . . . ? N1 C5 C6 N2 22.0(5) . . . . ? C4 C5 C6 N2 -151.8(4) . . . . ? N1 C5 C6 C7 -157.1(4) . . . . ? C4 C5 C6 C7 29.1(7) . . . . ? N2 C6 C7 C8 12.3(6) . . . . ? C5 C6 C7 C8 -168.7(4) . . . . ? N2 C6 C7 C15 -161.7(4) . . . . ? C5 C6 C7 C15 17.3(7) . . . . ? C6 C7 C8 C9 -2.8(6) . . . . ? C15 C7 C8 C9 171.5(4) . . . . ? C6 C7 C8 C20 -176.9(4) . . . . ? C15 C7 C8 C20 -2.7(6) . . . . ? N2 N3 C9 C8 9.0(6) . . . . ? Cu2 N3 C9 C8 -163.0(3) . . . . ? N2 N3 C9 C10 -172.4(3) . . . . ? Cu2 N3 C9 C10 15.6(4) . . . . ? C7 C8 C9 N3 -7.5(6) . . . . ? C20 C8 C9 N3 166.5(4) . . . . ? C7 C8 C9 C10 174.1(4) . . . . ? C20 C8 C9 C10 -11.9(7) . . . . ? C14 N4 C10 C11 0.3(6) . . . . ? Cu2 N4 C10 C11 -165.0(3) . . . . ? C14 N4 C10 C9 175.7(4) . . . . ? Cu2 N4 C10 C9 10.3(4) . . . . ? N3 C9 C10 N4 -16.6(5) . . . . ? C8 C9 C10 N4 161.9(4) . . . . ? N3 C9 C10 C11 158.5(4) . . . . ? C8 C9 C10 C11 -22.9(7) . . . . ? N4 C10 C11 C12 -1.5(7) . . . . ? C9 C10 C11 C12 -176.4(4) . . . . ? C10 C11 C12 C13 1.2(8) . . . . ? C11 C12 C13 C14 0.3(8) . . . . ? C10 N4 C14 C13 1.3(6) . . . . ? Cu2 N4 C14 C13 165.0(3) . . . . ? C12 C13 C14 N4 -1.6(7) . . . . ? C8 C7 C15 C16 -102.5(5) . . . . ? C6 C7 C15 C16 71.4(6) . . . . ? C8 C7 C15 C19 75.0(6) . . . . ? C6 C7 C15 C19 -111.1(5) . . . . ? C19 C15 C16 C17 -3.0(7) . . . . ? C7 C15 C16 C17 174.6(4) . . . . ? C18 N5 C17 C16 -1.1(9) . . . . ? C15 C16 C17 N5 2.9(9) . . . . ? C17 N5 C18 C19 -0.3(9) . . . . ? N5 C18 C19 C15 0.0(9) . . . . ? C16 C15 C19 C18 1.8(7) . . . . ? C7 C15 C19 C18 -175.8(4) . . . . ? C9 C8 C20 C21 -76.4(6) . . . . ? C7 C8 C20 C21 97.5(5) . . . . ? C9 C8 C20 C24 103.2(5) . . . . ? C7 C8 C20 C24 -82.9(6) . . . . ? C24 C20 C21 C22 -1.1(7) . . . . ? C8 C20 C21 C22 178.5(4) . . . . ? C23 N6 C22 C21 2.2(11) . . . . ? C20 C21 C22 N6 -1.1(9) . . . . ? C22 N6 C23 C24 -1.0(11) . . . . ? C21 C20 C24 C23 2.2(8) . . . . ? C8 C20 C24 C23 -177.4(5) . . . . ? N6 C23 C24 C20 -1.1(10) . . . . ? C211 P2 C25 P4 -75.7(3) . . . . ? C201 P2 C25 P4 175.3(2) . . . . ? Cu1 P2 C25 P4 59.8(3) . . . . ? C401 P4 C25 P2 76.2(3) . . . . ? C411 P4 C25 P2 -173.0(2) . . . . ? Cu2 P4 C25 P2 -55.9(3) . . . . ? C311 P3 C26 P1 -176.3(2) . . . . ? C301 P3 C26 P1 75.4(3) . . . . ? Cu2 P3 C26 P1 -51.5(3) . . . . ? C101 P1 C26 P3 -87.5(3) . . . . ? C111 P1 C26 P3 165.6(2) . . . . ? Cu1 P1 C26 P3 44.4(3) . . . . ? C111 P1 C101 C102 -103.9(4) . . . . ? C26 P1 C101 C102 151.4(4) . . . . ? Cu1 P1 C101 C102 21.5(4) . . . . ? C111 P1 C101 C106 74.9(4) . . . . ? C26 P1 C101 C106 -29.8(5) . . . . ? Cu1 P1 C101 C106 -159.6(4) . . . . ? C106 C101 C102 C103 -0.8(8) . . . . ? P1 C101 C102 C103 178.1(5) . . . . ? C101 C102 C103 C104 0.7(10) . . . . ? C102 C103 C104 C105 -0.6(11) . . . . ? C103 C104 C105 C106 0.7(11) . . . . ? C104 C105 C106 C101 -0.8(9) . . . . ? C102 C101 C106 C105 0.8(8) . . . . ? P1 C101 C106 C105 -178.0(4) . . . . ? C101 P1 C111 C116 -86.5(4) . . . . ? C26 P1 C111 C116 22.8(4) . . . . ? Cu1 P1 C111 C116 144.9(3) . . . . ? C101 P1 C111 C112 96.4(4) . . . . ? C26 P1 C111 C112 -154.4(3) . . . . ? Cu1 P1 C111 C112 -32.2(4) . . . . ? C116 C111 C112 C113 -2.6(7) . . . . ? P1 C111 C112 C113 174.7(4) . . . . ? C111 C112 C113 C114 1.0(8) . . . . ? C112 C113 C114 C115 0.6(9) . . . . ? C113 C114 C115 C116 -0.5(8) . . . . ? C114 C115 C116 C111 -1.1(7) . . . . ? C112 C111 C116 C115 2.6(7) . . . . ? P1 C111 C116 C115 -174.5(3) . . . . ? C211 P2 C201 C202 -152.2(4) . . . . ? C25 P2 C201 C202 -43.2(4) . . . . ? Cu1 P2 C201 C202 77.1(4) . . . . ? C211 P2 C201 C206 40.0(4) . . . . ? C25 P2 C201 C206 148.9(4) . . . . ? Cu1 P2 C201 C206 -90.7(4) . . . . ? C206 C201 C202 C203 0.2(7) . . . . ? P2 C201 C202 C203 -167.5(4) . . . . ? C201 C202 C203 C204 0.7(9) . . . . ? C202 C203 C204 C205 -1.4(10) . . . . ? C203 C204 C205 C206 1.1(10) . . . . ? C204 C205 C206 C201 -0.2(9) . . . . ? C202 C201 C206 C205 -0.4(7) . . . . ? P2 C201 C206 C205 167.7(4) . . . . ? C201 P2 C211 C212 -134.1(4) . . . . ? C25 P2 C211 C212 116.8(4) . . . . ? Cu1 P2 C211 C212 -13.6(5) . . . . ? C201 P2 C211 C216 49.5(5) . . . . ? C25 P2 C211 C216 -59.6(5) . . . . ? Cu1 P2 C211 C216 170.0(4) . . . . ? C216 C211 C212 C213 0.2(8) . . . . ? P2 C211 C212 C213 -176.4(5) . . . . ? C211 C212 C213 C214 -0.1(10) . . . . ? C212 C213 C214 C215 0.6(11) . . . . ? C213 C214 C215 C216 -1.4(11) . . . . ? C214 C215 C216 C211 1.6(11) . . . . ? C212 C211 C216 C215 -1.0(9) . . . . ? P2 C211 C216 C215 175.5(5) . . . . ? C26 P3 C301 C302 -89.2(4) . . . . ? C311 P3 C301 C302 164.9(3) . . . . ? Cu2 P3 C301 C302 40.4(4) . . . . ? C26 P3 C301 C306 91.7(4) . . . . ? C311 P3 C301 C306 -14.3(4) . . . . ? Cu2 P3 C301 C306 -138.7(3) . . . . ? C306 C301 C302 C303 -0.4(7) . . . . ? P3 C301 C302 C303 -179.5(4) . . . . ? C301 C302 C303 C304 1.3(8) . . . . ? C302 C303 C304 C305 -0.7(8) . . . . ? C303 C304 C305 C306 -0.7(8) . . . . ? C304 C305 C306 C301 1.6(8) . . . . ? C302 C301 C306 C305 -1.1(7) . . . . ? P3 C301 C306 C305 178.1(4) . . . . ? C26 P3 C311 C316 -0.8(4) . . . . ? C301 P3 C311 C316 106.3(4) . . . . ? Cu2 P3 C311 C316 -128.8(4) . . . . ? C26 P3 C311 C312 178.0(3) . . . . ? C301 P3 C311 C312 -74.9(4) . . . . ? Cu2 P3 C311 C312 50.0(4) . . . . ? C316 C311 C312 C313 -0.3(7) . . . . ? P3 C311 C312 C313 -179.2(4) . . . . ? C311 C312 C313 C314 1.0(8) . . . . ? C312 C313 C314 C315 -0.9(8) . . . . ? C313 C314 C315 C316 0.2(9) . . . . ? C312 C311 C316 C315 -0.4(8) . . . . ? P3 C311 C316 C315 178.3(4) . . . . ? C314 C315 C316 C311 0.5(9) . . . . ? C411 P4 C401 C406 123.4(4) . . . . ? C25 P4 C401 C406 -127.8(4) . . . . ? Cu2 P4 C401 C406 1.1(4) . . . . ? C411 P4 C401 C402 -57.1(5) . . . . ? C25 P4 C401 C402 51.7(5) . . . . ? Cu2 P4 C401 C402 -179.4(4) . . . . ? C406 C401 C402 C403 1.1(8) . . . . ? P4 C401 C402 C403 -178.5(5) . . . . ? C401 C402 C403 C404 -0.1(10) . . . . ? C402 C403 C404 C405 -0.7(11) . . . . ? C403 C404 C405 C406 0.5(10) . . . . ? C402 C401 C406 C405 -1.3(8) . . . . ? P4 C401 C406 C405 178.3(4) . . . . ? C404 C405 C406 C401 0.5(9) . . . . ? C401 P4 C411 C416 -25.0(5) . . . . ? C25 P4 C411 C416 -136.2(4) . . . . ? Cu2 P4 C411 C416 103.6(4) . . . . ? C401 P4 C411 C412 164.3(4) . . . . ? C25 P4 C411 C412 53.0(4) . . . . ? Cu2 P4 C411 C412 -67.1(4) . . . . ? C416 C411 C412 C413 -0.3(7) . . . . ? P4 C411 C412 C413 170.7(4) . . . . ? C411 C412 C413 C414 0.7(8) . . . . ? C412 C413 C414 C415 -0.4(9) . . . . ? C413 C414 C415 C416 -0.1(10) . . . . ? C412 C411 C416 C415 -0.3(8) . . . . ? P4 C411 C416 C415 -171.2(5) . . . . ? C414 C415 C416 C411 0.5(10) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 23.44 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.641 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.077 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.153 0.323 0.272 129 13 ' ' 2 0.152 0.677 0.728 128 13 ' ' 3 0.041 0.963 0.508 9 0 ' ' 4 0.186 0.877 0.639 13 1 ' ' 5 0.347 0.177 0.772 128 13 ' ' 6 0.314 0.377 0.861 13 1 ' ' 7 0.459 0.463 0.992 9 0 ' ' 8 0.653 0.823 0.228 129 13 ' ' 9 0.548 0.544 0.009 9 0 ' ' 10 0.686 0.623 0.139 12 1 ' ' 11 0.814 0.123 0.361 12 1 ' ' 12 0.951 0.044 0.491 8 0 ' ' _platon_squeeze_details ; ;