# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Craig Rice' _publ_contact_author_address ; Department of Chemical and Biological Sciences University of Huddersfield Queensgate Huddersfield West Yorkshire HD1 3DH UK ; _publ_contact_author_email C.R.RICE@HUD.AC.UK _publ_section_title ; A Dinuclear Double Helicate with a Reprogrammable Pitch Length. ; loop_ _publ_author_name 'Craig Rice' 'Christian J. Baylies' 'J. Jeffery' 'T. A. Miller' 'T. Riis-Johanessen' data_britannm _database_code_depnum_ccdc_archive 'CCDC 270151' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C77 H76.50 Cl4 Cu2 N14.50 O28.50 S4' _chemical_formula_weight 2058.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5921(3) _cell_length_b 17.9777(5) _cell_length_c 18.9909(5) _cell_angle_alpha 72.997(2) _cell_angle_beta 82.980(2) _cell_angle_gamma 85.769(2) _cell_volume 4400.87(19) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 5.144 _cell_measurement_theta_max 140.719 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2116 _exptl_absorpt_coefficient_mu 3.360 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.2121 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1990)' _exptl_special_details ; The complex cation features two Cu(II) coordination domains incorporated into a metallo-helical array with 18-crown-6 macrocycles spanning the central bipyrings on each side of the molecule. All atoms in the complex molecule are well resolved with only marginal disorder in one of the crown ether macrocycles (resolved into two positions with 0.55:0.45 site ocupancies). Two of the four non-coordinating perchlorate anions, ClO4(3) and ClO4(4), are disordered over two positions [ClO4(3a)/(3b) and ClO4(4a)/(4b)] and were refined using geometric similarity restraints (SAME/SADI) and ADP restraints (SIMU and ISOR). A total of 2.5 acetonitrile molecules were located in the residual electron density and a remaining electron density peak was refined as a (0.5 site occupancy) water molecule. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31372 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_sigmaI/netI 0.0666 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 70.35 _reflns_number_total 14656 _reflns_number_gt 11800 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHEXTL' _computing_publication_material 'Bruker SHEXTL' _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^)+(0.1381P)^2^+13.6171P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14656 _refine_ls_number_parameters 1282 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0830 _refine_ls_wR_factor_ref 0.2429 _refine_ls_wR_factor_gt 0.2307 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.84034(5) 0.86705(5) 0.19413(4) 0.0294(2) Uani 1 1 d . . . Cu2 Cu 0.64340(5) 0.64192(5) 0.32263(4) 0.0308(2) Uani 1 1 d . . . N11 N 0.9455(4) 0.8834(3) 0.0947(2) 0.0341(10) Uani 1 1 d . . . C12 C 0.9029(5) 0.9097(3) 0.0311(3) 0.0361(12) Uani 1 1 d . . . C13 C 0.9581(5) 0.9220(4) -0.0380(3) 0.0436(15) Uani 1 1 d . . . H105 H 0.9270 0.9400 -0.0824 0.052 Uiso 1 1 calc R . . C14 C 1.0594(6) 0.9073(4) -0.0400(4) 0.0495(16) Uani 1 1 d . . . H104 H 1.0987 0.9150 -0.0863 0.059 Uiso 1 1 calc R . . C15 C 1.1036(5) 0.8818(4) 0.0242(4) 0.0476(15) Uani 1 1 d . . . H103 H 1.1733 0.8723 0.0234 0.057 Uiso 1 1 calc R . . C16 C 1.0435(5) 0.8701(4) 0.0907(3) 0.0402(13) Uani 1 1 d . . . H102 H 1.0736 0.8517 0.1355 0.048 Uiso 1 1 calc R . . N21 N 0.7557(3) 0.9061(3) 0.1156(2) 0.0322(10) Uani 1 1 d . . . C22 C 0.6593(4) 0.9189(3) 0.1244(3) 0.0348(12) Uani 1 1 d . . . S23 S 0.60990(12) 0.95247(10) 0.04134(8) 0.0465(4) Uani 1 1 d . . . C24 C 0.7249(5) 0.9484(4) -0.0054(3) 0.0457(15) Uani 1 1 d . . . H108 H 0.7382 0.9620 -0.0578 0.055 Uiso 1 1 calc R . . C25 C 0.7950(5) 0.9229(3) 0.0427(3) 0.0362(13) Uani 1 1 d . . . N31 N 0.6666(3) 0.8624(3) 0.2512(2) 0.0288(9) Uani 1 1 d . . . C32 C 0.6295(4) 0.8443(3) 0.3217(3) 0.0275(11) Uani 1 1 d . . . C33 C 0.5316(4) 0.8653(3) 0.3446(3) 0.0295(11) Uani 1 1 d . . . C34 C 0.4718(4) 0.9068(3) 0.2893(3) 0.0352(12) Uani 1 1 d . . . H114 H 0.4052 0.9219 0.3023 0.042 Uiso 1 1 calc R . . C35 C 0.5106(4) 0.9251(4) 0.2169(3) 0.0371(13) Uani 1 1 d . . . H113 H 0.4712 0.9534 0.1791 0.044 Uiso 1 1 calc R . . C36 C 0.6084(4) 0.9021(3) 0.1988(3) 0.0302(11) Uani 1 1 d . . . N41 N 0.7254(3) 0.7280(3) 0.3698(2) 0.0269(9) Uani 1 1 d . . . C42 C 0.6982(3) 0.7984(3) 0.3760(3) 0.0271(11) Uani 1 1 d . . . C43 C 0.7328(4) 0.8300(3) 0.4263(3) 0.0297(11) Uani 1 1 d . . . C44 C 0.8030(4) 0.7859(3) 0.4715(3) 0.0327(12) Uani 1 1 d . . . H135 H 0.8294 0.8059 0.5061 0.039 Uiso 1 1 calc R . . C45 C 0.8330(4) 0.7131(3) 0.4650(3) 0.0347(12) Uani 1 1 d . . . H136 H 0.8805 0.6823 0.4951 0.042 Uiso 1 1 calc R . . C46 C 0.7933(4) 0.6853(3) 0.4143(3) 0.0302(11) Uani 1 1 d . . . N51 N 0.7637(3) 0.5883(3) 0.3581(2) 0.0298(10) Uani 1 1 d . . . C52 C 0.8180(4) 0.6103(3) 0.4002(3) 0.0334(12) Uani 1 1 d . . . S53 S 0.91168(12) 0.54311(10) 0.42879(9) 0.0485(4) Uani 1 1 d . . . C54 C 0.8748(6) 0.4852(4) 0.3811(4) 0.0525(18) Uani 1 1 d . . . H142 H 0.9061 0.4367 0.3793 0.063 Uiso 1 1 calc R . . C55 C 0.7932(5) 0.5187(3) 0.3455(3) 0.0378(13) Uani 1 1 d . . . N61 N 0.6502(3) 0.5431(3) 0.2812(3) 0.0357(11) Uani 1 1 d . . . C62 C 0.7314(5) 0.4949(3) 0.2984(3) 0.0392(13) Uani 1 1 d . . . C63 C 0.7522(6) 0.4294(4) 0.2736(3) 0.0504(17) Uani 1 1 d . . . H146 H 0.8101 0.3973 0.2852 0.060 Uiso 1 1 calc R . . C64 C 0.6850(7) 0.4128(4) 0.2310(4) 0.058(2) Uani 1 1 d . . . H147 H 0.6959 0.3680 0.2137 0.070 Uiso 1 1 calc R . . C65 C 0.6040(6) 0.4606(4) 0.2143(4) 0.0558(18) Uani 1 1 d . . . H148 H 0.5584 0.4495 0.1849 0.067 Uiso 1 1 calc R . . C66 C 0.5876(5) 0.5253(4) 0.2400(4) 0.0476(15) Uani 1 1 d . . . H149 H 0.5303 0.5580 0.2280 0.057 Uiso 1 1 calc R . . N71 N 0.8430(3) 0.9633(3) 0.2406(2) 0.0295(10) Uani 1 1 d . . . C72 C 0.9055(4) 0.9506(3) 0.2939(3) 0.0309(12) Uani 1 1 d . . . C73 C 0.9187(4) 1.0053(4) 0.3288(3) 0.0369(13) Uani 1 1 d . . . H246 H 0.9625 0.9945 0.3662 0.044 Uiso 1 1 calc R . . C74 C 0.8672(5) 1.0767(4) 0.3088(3) 0.0406(14) Uani 1 1 d . . . H247 H 0.8758 1.1157 0.3319 0.049 Uiso 1 1 calc R . . C75 C 0.8032(5) 1.0902(4) 0.2546(3) 0.0398(13) Uani 1 1 d . . . H248 H 0.7671 1.1385 0.2396 0.048 Uiso 1 1 calc R . . C76 C 0.7933(4) 1.0319(4) 0.2231(3) 0.0356(13) Uani 1 1 d . . . H249 H 0.7483 1.0409 0.1867 0.043 Uiso 1 1 calc R . . N81 N 0.9306(3) 0.8276(3) 0.2686(2) 0.0298(10) Uani 1 1 d . . . C82 C 0.9778(4) 0.7602(3) 0.2817(3) 0.0292(11) Uani 1 1 d . . . S83 S 1.05687(9) 0.74684(9) 0.34880(7) 0.0337(3) Uani 1 1 d . . . C84 C 1.0222(4) 0.8382(4) 0.3567(3) 0.0340(12) Uani 1 1 d . . . H242 H 1.0469 0.8607 0.3903 0.041 Uiso 1 1 calc R . . C85 C 0.9554(4) 0.8741(3) 0.3091(3) 0.0295(11) Uani 1 1 d . . . N91 N 0.8719(3) 0.7301(3) 0.2062(2) 0.0298(10) Uani 1 1 d . . . C92 C 0.8442(4) 0.6871(3) 0.1666(3) 0.0314(12) Uani 1 1 d . . . C93 C 0.8986(4) 0.6217(3) 0.1559(3) 0.0357(13) Uani 1 1 d . . . C94 C 0.9855(5) 0.5993(4) 0.1909(3) 0.0411(14) Uani 1 1 d . . . H235 H 1.0252 0.5555 0.1847 0.049 Uiso 1 1 calc R . . C95 C 1.0121(4) 0.6419(4) 0.2344(3) 0.0373(13) Uani 1 1 d . . . H236 H 1.0695 0.6266 0.2599 0.045 Uiso 1 1 calc R . . C96 C 0.9557(4) 0.7069(3) 0.2414(3) 0.0307(12) Uani 1 1 d . . . N101 N 0.6699(3) 0.7095(3) 0.1857(2) 0.0310(10) Uani 1 1 d . . . C102 C 0.7465(4) 0.7109(3) 0.1362(3) 0.0336(12) Uani 1 1 d . . . C103 C 0.7398(5) 0.7357(4) 0.0593(3) 0.0386(13) Uani 1 1 d . . . C104 C 0.6465(5) 0.7567(4) 0.0350(3) 0.0469(16) Uani 1 1 d . . . H214 H 0.6388 0.7730 -0.0164 0.056 Uiso 1 1 calc R . . C105 C 0.5647(5) 0.7531(4) 0.0874(3) 0.0441(15) Uani 1 1 d . . . H213 H 0.4999 0.7658 0.0724 0.053 Uiso 1 1 calc R . . C106 C 0.5794(4) 0.7308(4) 0.1618(3) 0.0363(13) Uani 1 1 d . . . N111 N 0.5192(3) 0.6925(3) 0.2906(3) 0.0333(10) Uani 1 1 d . . . C112 C 0.4998(4) 0.7257(4) 0.2223(3) 0.0369(13) Uani 1 1 d . . . S113 S 0.38029(11) 0.76156(11) 0.21604(10) 0.0484(4) Uani 1 1 d . . . C114 C 0.3555(4) 0.7280(4) 0.3104(4) 0.0473(16) Uani 1 1 d . . . H208 H 0.2929 0.7335 0.3371 0.057 Uiso 1 1 calc R . . C115 C 0.4387(4) 0.6922(4) 0.3419(3) 0.0366(13) Uani 1 1 d . . . N121 N 0.5479(3) 0.6218(3) 0.4276(3) 0.0347(10) Uani 1 1 d . . . C122 C 0.4549(4) 0.6541(4) 0.4188(4) 0.0390(13) Uani 1 1 d . . . C123 C 0.3853(5) 0.6518(4) 0.4785(4) 0.0460(15) Uani 1 1 d . . . H205 H 0.3208 0.6750 0.4713 0.055 Uiso 1 1 calc R . . C124 C 0.4103(5) 0.6158(4) 0.5476(4) 0.0525(17) Uani 1 1 d . . . H204 H 0.3632 0.6141 0.5893 0.063 Uiso 1 1 calc R . . C125 C 0.5043(5) 0.5814(4) 0.5578(4) 0.0488(16) Uani 1 1 d . . . H203 H 0.5230 0.5560 0.6059 0.059 Uiso 1 1 calc R . . C126 C 0.5700(5) 0.5857(4) 0.4949(3) 0.0421(14) Uani 1 1 d . . . H202 H 0.6341 0.5614 0.5008 0.051 Uiso 1 1 calc R . . O200 O 0.5041(3) 0.8418(2) 0.4175(2) 0.0329(8) Uani 1 1 d . . . C201 C 0.4050(4) 0.8640(4) 0.4432(3) 0.0372(13) Uani 1 1 d . . . H11A H 0.3553 0.8391 0.4245 0.045 Uiso 1 1 calc R . . H11B H 0.3940 0.9212 0.4253 0.045 Uiso 1 1 calc R . . C202 C 0.3958(4) 0.8374(4) 0.5263(3) 0.0380(13) Uani 1 1 d . . . H12A H 0.3248 0.8366 0.5459 0.046 Uiso 1 1 calc R . . H12B H 0.4249 0.7839 0.5434 0.046 Uiso 1 1 calc R . . O203 O 0.4452(3) 0.8879(2) 0.5532(2) 0.0377(9) Uani 1 1 d . . . C204 C 0.4311(5) 0.8700(4) 0.6320(3) 0.0422(14) Uani 1 1 d . . . H12C H 0.4657 0.8196 0.6542 0.051 Uiso 1 1 calc R . . H12D H 0.3595 0.8649 0.6492 0.051 Uiso 1 1 calc R . . C205 C 0.4705(5) 0.9322(4) 0.6567(4) 0.0453(15) Uani 1 1 d . . . H12E H 0.4441 0.9832 0.6275 0.054 Uiso 1 1 calc R . . H12F H 0.4450 0.9254 0.7092 0.054 Uiso 1 1 calc R . . O206 O 0.5762(3) 0.9339(3) 0.6498(2) 0.0432(10) Uani 1 1 d . . . C207 C 0.6182(5) 0.8864(4) 0.7149(3) 0.0440(14) Uani 1 1 d . . . H12G H 0.6022 0.8314 0.7239 0.053 Uiso 1 1 calc R . . H12H H 0.5901 0.9034 0.7585 0.053 Uiso 1 1 calc R . . C208 C 0.7290(5) 0.8941(4) 0.7034(4) 0.0472(16) Uani 1 1 d . . . H12I H 0.7448 0.9498 0.6856 0.057 Uiso 1 1 calc R . . H12J H 0.7575 0.8708 0.7509 0.057 Uiso 1 1 calc R . . O209 O 0.7712(3) 0.8555(3) 0.6503(2) 0.0427(10) Uani 1 1 d . . . C210 C 0.8742(4) 0.8695(4) 0.6291(4) 0.0467(16) Uani 1 1 d . . . H12K H 0.9056 0.8253 0.6123 0.056 Uiso 1 1 calc R . . H12L H 0.9052 0.8705 0.6733 0.056 Uiso 1 1 calc R . . C211 C 0.8968(4) 0.9438(4) 0.5689(4) 0.0418(14) Uani 1 1 d . . . H12M H 0.8694 0.9886 0.5863 0.050 Uiso 1 1 calc R . . H12N H 0.9696 0.9483 0.5585 0.050 Uiso 1 1 calc R . . O212 O 0.8565(3) 0.9468(2) 0.5024(2) 0.0381(9) Uani 1 1 d . . . C213 C 0.7586(4) 0.9806(3) 0.4962(3) 0.0349(12) Uani 1 1 d . . . H13A H 0.7590 1.0249 0.4506 0.042 Uiso 1 1 calc R . . H13B H 0.7380 1.0013 0.5390 0.042 Uiso 1 1 calc R . . C214 C 0.6849(4) 0.9243(4) 0.4940(3) 0.0339(12) Uani 1 1 d . . . H13C H 0.6902 0.8769 0.5361 0.041 Uiso 1 1 calc R . . H13D H 0.6172 0.9478 0.4991 0.041 Uiso 1 1 calc R . . O215 O 0.7008(3) 0.9030(2) 0.4246(2) 0.0327(8) Uani 1 1 d . . . O300 O 0.8602(3) 0.5830(2) 0.1162(2) 0.0402(9) Uani 1 1 d . . . C301 C 0.9175(5) 0.5195(4) 0.0980(4) 0.0441(15) Uani 1 1 d . . . H23C H 0.9345 0.4798 0.1438 0.053 Uiso 1 1 calc R . . H23D H 0.9799 0.5385 0.0675 0.053 Uiso 1 1 calc R . . C302 C 0.8574(6) 0.4847(4) 0.0562(4) 0.0492(16) Uani 1 1 d . . . H23A H 0.8899 0.4352 0.0509 0.059 Uiso 1 1 calc R . . H23B H 0.7908 0.4733 0.0835 0.059 Uiso 1 1 calc R . . O303 O 0.8479(4) 0.5375(3) -0.0149(2) 0.0475(11) Uani 1 1 d . . . C304 C 0.7765(6) 0.5122(5) -0.0508(4) 0.063(2) Uani 1 1 d . . . H22I H 0.7104 0.5128 -0.0225 0.076 Uiso 1 1 calc R . . H22J H 0.7938 0.4580 -0.0517 0.076 Uiso 1 1 calc R . . C305 C 0.7720(6) 0.5631(5) -0.1282(4) 0.0574(18) Uani 1 1 d . A . H22G H 0.7130 0.5514 -0.1483 0.069 Uiso 1 1 calc R . . H22H H 0.7659 0.6184 -0.1285 0.069 Uiso 1 1 calc R . . O306 O 0.8576(4) 0.5507(4) -0.1725(3) 0.0775(18) Uani 1 1 d . . . C307 C 0.8615(13) 0.5659(10) -0.2482(8) 0.051(4) Uani 0.45 1 d P A 1 H22U H 0.7946 0.5664 -0.2640 0.061 Uiso 0.45 1 calc PR A 1 H22V H 0.9053 0.5272 -0.2661 0.061 Uiso 0.45 1 calc PR A 1 C308 C 0.8498(14) 0.6195(11) -0.2424(7) 0.060(4) Uani 0.55 1 d P A 2 H22T H 0.7914 0.6147 -0.2670 0.072 Uiso 0.55 1 calc PR A 2 H22S H 0.8421 0.6692 -0.2292 0.072 Uiso 0.55 1 calc PR A 2 C309 C 0.9401(13) 0.6183(9) -0.2916(7) 0.051(4) Uani 0.55 1 d P A 2 H22X H 0.9518 0.5662 -0.2994 0.061 Uiso 0.55 1 calc PR A 2 H22W H 0.9334 0.6569 -0.3402 0.061 Uiso 0.55 1 calc PR A 2 C310 C 0.9059(14) 0.6493(12) -0.2769(10) 0.048(4) Uani 0.45 1 d P A 1 H22Z H 0.9002 0.6723 -0.3304 0.057 Uiso 0.45 1 calc PR A 1 H22Y H 0.8711 0.6846 -0.2496 0.057 Uiso 0.45 1 calc PR A 1 O311 O 1.0169(4) 0.6352(3) -0.2615(3) 0.0620(13) Uani 1 1 d . . . C312 C 1.0442(6) 0.7112(4) -0.2648(4) 0.0538(18) Uani 1 1 d . A . H22E H 0.9995 0.7503 -0.2951 0.065 Uiso 1 1 calc R . . H22F H 1.1127 0.7196 -0.2893 0.065 Uiso 1 1 calc R . . C313 C 1.0387(6) 0.7226(4) -0.1889(4) 0.0545(18) Uani 1 1 d . . . H22C H 1.0689 0.6764 -0.1547 0.065 Uiso 1 1 calc R A . H22D H 1.0765 0.7685 -0.1914 0.065 Uiso 1 1 calc R . . O314 O 0.9376(4) 0.7340(3) -0.1615(2) 0.0539(12) Uani 1 1 d . A . C315 C 0.9317(6) 0.7301(4) -0.0859(3) 0.0513(17) Uani 1 1 d . . . H22A H 0.9762 0.7679 -0.0787 0.062 Uiso 1 1 calc R A . H22B H 0.9522 0.6773 -0.0566 0.062 Uiso 1 1 calc R . . C316 C 0.8264(6) 0.7491(4) -0.0610(3) 0.0514(17) Uani 1 1 d . A . H21A H 0.8062 0.8030 -0.0878 0.062 Uiso 1 1 calc R . . H21B H 0.7808 0.7127 -0.0693 0.062 Uiso 1 1 calc R . . O317 O 0.8262(3) 0.7403(3) 0.0165(2) 0.0437(10) Uani 1 1 d . . . Cl1 Cl 0.13090(9) 0.75706(8) 0.53539(7) 0.0357(3) Uani 1 1 d D . . O1A O 0.1936(3) 0.7050(3) 0.5853(2) 0.0494(11) Uani 1 1 d D . . O1B O 0.1148(4) 0.8276(3) 0.5538(3) 0.0573(12) Uani 1 1 d D . . O1C O 0.0375(3) 0.7225(3) 0.5408(3) 0.0599(13) Uani 1 1 d D . . O1D O 0.1804(3) 0.7706(3) 0.4617(2) 0.0483(11) Uani 1 1 d D . . Cl2 Cl 0.20714(9) 0.93774(9) 0.22318(7) 0.0385(3) Uani 1 1 d . . . O2A O 0.2198(3) 0.9209(3) 0.3002(2) 0.0477(11) Uani 1 1 d . . . O2B O 0.2925(3) 0.9775(3) 0.1798(2) 0.0613(15) Uani 1 1 d . . . O2C O 0.1194(3) 0.9853(3) 0.2062(3) 0.0556(13) Uani 1 1 d . . . O2D O 0.1991(3) 0.8659(3) 0.2074(3) 0.0557(12) Uani 1 1 d . . . Cl3 Cl 0.58842(17) 0.14764(11) 0.07984(11) 0.0664(5) Uani 1 1 d . . . O3A O 0.5004(5) 0.1081(4) 0.0821(4) 0.0819(18) Uani 1 1 d . B . O3B O 0.6018(9) 0.2209(6) 0.0221(6) 0.079(3) Uani 0.65 1 d PU B 1 O3C O 0.5952(7) 0.1633(6) 0.1512(5) 0.069(2) Uani 0.65 1 d PU B 1 O3D O 0.6787(6) 0.0994(5) 0.0722(5) 0.0559(19) Uani 0.65 1 d PU B 1 O3E O 0.6218(11) 0.1519(10) -0.0010(11) 0.079(5) Uani 0.35 1 d PU B 2 O3F O 0.5384(17) 0.2199(11) 0.0736(16) 0.095(6) Uani 0.35 1 d PU B 2 O3G O 0.623(2) 0.1060(13) 0.1313(15) 0.128(10) Uani 0.35 1 d PU B 2 Cl4A Cl 0.2397(7) 0.5299(5) 0.3714(6) 0.066(2) Uani 0.50 1 d PDU C 1 O4A O 0.2132(11) 0.4527(6) 0.3991(7) 0.068(3) Uani 0.50 1 d PDU C 1 O4B O 0.3413(10) 0.5358(10) 0.3426(13) 0.118(8) Uani 0.50 1 d PDU C 1 O4C O 0.1896(10) 0.5891(7) 0.3257(8) 0.076(4) Uani 0.50 1 d PDU C 1 O4D O 0.2475(8) 0.5500(6) 0.4406(6) 0.064(3) Uani 0.50 1 d PDU C 1 Cl4B Cl 0.2222(7) 0.5226(6) 0.3626(7) 0.076(3) Uani 0.50 1 d PDU D 2 O4E O 0.1474(12) 0.4684(8) 0.3999(7) 0.079(4) Uani 0.50 1 d PDU D 2 O4F O 0.3143(11) 0.4898(11) 0.3533(10) 0.098(6) Uani 0.50 1 d PDU D 2 O4G O 0.1924(12) 0.5920(8) 0.3730(11) 0.099(5) Uani 0.50 1 d PDU D 2 O4H O 0.2117(9) 0.5354(8) 0.2804(5) 0.080(4) Uani 0.50 1 d PDU D 2 N1 N 0.5458(9) 0.4199(6) -0.0850(6) 0.112(3) Uani 1 1 d . . . C2 C 0.5280(9) 0.4033(6) -0.0199(7) 0.089(3) Uani 1 1 d . . . C3 C 0.5129(12) 0.3771(8) 0.0630(7) 0.125(5) Uani 1 1 d . . . H30A H 0.4767 0.3288 0.0795 0.188 Uiso 1 1 calc R . . H30B H 0.4747 0.4174 0.0811 0.188 Uiso 1 1 calc R . . H30C H 0.5775 0.3678 0.0826 0.188 Uiso 1 1 calc R . . N4 N 0.1557(14) 0.6975(8) -0.0085(11) 0.099(7) Uani 0.50 1 d P . . C5 C 0.1894(12) 0.6942(8) 0.0448(10) 0.059(4) Uani 0.50 1 d P . . C6 C 0.2388(8) 0.6865(9) 0.1100(7) 0.045(3) Uani 0.50 1 d P . . H40A H 0.2461 0.6313 0.1373 0.068 Uiso 0.50 1 calc PR . . H40B H 0.1993 0.7144 0.1418 0.068 Uiso 0.50 1 calc PR . . H40C H 0.3045 0.7087 0.0951 0.068 Uiso 0.50 1 calc PR . . N7 N 0.4350(7) 0.3348(5) 0.2371(5) 0.094(3) Uani 1 1 d . . . C8 C 0.3971(6) 0.3187(5) 0.2966(5) 0.065(2) Uani 1 1 d . . . C9 C 0.3444(6) 0.2977(5) 0.3700(4) 0.0604(19) Uani 1 1 d . . . H50A H 0.3130 0.3445 0.3808 0.091 Uiso 1 1 calc R . . H50B H 0.3912 0.2735 0.4064 0.091 Uiso 1 1 calc R . . H50C H 0.2935 0.2609 0.3726 0.091 Uiso 1 1 calc R . . O1 O 0.7232(11) 0.2740(8) 0.1511(9) 0.098(5) Uani 0.50 1 d PU . . 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 0.0267(4) 0.0369(5) 0.0245(4) -0.0083(3) -0.0078(3) 0.0050(3) Cu2 0.0230(4) 0.0366(5) 0.0339(4) -0.0123(3) -0.0061(3) 0.0066(3) N11 0.038(3) 0.035(3) 0.028(2) -0.0074(19) -0.0022(19) -0.001(2) C12 0.043(3) 0.031(3) 0.033(3) -0.009(2) 0.000(2) -0.003(3) C13 0.061(4) 0.036(3) 0.032(3) -0.009(2) 0.003(3) -0.004(3) C14 0.060(4) 0.044(4) 0.041(3) -0.014(3) 0.014(3) -0.001(3) C15 0.044(4) 0.046(4) 0.052(4) -0.016(3) 0.006(3) -0.004(3) C16 0.036(3) 0.043(3) 0.042(3) -0.013(3) -0.004(3) -0.002(3) N21 0.037(3) 0.032(2) 0.028(2) -0.0069(19) -0.0117(19) 0.005(2) C22 0.039(3) 0.035(3) 0.032(3) -0.011(2) -0.015(2) 0.010(2) S23 0.0511(9) 0.0548(10) 0.0348(7) -0.0130(7) -0.0232(7) 0.0220(7) C24 0.062(4) 0.045(4) 0.030(3) -0.011(3) -0.016(3) 0.013(3) C25 0.050(3) 0.032(3) 0.025(2) -0.007(2) -0.006(2) 0.004(3) N31 0.025(2) 0.032(2) 0.031(2) -0.0100(19) -0.0102(18) 0.0039(18) C32 0.025(3) 0.030(3) 0.031(3) -0.013(2) -0.010(2) 0.003(2) C33 0.024(3) 0.032(3) 0.038(3) -0.017(2) -0.009(2) 0.004(2) C34 0.029(3) 0.038(3) 0.044(3) -0.018(3) -0.013(2) 0.008(2) C35 0.031(3) 0.041(3) 0.043(3) -0.014(3) -0.020(2) 0.013(2) C36 0.026(3) 0.030(3) 0.036(3) -0.009(2) -0.013(2) 0.005(2) N41 0.018(2) 0.034(2) 0.026(2) -0.0058(18) -0.0021(16) 0.0019(18) C42 0.016(2) 0.037(3) 0.026(2) -0.007(2) -0.0002(19) 0.002(2) C43 0.025(3) 0.035(3) 0.029(2) -0.009(2) -0.003(2) 0.000(2) C44 0.025(3) 0.045(3) 0.030(3) -0.010(2) -0.007(2) -0.001(2) C45 0.029(3) 0.040(3) 0.034(3) -0.007(2) -0.009(2) 0.005(2) C46 0.025(3) 0.035(3) 0.029(2) -0.005(2) -0.006(2) 0.003(2) N51 0.024(2) 0.033(2) 0.030(2) -0.0068(18) -0.0011(18) 0.0051(19) C52 0.024(3) 0.043(3) 0.029(3) -0.005(2) -0.005(2) 0.010(2) S53 0.0465(9) 0.0548(10) 0.0460(8) -0.0175(7) -0.0224(7) 0.0287(7) C54 0.064(4) 0.050(4) 0.038(3) -0.011(3) -0.006(3) 0.026(3) C55 0.043(3) 0.036(3) 0.031(3) -0.008(2) -0.001(2) 0.008(3) N61 0.032(2) 0.041(3) 0.031(2) -0.007(2) -0.0028(19) 0.000(2) C62 0.050(4) 0.032(3) 0.031(3) -0.005(2) -0.001(3) 0.005(3) C63 0.075(5) 0.037(3) 0.034(3) -0.006(3) -0.002(3) 0.011(3) C64 0.101(6) 0.036(4) 0.043(4) -0.016(3) -0.011(4) -0.002(4) C65 0.073(5) 0.048(4) 0.050(4) -0.017(3) -0.010(4) -0.012(4) C66 0.056(4) 0.046(4) 0.046(3) -0.019(3) -0.008(3) -0.010(3) N71 0.022(2) 0.039(3) 0.026(2) -0.0081(19) -0.0013(17) -0.0009(19) C72 0.023(3) 0.042(3) 0.028(2) -0.010(2) 0.000(2) -0.006(2) C73 0.032(3) 0.047(4) 0.034(3) -0.015(3) -0.002(2) -0.008(3) C74 0.040(3) 0.043(3) 0.044(3) -0.022(3) 0.005(3) -0.011(3) C75 0.038(3) 0.037(3) 0.039(3) -0.008(3) 0.004(3) 0.003(3) C76 0.028(3) 0.045(3) 0.031(3) -0.008(2) -0.001(2) 0.000(3) N81 0.024(2) 0.038(3) 0.027(2) -0.0068(19) -0.0045(18) 0.0007(19) C82 0.019(2) 0.036(3) 0.029(2) -0.005(2) -0.002(2) 0.001(2) S83 0.0222(6) 0.0447(8) 0.0337(6) -0.0090(6) -0.0095(5) 0.0043(5) C84 0.023(3) 0.047(3) 0.034(3) -0.012(2) -0.005(2) -0.003(2) C85 0.023(3) 0.041(3) 0.026(2) -0.013(2) 0.002(2) -0.006(2) N91 0.027(2) 0.035(2) 0.027(2) -0.0080(19) -0.0042(18) 0.0036(19) C92 0.031(3) 0.036(3) 0.026(2) -0.009(2) -0.002(2) 0.000(2) C93 0.034(3) 0.038(3) 0.037(3) -0.014(2) 0.000(2) -0.002(3) C94 0.038(3) 0.041(3) 0.045(3) -0.016(3) -0.006(3) 0.010(3) C95 0.025(3) 0.042(3) 0.041(3) -0.008(3) -0.006(2) 0.005(2) C96 0.022(3) 0.037(3) 0.028(2) -0.002(2) 0.000(2) -0.001(2) N101 0.029(2) 0.034(2) 0.033(2) -0.0140(19) -0.011(2) 0.0062(19) C102 0.035(3) 0.034(3) 0.036(3) -0.016(2) -0.011(2) 0.005(2) C103 0.046(4) 0.038(3) 0.033(3) -0.014(2) -0.008(3) 0.006(3) C104 0.057(4) 0.054(4) 0.032(3) -0.016(3) -0.016(3) 0.013(3) C105 0.045(4) 0.050(4) 0.043(3) -0.019(3) -0.021(3) 0.011(3) C106 0.031(3) 0.039(3) 0.042(3) -0.015(3) -0.013(2) 0.008(2) N111 0.020(2) 0.042(3) 0.042(3) -0.019(2) -0.005(2) 0.0047(19) C112 0.029(3) 0.040(3) 0.048(3) -0.019(3) -0.018(3) 0.009(2) S113 0.0295(7) 0.0618(11) 0.0635(10) -0.0300(8) -0.0221(7) 0.0148(7) C114 0.021(3) 0.059(4) 0.069(4) -0.030(4) -0.012(3) 0.010(3) C115 0.024(3) 0.041(3) 0.051(3) -0.022(3) -0.007(3) 0.000(2) N121 0.025(2) 0.038(3) 0.042(3) -0.015(2) 0.001(2) -0.002(2) C122 0.027(3) 0.038(3) 0.057(4) -0.022(3) 0.001(3) 0.000(2) C123 0.031(3) 0.039(3) 0.068(4) -0.021(3) 0.011(3) -0.003(3) C124 0.050(4) 0.044(4) 0.057(4) -0.014(3) 0.020(3) -0.001(3) C125 0.057(4) 0.042(4) 0.041(3) -0.008(3) 0.010(3) -0.003(3) C126 0.042(3) 0.041(3) 0.043(3) -0.013(3) 0.001(3) 0.001(3) O200 0.0211(18) 0.042(2) 0.0363(19) -0.0136(17) -0.0030(15) 0.0046(16) C201 0.022(3) 0.048(4) 0.044(3) -0.020(3) -0.004(2) 0.006(2) C202 0.029(3) 0.040(3) 0.046(3) -0.015(3) 0.001(2) 0.001(2) O203 0.030(2) 0.048(2) 0.038(2) -0.0172(18) 0.0014(17) -0.0057(18) C204 0.033(3) 0.053(4) 0.040(3) -0.013(3) 0.000(3) 0.001(3) C205 0.037(3) 0.058(4) 0.043(3) -0.022(3) -0.002(3) 0.008(3) O206 0.040(2) 0.050(3) 0.040(2) -0.0113(19) -0.0088(18) 0.0006(19) C207 0.048(4) 0.047(4) 0.036(3) -0.010(3) -0.007(3) 0.001(3) C208 0.050(4) 0.055(4) 0.040(3) -0.017(3) -0.019(3) 0.011(3) O209 0.038(2) 0.051(3) 0.040(2) -0.0136(19) -0.0105(18) 0.0030(19) C210 0.035(3) 0.060(4) 0.053(4) -0.025(3) -0.022(3) 0.012(3) C211 0.032(3) 0.050(4) 0.051(3) -0.024(3) -0.017(3) 0.008(3) O212 0.0269(19) 0.048(2) 0.044(2) -0.0201(19) -0.0096(17) 0.0047(17) C213 0.030(3) 0.040(3) 0.038(3) -0.016(2) -0.009(2) 0.006(2) C214 0.028(3) 0.045(3) 0.033(3) -0.017(2) -0.007(2) 0.004(2) O215 0.034(2) 0.034(2) 0.0314(18) -0.0108(16) -0.0095(16) 0.0028(16) O300 0.040(2) 0.044(2) 0.042(2) -0.0221(19) -0.0072(18) 0.0042(19) C301 0.056(4) 0.039(3) 0.041(3) -0.019(3) -0.007(3) 0.010(3) C302 0.073(5) 0.038(3) 0.040(3) -0.016(3) -0.009(3) 0.004(3) O303 0.065(3) 0.044(2) 0.037(2) -0.0151(19) -0.009(2) 0.000(2) C304 0.067(5) 0.082(6) 0.044(4) -0.019(4) -0.010(3) -0.011(4) C305 0.056(4) 0.070(5) 0.049(4) -0.024(4) -0.009(3) 0.013(4) O306 0.060(3) 0.131(5) 0.033(2) -0.014(3) -0.010(2) 0.015(3) C307 0.065(10) 0.048(9) 0.046(8) -0.023(8) -0.020(7) 0.023(8) C308 0.080(12) 0.072(11) 0.027(6) -0.015(7) -0.017(7) 0.030(9) C309 0.074(11) 0.050(9) 0.026(6) -0.007(6) -0.009(7) 0.014(8) C310 0.044(10) 0.061(12) 0.031(8) -0.009(8) 0.004(8) 0.015(9) O311 0.084(4) 0.059(3) 0.041(2) -0.011(2) -0.008(3) -0.003(3) C312 0.069(5) 0.049(4) 0.039(3) -0.012(3) 0.000(3) 0.012(4) C313 0.064(5) 0.047(4) 0.047(4) -0.011(3) 0.003(3) 0.007(3) O314 0.068(3) 0.057(3) 0.034(2) -0.014(2) -0.001(2) 0.013(2) C315 0.073(5) 0.044(4) 0.033(3) -0.007(3) -0.006(3) 0.009(3) C316 0.067(4) 0.057(4) 0.033(3) -0.018(3) -0.010(3) 0.012(3) O317 0.051(3) 0.051(3) 0.029(2) -0.0126(18) -0.0039(19) 0.002(2) Cl1 0.0279(6) 0.0463(8) 0.0318(6) -0.0086(6) -0.0081(5) 0.0021(6) O1A 0.048(3) 0.061(3) 0.034(2) -0.008(2) -0.0062(19) 0.013(2) O1B 0.046(3) 0.051(3) 0.072(3) -0.021(2) 0.004(2) 0.007(2) O1C 0.038(3) 0.097(4) 0.047(3) -0.021(3) -0.004(2) -0.017(3) O1D 0.029(2) 0.078(3) 0.033(2) -0.010(2) -0.0054(17) 0.007(2) Cl2 0.0225(6) 0.0577(9) 0.0314(6) -0.0059(6) -0.0060(5) 0.0018(6) O2A 0.041(2) 0.066(3) 0.033(2) -0.005(2) -0.0095(18) -0.006(2) O2B 0.024(2) 0.105(4) 0.038(2) 0.007(2) -0.0038(18) -0.008(2) O2C 0.029(2) 0.063(3) 0.060(3) 0.004(2) -0.006(2) 0.010(2) O2D 0.037(2) 0.079(4) 0.060(3) -0.033(3) -0.015(2) 0.011(2) Cl3 0.0839(14) 0.0497(10) 0.0614(11) -0.0108(9) -0.0161(10) 0.0173(10) O3A 0.078(4) 0.094(5) 0.074(4) -0.029(3) -0.017(3) 0.032(4) O3B 0.089(7) 0.065(6) 0.076(6) 0.006(5) -0.051(6) -0.002(5) O3C 0.064(5) 0.088(7) 0.063(5) -0.038(5) -0.012(4) 0.011(5) O3D 0.049(4) 0.062(5) 0.051(4) -0.010(4) -0.006(3) 0.010(4) O3E 0.042(8) 0.068(11) 0.112(14) 0.002(10) -0.015(9) 0.001(7) O3F 0.090(14) 0.065(12) 0.14(2) -0.034(12) -0.047(14) 0.015(10) O3G 0.20(2) 0.077(13) 0.117(17) -0.006(13) -0.128(19) 0.058(15) Cl4A 0.055(4) 0.031(3) 0.124(5) -0.020(3) -0.063(3) -0.001(2) O4A 0.093(10) 0.043(7) 0.064(7) -0.010(5) -0.012(8) 0.013(7) O4B 0.088(12) 0.062(10) 0.21(2) -0.044(13) -0.051(12) 0.035(9) O4C 0.081(8) 0.047(7) 0.109(11) -0.023(7) -0.066(8) 0.033(6) O4D 0.074(7) 0.059(6) 0.073(7) -0.030(6) -0.033(6) 0.003(5) Cl4B 0.052(4) 0.049(4) 0.151(6) -0.047(3) -0.069(4) 0.014(3) O4E 0.114(12) 0.075(9) 0.059(7) -0.032(7) -0.012(8) -0.013(9) O4F 0.086(11) 0.092(12) 0.121(13) -0.039(11) -0.049(10) 0.062(10) O4G 0.102(11) 0.078(10) 0.138(15) -0.059(11) -0.031(11) 0.015(9) O4H 0.069(7) 0.107(10) 0.045(6) 0.008(6) -0.018(5) 0.024(7) N1 0.136(9) 0.094(7) 0.099(7) 0.001(6) -0.053(7) -0.014(6) C2 0.105(8) 0.080(7) 0.088(7) -0.029(6) -0.031(6) 0.006(6) C3 0.177(14) 0.133(11) 0.077(7) -0.052(8) -0.018(8) 0.016(10) N4 0.142(14) 0.047(8) 0.150(15) -0.066(9) -0.120(13) 0.053(9) C5 0.072(9) 0.031(7) 0.091(11) -0.037(7) -0.042(9) 0.021(7) C6 0.019(5) 0.076(9) 0.057(7) -0.042(7) -0.003(5) -0.012(6) N7 0.101(7) 0.084(6) 0.079(6) -0.004(4) 0.021(5) -0.022(5) C8 0.060(5) 0.050(4) 0.081(6) -0.011(4) -0.005(4) -0.005(4) C9 0.059(5) 0.064(5) 0.057(4) -0.014(4) -0.007(4) -0.005(4) O1 0.123(11) 0.082(8) 0.134(12) -0.084(9) -0.095(10) 0.058(8) _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 N81 1.928(4) . ? Cu1 N21 1.931(4) . ? Cu1 N71 2.164(5) . ? Cu1 N11 2.184(5) . ? Cu1 N91 2.415(5) . ? Cu1 N31 2.472(4) . ? Cu2 N51 1.927(4) . ? Cu2 N111 1.936(4) . ? Cu2 N61 2.136(5) . ? Cu2 N121 2.192(5) . ? Cu2 N41 2.397(4) . ? N11 C16 1.333(8) . ? N11 C12 1.348(7) . ? C12 C13 1.395(8) . ? C12 C25 1.468(9) . ? C13 C14 1.381(10) . ? C14 C15 1.367(10) . ? C15 C16 1.386(9) . ? N21 C22 1.312(7) . ? N21 C25 1.376(7) . ? C22 C36 1.452(8) . ? C22 S23 1.716(5) . ? S23 C24 1.709(7) . ? C24 C25 1.361(8) . ? N31 C32 1.326(7) . ? N31 C36 1.349(6) . ? C32 C33 1.408(7) . ? C32 C42 1.496(7) . ? C33 O200 1.337(7) . ? C33 C34 1.407(7) . ? C34 C35 1.363(8) . ? C35 C36 1.397(8) . ? N41 C42 1.326(7) . ? N41 C46 1.364(6) . ? C42 C43 1.389(8) . ? C43 O215 1.343(7) . ? C43 C44 1.403(7) . ? C44 C45 1.377(8) . ? C45 C46 1.385(8) . ? C46 C52 1.458(8) . ? N51 C52 1.310(7) . ? N51 C55 1.363(7) . ? C52 S53 1.712(5) . ? S53 C54 1.702(8) . ? C54 C55 1.378(9) . ? C55 C62 1.467(9) . ? N61 C66 1.337(8) . ? N61 C62 1.363(8) . ? C62 C63 1.389(9) . ? C63 C64 1.394(11) . ? C64 C65 1.356(11) . ? C65 C66 1.381(10) . ? N71 C76 1.334(7) . ? N71 C72 1.359(7) . ? C72 C73 1.369(8) . ? C72 C85 1.454(8) . ? C73 C74 1.389(9) . ? C74 C75 1.385(9) . ? C75 C76 1.372(9) . ? N81 C82 1.299(7) . ? N81 C85 1.374(7) . ? C82 C96 1.458(8) . ? C82 S83 1.718(5) . ? S83 C84 1.720(6) . ? C84 C85 1.353(7) . ? N91 C92 1.326(7) . ? N91 C96 1.367(7) . ? C92 C93 1.396(8) . ? C92 C102 1.496(7) . ? C93 O300 1.335(7) . ? C93 C94 1.401(8) . ? C94 C95 1.373(9) . ? C95 C96 1.379(8) . ? N101 C102 1.311(8) . ? N101 C106 1.354(7) . ? C102 C103 1.410(8) . ? C103 O317 1.337(8) . ? C103 C104 1.392(9) . ? C104 C105 1.390(10) . ? C105 C106 1.387(8) . ? C106 C112 1.465(9) . ? N111 C112 1.310(7) . ? N111 C115 1.372(8) . ? C112 S113 1.708(5) . ? S113 C114 1.714(8) . ? C114 C115 1.373(8) . ? C115 C122 1.456(9) . ? N121 C126 1.313(8) . ? N121 C122 1.360(7) . ? C122 C123 1.378(9) . ? C123 C124 1.356(10) . ? C124 C125 1.388(10) . ? C125 C126 1.388(9) . ? O200 C201 1.445(6) . ? C201 C202 1.501(8) . ? C202 O203 1.409(7) . ? O203 C204 1.426(7) . ? C204 C205 1.488(9) . ? C205 O206 1.429(7) . ? O206 C207 1.437(7) . ? C207 C208 1.505(9) . ? C208 O209 1.426(8) . ? O209 C210 1.428(8) . ? C210 C211 1.505(10) . ? C211 O212 1.422(7) . ? O212 C213 1.425(6) . ? C213 C214 1.488(8) . ? C214 O215 1.463(6) . ? O300 C301 1.436(7) . ? C301 C302 1.488(10) . ? C302 O303 1.420(8) . ? O303 C304 1.422(9) . ? C304 C305 1.493(10) . ? C305 O306 1.394(9) . ? O306 C307 1.379(16) . ? O306 C308 1.537(17) . ? C307 C310 1.58(3) . ? C308 C309 1.45(2) . ? C309 O311 1.342(16) . ? C310 O311 1.559(18) . ? O311 C312 1.423(9) . ? C312 C313 1.507(10) . ? C313 O314 1.430(9) . ? O314 C315 1.409(8) . ? C315 C316 1.499(10) . ? C316 O317 1.432(7) . ? Cl1 O1B 1.406(5) . ? Cl1 O1C 1.433(5) . ? Cl1 O1A 1.436(4) . ? Cl1 O1D 1.438(4) . ? Cl2 O2D 1.424(5) . ? Cl2 O2C 1.428(4) . ? Cl2 O2A 1.434(4) . ? Cl2 O2B 1.443(5) . ? Cl3 O3G 1.171(15) . ? Cl3 O3F 1.401(19) . ? Cl3 O3A 1.425(8) . ? Cl3 O3B 1.453(9) . ? Cl3 O3D 1.467(8) . ? Cl3 O3C 1.477(8) . ? Cl3 O3E 1.53(2) . ? Cl4A O4C 1.359(11) . ? Cl4A O4A 1.390(11) . ? Cl4A O4B 1.422(13) . ? Cl4A O4D 1.479(14) . ? Cl4B O4G 1.344(12) . ? Cl4B O4F 1.358(12) . ? Cl4B O4E 1.433(13) . ? Cl4B O4H 1.533(14) . ? N1 C2 1.183(15) . ? C2 C3 1.497(16) . ? N4 C5 1.144(19) . ? C5 C6 1.448(18) . ? N7 C8 1.148(12) . ? C8 C9 1.444(12) . ? 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 N81 Cu1 N21 176.9(2) . . ? N81 Cu1 N71 77.70(18) . . ? N21 Cu1 N71 103.75(18) . . ? N81 Cu1 N11 99.51(18) . . ? N21 Cu1 N11 77.44(19) . . ? N71 Cu1 N11 110.51(17) . . ? N81 Cu1 N91 72.55(17) . . ? N21 Cu1 N91 106.46(17) . . ? N71 Cu1 N91 148.66(15) . . ? N11 Cu1 N91 84.29(16) . . ? N81 Cu1 N31 110.84(17) . . ? N21 Cu1 N31 72.14(17) . . ? N71 Cu1 N31 82.48(15) . . ? N11 Cu1 N31 149.08(16) . . ? N91 Cu1 N31 98.93(15) . . ? N51 Cu2 N111 177.4(2) . . ? N51 Cu2 N61 78.27(19) . . ? N111 Cu2 N61 101.21(19) . . ? N51 Cu2 N121 99.87(18) . . ? N111 Cu2 N121 77.94(19) . . ? N61 Cu2 N121 111.04(18) . . ? N51 Cu2 N41 72.84(17) . . ? N111 Cu2 N41 108.10(17) . . ? N61 Cu2 N41 149.38(16) . . ? N121 Cu2 N41 84.12(16) . . ? C16 N11 C12 118.4(5) . . ? C16 N11 Cu1 127.8(4) . . ? C12 N11 Cu1 113.8(4) . . ? N11 C12 C13 121.9(6) . . ? N11 C12 C25 113.3(5) . . ? C13 C12 C25 124.9(6) . . ? C14 C13 C12 118.2(6) . . ? C15 C14 C13 120.4(6) . . ? C14 C15 C16 118.0(6) . . ? N11 C16 C15 123.2(6) . . ? C22 N21 C25 113.7(5) . . ? C22 N21 Cu1 125.8(4) . . ? C25 N21 Cu1 120.5(4) . . ? N21 C22 C36 119.2(5) . . ? N21 C22 S23 112.1(4) . . ? C36 C22 S23 128.7(4) . . ? C24 S23 C22 90.5(3) . . ? C25 C24 S23 110.8(5) . . ? C24 C25 N21 112.8(6) . . ? C24 C25 C12 132.2(5) . . ? N21 C25 C12 115.0(5) . . ? C32 N31 C36 119.0(4) . . ? C32 N31 Cu1 130.8(3) . . ? C36 N31 Cu1 108.2(3) . . ? N31 C32 C33 122.8(5) . . ? N31 C32 C42 115.5(4) . . ? C33 C32 C42 121.7(5) . . ? O200 C33 C34 126.5(5) . . ? O200 C33 C32 116.0(4) . . ? C34 C33 C32 117.5(5) . . ? C35 C34 C33 119.3(5) . . ? C34 C35 C36 119.6(5) . . ? N31 C36 C35 121.7(5) . . ? N31 C36 C22 113.0(5) . . ? C35 C36 C22 125.3(5) . . ? C42 N41 C46 117.8(5) . . ? C42 N41 Cu2 130.7(3) . . ? C46 N41 Cu2 108.5(3) . . ? N41 C42 C43 123.8(5) . . ? N41 C42 C32 115.1(4) . . ? C43 C42 C32 121.1(5) . . ? O215 C43 C42 117.0(4) . . ? O215 C43 C44 124.9(5) . . ? C42 C43 C44 117.9(5) . . ? C45 C44 C43 118.9(5) . . ? C44 C45 C46 119.4(5) . . ? N41 C46 C45 122.1(5) . . ? N41 C46 C52 111.8(5) . . ? C45 C46 C52 126.1(5) . . ? C52 N51 C55 114.8(5) . . ? C52 N51 Cu2 124.6(4) . . ? C55 N51 Cu2 120.4(4) . . ? N51 C52 C46 118.1(4) . . ? N51 C52 S53 111.5(4) . . ? C46 C52 S53 130.3(4) . . ? C54 S53 C52 91.1(3) . . ? C55 C54 S53 110.3(5) . . ? N51 C55 C54 112.3(6) . . ? N51 C55 C62 114.1(5) . . ? C54 C55 C62 133.6(6) . . ? C66 N61 C62 118.2(5) . . ? C66 N61 Cu2 128.3(4) . . ? C62 N61 Cu2 113.5(4) . . ? N61 C62 C63 122.6(6) . . ? N61 C62 C55 113.5(5) . . ? C63 C62 C55 123.9(6) . . ? C62 C63 C64 117.4(7) . . ? C65 C64 C63 119.9(6) . . ? C64 C65 C66 120.1(7) . . ? N61 C66 C65 121.9(7) . . ? C76 N71 C72 117.4(5) . . ? C76 N71 Cu1 128.8(4) . . ? C72 N71 Cu1 113.8(4) . . ? N71 C72 C73 122.3(5) . . ? N71 C72 C85 113.1(5) . . ? C73 C72 C85 124.6(5) . . ? C72 C73 C74 119.2(5) . . ? C75 C74 C73 118.9(6) . . ? C76 C75 C74 118.2(6) . . ? N71 C76 C75 124.0(5) . . ? C82 N81 C85 114.3(4) . . ? C82 N81 Cu1 125.4(4) . . ? C85 N81 Cu1 120.1(4) . . ? N81 C82 C96 118.0(4) . . ? N81 C82 S83 112.6(4) . . ? C96 C82 S83 129.4(4) . . ? C82 S83 C84 89.6(3) . . ? C85 C84 S83 111.3(4) . . ? C84 C85 N81 112.2(5) . . ? C84 C85 C72 132.5(5) . . ? N81 C85 C72 115.3(4) . . ? C92 N91 C96 118.2(5) . . ? C92 N91 Cu1 129.8(3) . . ? C96 N91 Cu1 107.8(4) . . ? N91 C92 C93 123.5(5) . . ? N91 C92 C102 115.5(5) . . ? C93 C92 C102 121.0(5) . . ? O300 C93 C92 116.7(5) . . ? O300 C93 C94 125.4(5) . . ? C92 C93 C94 117.8(5) . . ? C95 C94 C93 118.8(5) . . ? C94 C95 C96 120.3(5) . . ? N91 C96 C95 121.4(5) . . ? N91 C96 C82 112.1(5) . . ? C95 C96 C82 126.5(5) . . ? C102 N101 C106 118.4(5) . . ? N101 C102 C103 123.3(5) . . ? N101 C102 C92 115.4(5) . . ? C103 C102 C92 121.2(5) . . ? O317 C103 C104 126.2(5) . . ? O317 C103 C102 115.6(5) . . ? C104 C103 C102 118.1(6) . . ? C105 C104 C103 118.7(5) . . ? C106 C105 C104 118.9(6) . . ? N101 C106 C105 122.6(6) . . ? N101 C106 C112 113.1(5) . . ? C105 C106 C112 124.3(5) . . ? C112 N111 C115 113.4(5) . . ? C112 N111 Cu2 126.8(4) . . ? C115 N111 Cu2 119.7(4) . . ? N111 C112 C106 119.2(5) . . ? N111 C112 S113 113.1(5) . . ? C106 C112 S113 127.6(4) . . ? C112 S113 C114 90.2(3) . . ? C115 C114 S113 110.6(5) . . ? N111 C115 C114 112.7(6) . . ? N111 C115 C122 116.0(5) . . ? C114 C115 C122 131.3(6) . . ? C126 N121 C122 118.5(5) . . ? C126 N121 Cu2 128.8(4) . . ? C122 N121 Cu2 112.7(4) . . ? N121 C122 C123 121.7(6) . . ? N121 C122 C115 113.7(5) . . ? C123 C122 C115 124.6(6) . . ? C124 C123 C122 118.9(6) . . ? C123 C124 C125 120.4(6) . . ? C126 C125 C124 117.3(6) . . ? N121 C126 C125 123.2(6) . . ? C33 O200 C201 117.5(4) . . ? O200 C201 C202 107.2(4) . . ? O203 C202 C201 110.1(5) . . ? C202 O203 C204 112.7(5) . . ? O203 C204 C205 110.5(5) . . ? O206 C205 C204 115.0(5) . . ? C205 O206 C207 112.8(5) . . ? O206 C207 C208 108.9(5) . . ? O209 C208 C207 109.5(5) . . ? C208 O209 C210 112.6(5) . . ? O209 C210 C211 115.3(5) . . ? O212 C211 C210 112.3(5) . . ? C211 O212 C213 115.3(4) . . ? O212 C213 C214 112.9(5) . . ? O215 C214 C213 111.4(5) . . ? C43 O215 C214 119.0(4) . . ? C93 O300 C301 118.8(5) . . ? O300 C301 C302 108.3(5) . . ? O303 C302 C301 109.5(6) . . ? C302 O303 C304 110.6(5) . . ? O303 C304 C305 111.3(7) . . ? O306 C305 C304 109.9(6) . . ? C307 O306 C305 123.1(8) . . ? C307 O306 C308 39.7(8) . . ? C305 O306 C308 101.5(8) . . ? O306 C307 C310 102.2(14) . . ? C309 C308 O306 107.7(11) . . ? O311 C309 C308 109.4(13) . . ? O311 C310 C307 104.5(13) . . ? C309 O311 C312 126.0(8) . . ? C309 O311 C310 30.5(8) . . ? C312 O311 C310 102.1(9) . . ? O311 C312 C313 111.9(6) . . ? O314 C313 C312 110.2(6) . . ? C315 O314 C313 109.7(5) . . ? O314 C315 C316 108.0(6) . . ? O317 C316 C315 104.3(5) . . ? C103 O317 C316 119.4(5) . . ? O1B Cl1 O1C 109.3(3) . . ? O1B Cl1 O1A 109.6(3) . . ? O1C Cl1 O1A 109.6(3) . . ? O1B Cl1 O1D 110.2(3) . . ? O1C Cl1 O1D 110.3(3) . . ? O1A Cl1 O1D 107.8(3) . . ? O2D Cl2 O2C 109.4(3) . . ? O2D Cl2 O2A 108.0(3) . . ? O2C Cl2 O2A 110.7(3) . . ? O2D Cl2 O2B 110.0(3) . . ? O2C Cl2 O2B 109.7(3) . . ? O2A Cl2 O2B 108.9(3) . . ? O3G Cl3 O3F 128.3(18) . . ? O3G Cl3 O3A 100.4(15) . . ? O3F Cl3 O3A 94.0(10) . . ? O3G Cl3 O3B 143.1(15) . . ? O3F Cl3 O3B 50.5(11) . . ? O3A Cl3 O3B 116.4(5) . . ? O3G Cl3 O3D 58.0(16) . . ? O3F Cl3 O3D 151.9(11) . . ? O3A Cl3 O3D 112.4(4) . . ? O3B Cl3 O3D 106.3(6) . . ? O3G Cl3 O3C 53.3(13) . . ? O3F Cl3 O3C 75.2(11) . . ? O3A Cl3 O3C 111.1(5) . . ? O3B Cl3 O3C 107.2(6) . . ? O3D Cl3 O3C 102.3(5) . . ? O3G Cl3 O3E 125.6(17) . . ? O3F Cl3 O3E 102.2(13) . . ? O3A Cl3 O3E 93.8(7) . . ? O3B Cl3 O3E 57.3(8) . . ? O3D Cl3 O3E 68.0(7) . . ? O3C Cl3 O3E 155.0(8) . . ? O4C Cl4A O4A 127.0(10) . . ? O4C Cl4A O4B 106.5(12) . . ? O4A Cl4A O4B 111.6(11) . . ? O4C Cl4A O4D 108.5(11) . . ? O4A Cl4A O4D 101.1(9) . . ? O4B Cl4A O4D 98.2(11) . . ? O4G Cl4B O4F 131.2(13) . . ? O4G Cl4B O4E 107.7(12) . . ? O4F Cl4B O4E 114.6(12) . . ? O4G Cl4B O4H 103.1(11) . . ? O4F Cl4B O4H 89.7(10) . . ? O4E Cl4B O4H 103.6(9) . . ? N1 C2 C3 174.9(13) . . ? N4 C5 C6 175.3(17) . . ? N7 C8 C9 176.9(10) . . ? _diffrn_measured_fraction_theta_max 0.872 _diffrn_reflns_theta_full 70.35 _diffrn_measured_fraction_theta_full 0.872 _refine_diff_density_max 2.743 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.144 #======================================================== data_craig7m _database_code_depnum_ccdc_archive 'CCDC 270152' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H77 Cl6 Cu2 N15 Na2 O36 S4' _chemical_formula_weight 2314.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5033(3) _cell_length_b 17.4605(4) _cell_length_c 21.8269(5) _cell_angle_alpha 93.053(2) _cell_angle_beta 94.952(2) _cell_angle_gamma 106.6530(10) _cell_volume 4895.55(19) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 3.723 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.266221 _exptl_absorpt_correction_T_max 0.607036 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The complex cation is well resolved and features two Cu(II) coordination domains incorporated into a metallo-helical array. Na+ cations occupy both of the crown ether host cavities spanning the central bipy rings, each being stabilised by four Na-O interactions (with the crown ethers) and coordinating acetonitrile and perchlorate ligands. Although the atoms comprising the complex molecule are well ordered, regions of disorder were identified in the peripherally 'guest-bound' perchlorate and acetonitrile ligands. Thus, ClO4(6) and the acetonitrile ligand coordinating to Na(1), are disordered over two positions, with site occupancies of 0.6:0.4 (for the MeCN positions) and 0.5:0.5 [for the ClO4(6a) and ClO4(6b) positions]. The geometries of both ClO4(6a)/(6b) components were restrained using similarity restraints (SADI) and the ADP's on the oxygen atoms were constrained to be equal (EADP). The geometries of each component of the disordered acetonitrile molecule were also restrained (DFIX) and only the nitroge ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source '4.8 kW rotating anode' _diffrn_radiation_monochromator 'Osmic ConFocal MaxFlux mirror optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Frames, each covering 0.3 \% in \w' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37678 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0955 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 70.02 _reflns_number_total 16519 _reflns_number_gt 9589 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.1363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16519 _refine_ls_number_parameters 1263 _refine_ls_number_restraints 148 _refine_ls_R_factor_all 0.1161 _refine_ls_R_factor_gt 0.0809 _refine_ls_wR_factor_ref 0.2290 _refine_ls_wR_factor_gt 0.2105 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.004 _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 0.36568(7) -0.03340(5) 0.17021(4) 0.0336(2) Uani 1 1 d . . . N11 N 0.4525(5) 0.0347(3) 0.1020(2) 0.0419(13) Uani 1 1 d . . . C12 C 0.5539(6) 0.0596(4) 0.0997(3) 0.0527(19) Uani 1 1 d . . . H12 H 0.5973 0.0493 0.1316 0.063 Uiso 1 1 calc R . . C13 C 0.5995(7) 0.1016(4) 0.0503(4) 0.065(2) Uani 1 1 d . . . H13 H 0.6711 0.1183 0.0490 0.078 Uiso 1 1 calc R . . C14 C 0.5321(8) 0.1164(4) 0.0044(4) 0.065(3) Uani 1 1 d . . . H14 H 0.5590 0.1449 -0.0282 0.078 Uiso 1 1 calc R . . C15 C 0.4265(7) 0.0900(4) 0.0056(3) 0.057(2) Uani 1 1 d . . . H15 H 0.3817 0.0987 -0.0263 0.068 Uiso 1 1 calc R . . C16 C 0.3879(6) 0.0498(4) 0.0561(3) 0.0481(19) Uani 1 1 d . . . N21 N 0.2554(5) -0.0142(3) 0.1167(2) 0.0384(12) Uani 1 1 d . . . C22 C 0.2781(6) 0.0206(4) 0.0633(3) 0.0452(17) Uani 1 1 d . . . C23 C 0.1845(7) 0.0191(4) 0.0281(3) 0.066(3) Uani 1 1 d . . . H23 H 0.1824 0.0410 -0.0098 0.079 Uiso 1 1 calc R . . S24 S 0.08034(16) -0.02475(11) 0.06051(8) 0.0546(5) Uani 1 1 d . . . C25 C 0.1551(5) -0.0427(4) 0.1218(3) 0.0423(15) Uani 1 1 d . . . N31 N 0.2034(4) -0.0813(3) 0.2177(2) 0.0361(12) Uani 1 1 d . . . C32 C 0.1209(5) -0.0845(3) 0.1754(3) 0.0341(13) Uani 1 1 d . . . C33 C 0.0210(5) -0.1274(4) 0.1845(3) 0.0422(15) Uani 1 1 d . . . H33 H -0.0337 -0.1297 0.1548 0.051 Uiso 1 1 calc R . . C34 C 0.0018(6) -0.1665(4) 0.2368(3) 0.0464(17) Uani 1 1 d . . . H34 H -0.0658 -0.1945 0.2432 0.056 Uiso 1 1 calc R . . C35 C 0.0844(5) -0.1639(4) 0.2803(3) 0.0430(16) Uani 1 1 d . . . C36 C 0.1850(5) -0.1182(3) 0.2678(3) 0.0345(14) Uani 1 1 d . . . N71 N 0.3417(4) -0.1604(3) 0.1417(2) 0.0353(12) Uani 1 1 d . . . C72 C 0.4164(5) -0.1901(3) 0.1679(3) 0.0363(14) Uani 1 1 d . . . C73 C 0.4177(6) -0.2672(4) 0.1529(3) 0.0450(16) Uani 1 1 d . . . H73 H 0.4699 -0.2864 0.1709 0.054 Uiso 1 1 calc R . . C74 C 0.3399(7) -0.3159(4) 0.1105(3) 0.0533(19) Uani 1 1 d . . . H74 H 0.3388 -0.3684 0.0999 0.064 Uiso 1 1 calc R . . C75 C 0.2645(7) -0.2856(4) 0.0845(3) 0.054(2) Uani 1 1 d . . . H75 H 0.2119 -0.3176 0.0559 0.064 Uiso 1 1 calc R . . C76 C 0.2669(6) -0.2087(4) 0.1006(3) 0.0441(16) Uani 1 1 d . . . H76 H 0.2152 -0.1889 0.0827 0.053 Uiso 1 1 calc R . . N81 N 0.4781(4) -0.0569(3) 0.2188(2) 0.0321(11) Uani 1 1 d . . . C82 C 0.5500(5) -0.0054(4) 0.2559(3) 0.0363(14) Uani 1 1 d . . . S83 S 0.64289(13) -0.04628(10) 0.28694(8) 0.0441(4) Uani 1 1 d . . . C84 C 0.5782(5) -0.1371(4) 0.2467(3) 0.0452(16) Uani 1 1 d . . . H84 H 0.5989 -0.1835 0.2486 0.054 Uiso 1 1 calc R . . C85 C 0.4930(5) -0.1313(4) 0.2119(3) 0.0364(14) Uani 1 1 d . . . N91 N 0.4538(4) 0.0866(3) 0.2418(2) 0.0324(11) Uani 1 1 d . . . C92 C 0.5432(5) 0.0765(3) 0.2678(3) 0.0378(14) Uani 1 1 d . . . C93 C 0.6191(5) 0.1377(4) 0.3022(3) 0.0423(15) Uani 1 1 d . . . H93 H 0.6813 0.1296 0.3178 0.051 Uiso 1 1 calc R . . C94 C 0.6012(6) 0.2112(4) 0.3130(3) 0.0430(16) Uani 1 1 d . . . H94 H 0.6500 0.2525 0.3375 0.052 Uiso 1 1 calc R . . C95 C 0.5097(5) 0.2228(3) 0.2868(3) 0.0380(15) Uani 1 1 d . . . C96 C 0.4374(5) 0.1579(3) 0.2507(3) 0.0371(15) Uani 1 1 d . . . Cu2 Cu 0.24925(7) 0.07221(5) 0.36234(4) 0.0401(2) Uani 1 1 d . . . N41 N 0.3193(4) -0.0401(3) 0.3419(2) 0.0343(11) Uani 1 1 d . . . C42 C 0.4083(5) -0.0297(4) 0.3799(3) 0.0384(14) Uani 1 1 d . . . C43 C 0.4527(5) -0.0912(4) 0.3883(3) 0.0418(15) Uani 1 1 d . . . H43 H 0.5139 -0.0819 0.4144 0.050 Uiso 1 1 calc R . . C44 C 0.4069(6) -0.1661(4) 0.3582(3) 0.0433(16) Uani 1 1 d . . . H44 H 0.4359 -0.2078 0.3637 0.052 Uiso 1 1 calc R . . C45 C 0.3163(5) -0.1771(3) 0.3197(3) 0.0379(15) Uani 1 1 d . C . C46 C 0.2770(5) -0.1111(3) 0.3130(3) 0.0312(13) Uani 1 1 d . . . N51 N 0.3871(4) 0.0982(3) 0.4056(2) 0.0373(12) Uani 1 1 d . . . C52 C 0.4475(5) 0.0511(4) 0.4103(3) 0.0389(14) Uani 1 1 d . . . S53 S 0.56240(14) 0.09584(10) 0.45499(8) 0.0463(4) Uani 1 1 d . . . C54 C 0.5250(6) 0.1810(4) 0.4676(3) 0.0466(17) Uani 1 1 d . . . H54 H 0.5652 0.2269 0.4914 0.056 Uiso 1 1 calc R . . C55 C 0.4288(5) 0.1727(4) 0.4382(3) 0.0378(14) Uani 1 1 d . . . N61 N 0.2724(4) 0.1938(3) 0.3988(2) 0.0394(12) Uani 1 1 d . . . C62 C 0.3620(5) 0.2253(4) 0.4351(3) 0.0362(14) Uani 1 1 d . . . C63 C 0.3880(5) 0.2999(4) 0.4673(3) 0.0419(15) Uani 1 1 d . . . H63 H 0.4492 0.3193 0.4937 0.050 Uiso 1 1 calc R . . C64 C 0.3188(6) 0.3446(4) 0.4587(3) 0.0459(17) Uani 1 1 d . . . H64 H 0.3353 0.3962 0.4778 0.055 Uiso 1 1 calc R . . C65 C 0.2261(6) 0.3134(4) 0.4223(3) 0.0455(16) Uani 1 1 d . . . H65 H 0.1780 0.3422 0.4177 0.055 Uiso 1 1 calc R . . C66 C 0.2063(6) 0.2375(4) 0.3925(3) 0.0473(16) Uani 1 1 d . . . H66 H 0.1444 0.2162 0.3670 0.057 Uiso 1 1 calc R . . N101 N 0.2572(4) 0.1215(3) 0.2551(2) 0.0360(12) Uani 1 1 d . . . C102 C 0.3334(6) 0.1608(3) 0.2253(3) 0.0389(15) Uani 1 1 d . . . C103 C 0.3187(7) 0.1978(4) 0.1700(3) 0.0495(18) Uani 1 1 d . . . C104 C 0.2174(7) 0.1903(4) 0.1466(3) 0.057(2) Uani 1 1 d . . . H104 H 0.2042 0.2135 0.1106 0.069 Uiso 1 1 calc R . . C105 C 0.1364(7) 0.1484(4) 0.1769(4) 0.058(2) Uani 1 1 d . . . H105 H 0.0681 0.1425 0.1615 0.070 Uiso 1 1 calc R . . C106 C 0.1581(6) 0.1147(4) 0.2315(3) 0.0499(18) Uani 1 1 d . . . N111 N 0.1095(4) 0.0451(3) 0.3212(3) 0.0479(15) Uani 1 1 d . . . C112 C 0.0783(5) 0.0676(4) 0.2675(4) 0.0466(17) Uani 1 1 d . . . S113 S -0.05182(15) 0.03309(11) 0.24792(12) 0.0692(7) Uani 1 1 d . . . C114 C -0.0658(7) -0.0135(4) 0.3147(5) 0.075(3) Uani 1 1 d . . . H114 H -0.1291 -0.0434 0.3266 0.090 Uiso 1 1 calc R . . C115 C 0.0301(6) -0.0010(4) 0.3490(4) 0.055(2) Uani 1 1 d . . . N121 N 0.1607(4) -0.0021(3) 0.4266(3) 0.0476(14) Uani 1 1 d . . . C122 C 0.0571(6) -0.0278(4) 0.4078(4) 0.054(2) Uani 1 1 d . . . C123 C -0.0111(7) -0.0745(5) 0.4443(5) 0.069(3) Uani 1 1 d . . . H123 H -0.0820 -0.0919 0.4313 0.083 Uiso 1 1 calc R . . C124 C 0.0259(8) -0.0952(5) 0.5001(5) 0.075(3) Uani 1 1 d . . . H124 H -0.0198 -0.1263 0.5248 0.091 Uiso 1 1 calc R . . C125 C 0.1303(7) -0.0697(4) 0.5187(4) 0.064(2) Uani 1 1 d . . . H125 H 0.1577 -0.0831 0.5558 0.076 Uiso 1 1 calc R . . C126 C 0.1931(6) -0.0230(4) 0.4795(4) 0.0535(19) Uani 1 1 d . . . H126 H 0.2642 -0.0050 0.4918 0.064 Uiso 1 1 calc R . . Na1 Na 0.5438(3) 0.44673(16) 0.18510(12) 0.0602(8) Uani 1 1 d . . . O200 O 0.4050(4) 0.2345(3) 0.1440(2) 0.0539(13) Uani 1 1 d . . . C201 C 0.3896(8) 0.2594(4) 0.0824(3) 0.067(3) Uani 1 1 d . . . H20E H 0.3517 0.2989 0.0831 0.080 Uiso 1 1 calc R . . H20F H 0.3494 0.2136 0.0547 0.080 Uiso 1 1 calc R . . C202 C 0.4943(9) 0.2949(4) 0.0599(4) 0.078(3) Uani 1 1 d . . . H20A H 0.5432 0.2681 0.0765 0.094 Uiso 1 1 calc R . . H20B H 0.4884 0.2874 0.0152 0.094 Uiso 1 1 calc R . . O203 O 0.5312(5) 0.3785(3) 0.0793(2) 0.0706(17) Uani 1 1 d . . . C204 C 0.6249(9) 0.4160(5) 0.0525(4) 0.084(3) Uani 1 1 d . . . H20I H 0.6185 0.3964 0.0095 0.101 Uiso 1 1 calc R . . H20J H 0.6834 0.4035 0.0740 0.101 Uiso 1 1 calc R . . C205 C 0.6419(9) 0.5052(5) 0.0576(4) 0.086(3) Uani 1 1 d . . . H20K H 0.7026 0.5316 0.0376 0.103 Uiso 1 1 calc R . . H20L H 0.5822 0.5174 0.0371 0.103 Uiso 1 1 calc R . . O206 O 0.6564(5) 0.5335(3) 0.1209(2) 0.0689(16) Uani 1 1 d . . . C207 C 0.6597(8) 0.6171(4) 0.1290(4) 0.068(2) Uani 1 1 d . . . H20G H 0.5972 0.6250 0.1084 0.082 Uiso 1 1 calc R . . H20H H 0.7192 0.6503 0.1113 0.082 Uiso 1 1 calc R . . C208 C 0.6676(7) 0.6392(4) 0.1956(4) 0.063(2) Uani 1 1 d . . . H20C H 0.7310 0.6323 0.2159 0.076 Uiso 1 1 calc R . . H20D H 0.6697 0.6950 0.2027 0.076 Uiso 1 1 calc R . . O209 O 0.5801(4) 0.5892(3) 0.2199(2) 0.0574(14) Uani 1 1 d . . . C210 C 0.5742(7) 0.6098(4) 0.2828(3) 0.061(2) Uani 1 1 d . . . H21G H 0.5538 0.6586 0.2870 0.074 Uiso 1 1 calc R . . H21H H 0.6415 0.6189 0.3062 0.074 Uiso 1 1 calc R . . C211 C 0.4971(8) 0.5435(4) 0.3062(3) 0.064(2) Uani 1 1 d . . . H21E H 0.4898 0.5568 0.3490 0.077 Uiso 1 1 calc R . . H21F H 0.4301 0.5338 0.2824 0.077 Uiso 1 1 calc R . . O212 O 0.5321(5) 0.4727(3) 0.3011(2) 0.0573(14) Uani 1 1 d . . . C213 C 0.4941(6) 0.4178(4) 0.3453(3) 0.0489(18) Uani 1 1 d . . . H21C H 0.4191 0.3965 0.3378 0.059 Uiso 1 1 calc R . . H21D H 0.5117 0.4448 0.3865 0.059 Uiso 1 1 calc R . . C214 C 0.5434(6) 0.3510(3) 0.3397(3) 0.0429(16) Uani 1 1 d . . . H21A H 0.6129 0.3714 0.3274 0.051 Uiso 1 1 calc R . . H21B H 0.5485 0.3285 0.3791 0.051 Uiso 1 1 calc R . . O215 O 0.4793(4) 0.2896(2) 0.29360(19) 0.0442(11) Uani 1 1 d . . . Na2 Na 0.0730(2) -0.44812(15) 0.36341(12) 0.0487(7) Uani 1 1 d . . . O300 O 0.0793(4) -0.1974(2) 0.3345(2) 0.0444(11) Uani 1 1 d . . . C301 C -0.0208(6) -0.2449(4) 0.3493(4) 0.058(2) Uani 1 1 d . C . H30C H -0.0465 -0.2922 0.3204 0.069 Uiso 1 1 calc R . . H30D H -0.0699 -0.2139 0.3457 0.069 Uiso 1 1 calc R . . C302 C -0.0117(7) -0.2697(4) 0.4135(4) 0.057(2) Uani 1 1 d . . . H30E H 0.0302 -0.2240 0.4406 0.069 Uiso 1 1 calc R C . H30F H -0.0804 -0.2864 0.4275 0.069 Uiso 1 1 calc R . . O303 O 0.0343(4) -0.3342(3) 0.4175(2) 0.0512(12) Uani 1 1 d . C . C304 C 0.0139(7) -0.3718(4) 0.4743(3) 0.057(2) Uani 1 1 d . C . H30G H 0.0105 -0.3323 0.5064 0.068 Uiso 1 1 calc R . . H30H H 0.0699 -0.3938 0.4874 0.068 Uiso 1 1 calc R . . C305 C -0.0874(6) -0.4379(4) 0.4647(3) 0.056(2) Uani 1 1 d . . . H30A H -0.1041 -0.4607 0.5034 0.068 Uiso 1 1 calc R C . H30B H -0.1432 -0.4169 0.4493 0.068 Uiso 1 1 calc R . . O306 O -0.0758(4) -0.4978(3) 0.4208(2) 0.0537(13) Uani 1 1 d . C . C307 C -0.1645(7) -0.5365(5) 0.3803(4) 0.067(2) Uani 1 1 d . . . H30I H -0.2259 -0.5432 0.4019 0.081 Uiso 1 1 calc R C . H30J H -0.1615 -0.5894 0.3664 0.081 Uiso 1 1 calc R . . C308 C -0.1731(7) -0.4883(5) 0.3240(3) 0.065(2) Uani 1 1 d . C . H30K H -0.2359 -0.5142 0.2968 0.077 Uiso 1 1 calc R . . H30L H -0.1732 -0.4342 0.3368 0.077 Uiso 1 1 calc R . . O309 O -0.0812(4) -0.4875(3) 0.2940(2) 0.0576(13) Uani 1 1 d . C . C310 C -0.0732(7) -0.4471(5) 0.2391(4) 0.070(2) Uani 1 1 d . . . H31E H -0.0829 -0.3946 0.2465 0.085 Uiso 1 1 calc R C . H31F H -0.1263 -0.4775 0.2070 0.085 Uiso 1 1 calc R . . C311 C 0.0317(7) -0.4389(5) 0.2194(3) 0.062(2) Uani 1 1 d . C . H31G H 0.0420 -0.4913 0.2130 0.074 Uiso 1 1 calc R . . H31H H 0.0387 -0.4133 0.1810 0.074 Uiso 1 1 calc R . . O312 O 0.1065(4) -0.3915(3) 0.2665(2) 0.0523(13) Uani 1 1 d . C . C313 C 0.2093(6) -0.3801(4) 0.2488(4) 0.057(2) Uani 1 1 d . . . H31C H 0.2127 -0.3628 0.2073 0.069 Uiso 1 1 calc R C . H31D H 0.2271 -0.4300 0.2494 0.069 Uiso 1 1 calc R . . C314 C 0.2834(6) -0.3181(4) 0.2931(4) 0.0516(18) Uani 1 1 d . C . H31A H 0.2741 -0.3318 0.3352 0.062 Uiso 1 1 calc R . . H31B H 0.3544 -0.3141 0.2858 0.062 Uiso 1 1 calc R . . O315 O 0.2617(4) -0.2436(2) 0.28362(19) 0.0435(11) Uani 1 1 d . . . Cl1 Cl 0.73708(13) 0.86390(10) 0.13062(7) 0.0461(4) Uani 1 1 d D . . O1A O 0.7773(4) 0.8473(3) 0.1899(2) 0.0541(12) Uani 1 1 d D . . O1B O 0.7061(5) 0.9356(3) 0.1349(3) 0.0711(16) Uani 1 1 d D . . O1C O 0.6492(5) 0.7992(3) 0.1076(3) 0.0709(16) Uani 1 1 d D . . O1D O 0.8149(4) 0.8729(4) 0.0899(2) 0.0754(18) Uani 1 1 d D . . Cl2 Cl 0.70169(13) 0.80675(9) 0.39666(7) 0.0469(4) Uani 1 1 d . . . O2A O 0.7424(4) 0.8259(4) 0.3396(2) 0.0651(15) Uani 1 1 d . . . O2B O 0.6988(7) 0.8803(4) 0.4278(3) 0.106(3) Uani 1 1 d . . . O2C O 0.5982(4) 0.7579(3) 0.3872(2) 0.0608(14) Uani 1 1 d . . . O2D O 0.7662(5) 0.7735(5) 0.4329(3) 0.108(3) Uani 1 1 d . . . Cl3A Cl 0.1074(6) 0.8331(6) 0.9126(4) 0.072(2) Uani 0.55 1 d PD A 1 O3A O 0.0641(10) 0.8977(7) 0.9185(5) 0.0799(14) Uani 0.55 1 d PD A 1 O3B O 0.1903(9) 0.8578(7) 0.8729(5) 0.0799(14) Uani 0.55 1 d PD A 1 O3C O 0.1453(15) 0.8230(9) 0.9739(6) 0.0799(14) Uani 0.55 1 d PD A 1 O3D O 0.0338(11) 0.7655(7) 0.8806(5) 0.0799(14) Uani 0.55 1 d PD A 1 Cl3B Cl 0.0756(9) 0.8213(8) 0.9265(6) 0.072(2) Uani 0.45 1 d PD B 2 O3E O 0.0053(11) 0.8596(9) 0.9468(6) 0.0799(14) Uani 0.45 1 d PD B 2 O3F O 0.1407(12) 0.8763(9) 0.8870(6) 0.0799(14) Uani 0.45 1 d PD B 2 O3G O 0.1461(17) 0.8055(11) 0.9725(8) 0.0799(14) Uani 0.45 1 d PD B 2 O3H O 0.0199(14) 0.7474(8) 0.8973(7) 0.0799(14) Uani 0.45 1 d PD B 2 Cl4 Cl 0.3173(2) 0.45162(12) 0.12967(10) 0.0739(6) Uani 1 1 d . . . O4A O 0.3981(5) 0.5081(4) 0.1016(3) 0.0799(18) Uani 1 1 d . . . O4B O 0.2565(6) 0.4936(4) 0.1607(3) 0.097(2) Uani 1 1 d . . . O4C O 0.2521(6) 0.3931(4) 0.0834(3) 0.089(2) Uani 1 1 d . . . O4D O 0.3647(5) 0.4098(3) 0.1749(3) 0.0755(17) Uani 1 1 d . . . Cl5 Cl 0.90509(17) 0.21812(13) 0.35560(9) 0.0653(6) Uani 1 1 d D . . O5A O 0.8488(4) 0.1353(3) 0.3463(3) 0.0720(16) Uani 1 1 d D . . O5B O 0.9725(6) 0.2261(4) 0.3054(4) 0.132(2) Uani 1 1 d D . . O5C O 0.9777(5) 0.2357(5) 0.4082(3) 0.108(3) Uani 1 1 d D . . O5D O 0.8475(6) 0.2664(4) 0.3487(5) 0.132(2) Uani 1 1 d DU . . Cl6 Cl 0.31921(15) -0.40628(11) 0.45975(9) 0.0610(5) Uani 1 1 d D . . O6G O 0.3927(4) -0.3522(3) 0.4302(2) 0.0736(17) Uani 1 1 d D C . O6A O 0.2184(7) -0.3975(7) 0.4353(6) 0.0820(17) Uani 0.50 1 d PDU C 1 O6C O 0.3150(9) -0.4863(5) 0.4386(5) 0.0820(17) Uani 0.50 1 d PDU C 1 O6E O 0.3365(10) -0.3916(8) 0.5225(4) 0.0820(17) Uani 0.50 1 d PDU C 1 O6B O 0.2247(8) -0.4408(7) 0.4319(6) 0.0820(17) Uani 0.50 1 d PDU C 2 O6D O 0.3565(9) -0.4533(6) 0.4984(5) 0.0820(17) Uani 0.50 1 d PDU C 2 O6F O 0.3000(9) -0.3522(7) 0.5130(5) 0.0820(17) Uani 0.50 1 d PDU C 2 C0A C 0.8312(13) 0.3145(10) 0.2074(8) 0.082(4) Uiso 0.60 1 d PD D 1 H300 H 0.8787 0.3421 0.1800 0.123 Uiso 0.60 1 calc PR D 1 H301 H 0.8078 0.2583 0.1945 0.123 Uiso 0.60 1 calc PR D 1 H302 H 0.8656 0.3224 0.2486 0.123 Uiso 0.60 1 calc PR D 1 C1A C 0.7423(11) 0.3460(8) 0.2062(6) 0.048(3) Uiso 0.60 1 d PD D 1 C0B C 0.777(2) 0.2772(16) 0.1797(13) 0.096(8) Uiso 0.40 1 d PD D 2 H303 H 0.8398 0.3107 0.1663 0.145 Uiso 0.40 1 calc PR D 2 H304 H 0.7430 0.2357 0.1478 0.145 Uiso 0.40 1 calc PR D 2 H305 H 0.7938 0.2533 0.2164 0.145 Uiso 0.40 1 calc PR D 2 C1B C 0.709(2) 0.3247(14) 0.1927(12) 0.067(7) Uiso 0.40 1 d PD D 2 N2 N 0.6684(6) 0.3701(4) 0.2061(3) 0.0644(18) Uani 1 1 d D . . C3 C 0.1471(9) -0.6687(6) 0.2424(5) 0.088(3) Uani 1 1 d . C . H3A H 0.1108 -0.6683 0.2026 0.131 Uiso 1 1 calc R . . H3B H 0.1210 -0.7203 0.2579 0.131 Uiso 1 1 calc R . . H3C H 0.2200 -0.6581 0.2386 0.131 Uiso 1 1 calc R . . C4 C 0.1314(7) -0.6088(4) 0.2838(4) 0.061(2) Uani 1 1 d . . . N5 N 0.1194(6) -0.5590(4) 0.3165(3) 0.072(2) Uani 1 1 d . C . C6 C 0.8925(13) 0.7345(9) 0.0223(7) 0.057(4) Uiso 0.50 1 d P . . H6A H 0.8617 0.7732 0.0389 0.086 Uiso 0.50 1 calc PR . . H6B H 0.8394 0.6913 -0.0007 0.086 Uiso 0.50 1 calc PR . . H6C H 0.9429 0.7596 -0.0044 0.086 Uiso 0.50 1 calc PR . . C7 C 0.9400(14) 0.7049(10) 0.0695(8) 0.060(4) Uiso 0.50 1 d P . . N8 N 0.9794(14) 0.6869(10) 0.1036(8) 0.087(5) Uiso 0.50 1 d P . . 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 0.0372(5) 0.0280(4) 0.0358(4) 0.0030(3) 0.0026(4) 0.0106(4) N11 0.056(4) 0.033(3) 0.035(3) -0.002(2) 0.008(3) 0.010(2) C12 0.049(5) 0.045(4) 0.058(4) -0.012(3) 0.019(4) 0.004(3) C13 0.066(6) 0.047(4) 0.074(5) -0.015(4) 0.033(5) 0.000(4) C14 0.101(8) 0.034(4) 0.056(4) 0.000(3) 0.033(5) 0.007(4) C15 0.088(7) 0.036(4) 0.042(4) 0.002(3) 0.020(4) 0.008(4) C16 0.080(6) 0.027(3) 0.035(3) -0.005(2) 0.011(4) 0.012(3) N21 0.055(4) 0.031(3) 0.030(2) -0.0001(19) 0.004(2) 0.014(2) C22 0.064(5) 0.030(3) 0.040(3) -0.002(2) 0.010(3) 0.011(3) C23 0.113(7) 0.043(4) 0.034(3) -0.003(3) -0.049(4) 0.031(4) S24 0.0568(12) 0.0514(10) 0.0493(9) 0.0037(7) -0.0137(9) 0.0115(8) C25 0.043(4) 0.034(3) 0.048(3) -0.008(3) -0.003(3) 0.011(3) N31 0.043(3) 0.018(2) 0.047(3) -0.001(2) 0.005(3) 0.010(2) C32 0.030(4) 0.029(3) 0.040(3) -0.007(2) -0.010(3) 0.009(2) C33 0.036(4) 0.035(3) 0.054(4) -0.010(3) -0.004(3) 0.013(3) C34 0.037(4) 0.034(3) 0.067(4) 0.002(3) 0.012(4) 0.006(3) C35 0.045(4) 0.029(3) 0.055(4) -0.006(3) 0.008(3) 0.012(3) C36 0.038(4) 0.018(3) 0.046(3) -0.001(2) 0.007(3) 0.005(2) N71 0.042(3) 0.026(2) 0.040(3) 0.003(2) 0.011(2) 0.010(2) C72 0.038(4) 0.034(3) 0.040(3) 0.007(2) 0.017(3) 0.012(3) C73 0.051(4) 0.032(3) 0.059(4) 0.010(3) 0.018(3) 0.019(3) C74 0.071(6) 0.032(3) 0.059(4) 0.002(3) 0.023(4) 0.015(3) C75 0.068(6) 0.035(4) 0.053(4) -0.004(3) 0.014(4) 0.006(3) C76 0.047(4) 0.040(4) 0.041(3) 0.000(3) 0.002(3) 0.007(3) N81 0.027(3) 0.033(3) 0.038(2) 0.003(2) 0.003(2) 0.011(2) C82 0.029(3) 0.040(3) 0.042(3) 0.006(3) 0.008(3) 0.011(3) S83 0.0319(9) 0.0434(9) 0.0581(9) 0.0042(7) 0.0013(8) 0.0137(7) C84 0.045(4) 0.041(4) 0.057(4) 0.006(3) 0.015(3) 0.021(3) C85 0.039(4) 0.034(3) 0.040(3) 0.010(2) 0.012(3) 0.015(3) N91 0.033(3) 0.030(3) 0.034(2) 0.0040(19) -0.002(2) 0.009(2) C92 0.041(4) 0.031(3) 0.040(3) 0.004(2) 0.010(3) 0.006(3) C93 0.033(4) 0.043(4) 0.048(3) 0.007(3) 0.004(3) 0.006(3) C94 0.044(4) 0.037(3) 0.038(3) 0.002(3) -0.007(3) -0.001(3) C95 0.050(4) 0.026(3) 0.035(3) 0.004(2) 0.000(3) 0.006(3) C96 0.041(4) 0.033(3) 0.032(3) -0.003(2) 0.007(3) 0.002(3) Cu2 0.0303(5) 0.0335(5) 0.0528(5) -0.0059(4) 0.0027(4) 0.0060(4) N41 0.031(3) 0.034(3) 0.040(3) 0.007(2) 0.007(2) 0.011(2) C42 0.043(4) 0.040(3) 0.039(3) 0.010(3) 0.012(3) 0.019(3) C43 0.038(4) 0.051(4) 0.038(3) 0.007(3) 0.007(3) 0.015(3) C44 0.052(5) 0.042(4) 0.047(4) 0.017(3) 0.017(3) 0.027(3) C45 0.047(4) 0.030(3) 0.043(3) 0.010(2) 0.019(3) 0.015(3) C46 0.033(3) 0.029(3) 0.036(3) 0.011(2) 0.012(3) 0.013(2) N51 0.036(3) 0.036(3) 0.039(3) 0.002(2) 0.007(2) 0.009(2) C52 0.041(4) 0.035(3) 0.043(3) 0.009(3) 0.009(3) 0.012(3) S53 0.0407(10) 0.0490(9) 0.0478(9) 0.0052(7) -0.0031(8) 0.0128(7) C54 0.046(5) 0.041(4) 0.043(3) 0.002(3) -0.003(3) 0.000(3) C55 0.031(4) 0.039(3) 0.036(3) 0.000(2) -0.001(3) 0.001(3) N61 0.038(3) 0.031(3) 0.043(3) -0.008(2) -0.003(3) 0.005(2) C62 0.037(4) 0.036(3) 0.034(3) 0.004(2) 0.002(3) 0.010(3) C63 0.041(4) 0.039(3) 0.041(3) 0.000(3) 0.004(3) 0.005(3) C64 0.053(5) 0.034(3) 0.044(3) -0.003(3) 0.005(3) 0.003(3) C65 0.044(4) 0.037(3) 0.056(4) 0.001(3) 0.001(3) 0.015(3) C66 0.040(4) 0.041(4) 0.057(4) -0.005(3) -0.002(3) 0.010(3) N101 0.032(3) 0.031(3) 0.043(3) -0.010(2) -0.014(2) 0.014(2) C102 0.052(4) 0.026(3) 0.041(3) -0.004(2) -0.011(3) 0.019(3) C103 0.074(6) 0.031(3) 0.045(4) -0.009(3) -0.011(4) 0.024(3) C104 0.076(6) 0.046(4) 0.050(4) -0.006(3) -0.015(4) 0.026(4) C105 0.061(5) 0.042(4) 0.069(5) -0.020(4) -0.035(4) 0.028(4) C106 0.053(5) 0.027(3) 0.067(4) -0.018(3) -0.016(4) 0.019(3) N111 0.029(3) 0.034(3) 0.078(4) -0.015(3) 0.007(3) 0.009(2) C112 0.031(4) 0.032(3) 0.074(5) -0.019(3) -0.014(3) 0.015(3) S113 0.0363(11) 0.0460(10) 0.1207(18) -0.0273(11) -0.0189(11) 0.0190(8) C114 0.048(5) 0.037(4) 0.134(8) -0.015(5) 0.012(5) 0.007(3) C115 0.035(4) 0.032(3) 0.095(6) -0.015(4) 0.001(4) 0.011(3) N121 0.029(3) 0.035(3) 0.078(4) -0.003(3) 0.013(3) 0.007(2) C122 0.041(4) 0.030(3) 0.090(5) -0.008(3) 0.024(4) 0.004(3) C123 0.041(5) 0.045(4) 0.120(8) -0.011(5) 0.024(5) 0.007(3) C124 0.067(6) 0.042(4) 0.124(8) 0.011(5) 0.052(6) 0.015(4) C125 0.066(6) 0.040(4) 0.091(6) 0.008(4) 0.036(5) 0.017(4) C126 0.049(5) 0.039(4) 0.073(5) -0.004(3) 0.014(4) 0.014(3) Na1 0.093(2) 0.0382(14) 0.0491(14) -0.0026(11) 0.0116(15) 0.0189(14) O200 0.078(4) 0.039(3) 0.043(2) 0.0046(19) -0.004(2) 0.018(2) C201 0.128(8) 0.038(4) 0.035(3) -0.002(3) -0.012(4) 0.031(4) C202 0.153(10) 0.041(4) 0.047(4) -0.001(3) 0.023(5) 0.037(5) O203 0.127(5) 0.036(3) 0.051(3) 0.000(2) 0.016(3) 0.025(3) C204 0.148(10) 0.053(5) 0.055(5) 0.009(4) 0.041(6) 0.028(5) C205 0.146(10) 0.047(5) 0.067(5) 0.003(4) 0.039(6) 0.023(5) O206 0.102(5) 0.042(3) 0.070(3) 0.006(2) 0.026(3) 0.027(3) C207 0.087(7) 0.041(4) 0.082(5) 0.011(4) 0.031(5) 0.020(4) C208 0.071(6) 0.035(4) 0.082(5) 0.001(4) 0.008(5) 0.013(4) O209 0.079(4) 0.038(3) 0.051(3) -0.002(2) 0.007(3) 0.012(2) C210 0.086(6) 0.043(4) 0.057(4) -0.008(3) -0.004(4) 0.027(4) C211 0.095(7) 0.050(4) 0.052(4) -0.006(3) 0.017(4) 0.029(4) O212 0.093(4) 0.037(2) 0.048(3) 0.002(2) 0.021(3) 0.026(2) C213 0.066(5) 0.036(3) 0.035(3) -0.005(3) 0.003(3) 0.003(3) C214 0.051(4) 0.031(3) 0.035(3) -0.004(2) -0.002(3) -0.002(3) O215 0.055(3) 0.028(2) 0.044(2) -0.0034(17) -0.003(2) 0.0070(19) Na2 0.0523(17) 0.0403(14) 0.0507(14) -0.0011(11) 0.0111(13) 0.0083(12) O300 0.041(3) 0.037(2) 0.058(3) 0.0117(19) 0.018(2) 0.0104(19) C301 0.052(5) 0.040(4) 0.089(5) 0.016(4) 0.030(4) 0.019(3) C302 0.066(5) 0.040(4) 0.074(5) 0.018(3) 0.029(4) 0.021(3) O303 0.055(3) 0.036(2) 0.064(3) 0.007(2) 0.018(2) 0.012(2) C304 0.082(6) 0.036(4) 0.050(4) 0.001(3) 0.015(4) 0.012(4) C305 0.067(5) 0.045(4) 0.051(4) 0.004(3) 0.025(4) 0.002(3) O306 0.059(3) 0.040(3) 0.056(3) -0.004(2) 0.012(2) 0.004(2) C307 0.060(6) 0.052(4) 0.072(5) -0.008(4) 0.017(4) -0.012(4) C308 0.060(6) 0.068(5) 0.054(4) -0.007(4) 0.013(4) 0.001(4) O309 0.053(3) 0.066(3) 0.049(3) -0.003(2) 0.008(2) 0.009(2) C310 0.081(7) 0.072(5) 0.053(4) -0.003(4) 0.015(4) 0.013(5) C311 0.075(6) 0.065(5) 0.053(4) 0.008(4) 0.024(4) 0.029(4) O312 0.065(3) 0.043(3) 0.050(3) 0.001(2) 0.021(3) 0.015(2) C313 0.065(5) 0.033(4) 0.078(5) 0.004(3) 0.035(4) 0.014(3) C314 0.055(5) 0.033(3) 0.078(5) 0.019(3) 0.025(4) 0.023(3) O315 0.058(3) 0.032(2) 0.049(2) 0.0081(18) 0.015(2) 0.022(2) Cl1 0.0372(9) 0.0519(9) 0.0504(9) 0.0184(7) 0.0071(7) 0.0114(7) O1A 0.046(3) 0.073(3) 0.051(3) 0.026(2) 0.013(2) 0.025(2) O1B 0.087(4) 0.046(3) 0.085(4) 0.021(3) 0.012(3) 0.024(3) O1C 0.083(4) 0.052(3) 0.075(3) 0.016(3) -0.004(3) 0.016(3) O1D 0.054(4) 0.127(5) 0.056(3) 0.045(3) 0.019(3) 0.035(3) Cl2 0.0375(9) 0.0425(8) 0.0549(9) 0.0086(7) 0.0012(7) 0.0025(7) O2A 0.039(3) 0.091(4) 0.072(3) 0.041(3) 0.012(3) 0.023(3) O2B 0.125(7) 0.077(4) 0.097(5) -0.029(4) -0.011(4) 0.012(4) O2C 0.046(3) 0.059(3) 0.074(3) 0.005(3) 0.011(3) 0.008(2) O2D 0.052(4) 0.161(7) 0.135(6) 0.111(6) 0.027(4) 0.047(4) Cl3A 0.065(5) 0.075(3) 0.075(4) -0.021(3) -0.024(3) 0.032(4) O3A 0.087(3) 0.083(4) 0.076(3) -0.003(2) -0.010(2) 0.042(3) O3B 0.087(3) 0.083(4) 0.076(3) -0.003(2) -0.010(2) 0.042(3) O3C 0.087(3) 0.083(4) 0.076(3) -0.003(2) -0.010(2) 0.042(3) O3D 0.087(3) 0.083(4) 0.076(3) -0.003(2) -0.010(2) 0.042(3) Cl3B 0.065(5) 0.075(3) 0.075(4) -0.021(3) -0.024(3) 0.032(4) O3E 0.087(3) 0.083(4) 0.076(3) -0.003(2) -0.010(2) 0.042(3) O3F 0.087(3) 0.083(4) 0.076(3) -0.003(2) -0.010(2) 0.042(3) O3G 0.087(3) 0.083(4) 0.076(3) -0.003(2) -0.010(2) 0.042(3) O3H 0.087(3) 0.083(4) 0.076(3) -0.003(2) -0.010(2) 0.042(3) Cl4 0.0929(17) 0.0505(11) 0.0809(13) -0.0173(10) 0.0080(12) 0.0294(11) O4A 0.087(5) 0.060(4) 0.093(4) 0.004(3) 0.017(4) 0.021(3) O4B 0.126(6) 0.071(4) 0.112(5) -0.012(4) 0.036(5) 0.052(4) O4C 0.101(5) 0.068(4) 0.102(5) -0.022(3) -0.017(4) 0.043(4) O4D 0.101(5) 0.060(3) 0.072(3) 0.004(3) 0.003(3) 0.035(3) Cl5 0.0473(12) 0.0684(12) 0.0650(11) 0.0057(9) 0.0019(10) -0.0060(9) O5A 0.063(4) 0.065(3) 0.086(4) -0.022(3) -0.017(3) 0.028(3) O5B 0.092(4) 0.066(3) 0.217(7) -0.034(4) -0.034(4) 0.014(3) O5C 0.065(5) 0.137(6) 0.102(5) -0.059(5) -0.017(4) 0.020(4) O5D 0.092(4) 0.066(3) 0.217(7) -0.034(4) -0.034(4) 0.014(3) Cl6 0.0441(11) 0.0544(10) 0.0761(12) 0.0197(9) 0.0034(9) -0.0006(8) O6G 0.053(4) 0.083(4) 0.070(3) 0.022(3) 0.003(3) -0.004(3) O6A 0.070(4) 0.076(4) 0.090(3) 0.011(3) -0.003(3) 0.008(3) O6C 0.070(4) 0.076(4) 0.090(3) 0.011(3) -0.003(3) 0.008(3) O6E 0.070(4) 0.076(4) 0.090(3) 0.011(3) -0.003(3) 0.008(3) O6B 0.070(4) 0.076(4) 0.090(3) 0.011(3) -0.003(3) 0.008(3) O6D 0.070(4) 0.076(4) 0.090(3) 0.011(3) -0.003(3) 0.008(3) O6F 0.070(4) 0.076(4) 0.090(3) 0.011(3) -0.003(3) 0.008(3) N2 0.087(6) 0.054(4) 0.053(3) 0.003(3) 0.010(4) 0.023(4) C3 0.113(9) 0.064(6) 0.090(6) -0.008(5) 0.025(6) 0.031(5) C4 0.079(6) 0.036(4) 0.070(5) 0.009(4) 0.009(4) 0.019(4) N5 0.092(6) 0.040(4) 0.088(5) 0.007(3) 0.005(4) 0.028(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N21 1.928(6) . ? Cu1 N81 1.929(5) . ? Cu1 N11 2.168(5) . ? Cu1 N71 2.195(5) . ? Cu1 N31 2.451(5) . ? Cu1 N91 2.479(5) . ? N11 C12 1.319(9) . ? N11 C16 1.357(9) . ? C12 C13 1.420(10) . ? C13 C14 1.380(13) . ? C14 C15 1.370(12) . ? C15 C16 1.397(9) . ? C16 C22 1.449(11) . ? N21 C25 1.319(9) . ? N21 C22 1.361(8) . ? C22 C23 1.415(11) . ? C23 S24 1.636(10) . ? S24 C25 1.702(7) . ? C25 C32 1.452(9) . ? N31 C36 1.306(7) . ? N31 C32 1.370(8) . ? C32 C33 1.379(9) . ? C33 C34 1.368(10) . ? C34 C35 1.389(10) . ? C35 O300 1.346(8) . ? C35 C36 1.422(9) . ? C36 C46 1.489(9) . ? N71 C76 1.346(8) . ? N71 C72 1.359(8) . ? C72 C73 1.373(9) . ? C72 C85 1.470(9) . ? C73 C74 1.386(10) . ? C74 C75 1.370(11) . ? C75 C76 1.360(9) . ? N81 C82 1.301(8) . ? N81 C85 1.372(8) . ? C82 C92 1.471(9) . ? C82 S83 1.721(7) . ? S83 C84 1.725(7) . ? C84 C85 1.355(10) . ? N91 C96 1.333(8) . ? N91 C92 1.350(8) . ? C92 C93 1.381(9) . ? C93 C94 1.386(10) . ? C94 C95 1.388(10) . ? C95 O215 1.348(8) . ? C95 C96 1.413(8) . ? C96 C102 1.480(10) . ? Cu2 N51 1.931(6) . ? Cu2 N111 1.934(6) . ? Cu2 N61 2.153(5) . ? Cu2 N121 2.162(6) . ? Cu2 N41 2.447(5) . ? N41 C46 1.307(7) . ? N41 C42 1.361(8) . ? C42 C43 1.385(9) . ? C42 C52 1.456(9) . ? C43 C44 1.378(9) . ? C44 C45 1.382(10) . ? C45 O315 1.350(7) . ? C45 C46 1.411(9) . ? N51 C52 1.315(8) . ? N51 C55 1.388(7) . ? C52 S53 1.713(7) . ? S53 C54 1.718(8) . ? C54 C55 1.362(10) . ? C55 C62 1.461(9) . ? N61 C66 1.333(9) . ? N61 C62 1.342(8) . ? C62 C63 1.383(8) . ? C63 C64 1.386(10) . ? C64 C65 1.374(10) . ? C65 C66 1.388(9) . ? N101 C102 1.307(8) . ? N101 C106 1.360(9) . ? C102 C103 1.425(9) . ? C103 O200 1.348(9) . ? C103 C104 1.386(11) . ? C104 C105 1.373(12) . ? C105 C106 1.401(11) . ? C106 C112 1.470(11) . ? N111 C112 1.329(10) . ? N111 C115 1.355(9) . ? C112 S113 1.694(7) . ? S113 C114 1.705(11) . ? C114 C115 1.393(12) . ? C115 C122 1.441(12) . ? N121 C126 1.306(10) . ? N121 C122 1.359(9) . ? C122 C123 1.384(11) . ? C123 C124 1.382(14) . ? C124 C125 1.368(13) . ? C125 C126 1.386(10) . ? Na1 O4D 2.304(8) . ? Na1 O206 2.418(6) . ? Na1 O209 2.458(5) . ? Na1 N2 2.461(8) . ? Na1 O203 2.510(5) . ? Na1 O212 2.574(5) . ? Na1 Cl4 3.217(4) . ? O200 C201 1.452(8) . ? C201 C202 1.508(13) . ? C202 O203 1.428(9) . ? O203 C204 1.438(11) . ? C204 C205 1.504(11) . ? C205 O206 1.420(10) . ? O206 C207 1.448(9) . ? C207 C208 1.471(11) . ? C208 O209 1.417(9) . ? O209 C210 1.415(8) . ? C210 C211 1.466(11) . ? C211 O212 1.447(9) . ? O212 C213 1.419(8) . ? C213 C214 1.505(10) . ? C214 O215 1.454(7) . ? Na2 O6A 2.330(11) . ? Na2 O309 2.372(6) . ? Na2 O6B 2.398(11) . ? Na2 O312 2.405(5) . ? Na2 N5 2.405(7) . ? Na2 O306 2.432(5) . ? Na2 O303 2.466(5) . ? Na2 C304 2.978(7) . ? O300 C301 1.442(8) . ? C301 C302 1.493(11) . ? C302 O303 1.437(9) . ? O303 C304 1.444(8) . ? C304 C305 1.505(10) . ? C305 O306 1.432(8) . ? O306 C307 1.402(9) . ? C307 C308 1.540(12) . ? C308 O309 1.450(9) . ? O309 C310 1.420(10) . ? C310 C311 1.485(12) . ? C311 O312 1.418(9) . ? O312 C313 1.435(9) . ? C313 C314 1.486(11) . ? C314 O315 1.433(8) . ? Cl1 O1D 1.415(5) . ? Cl1 O1C 1.416(5) . ? Cl1 O1B 1.431(6) . ? Cl1 O1A 1.435(5) . ? Cl2 O2D 1.394(6) . ? Cl2 O2C 1.405(5) . ? Cl2 O2A 1.422(5) . ? Cl2 O2B 1.432(7) . ? Cl3A O3D 1.410(11) . ? Cl3A O3A 1.416(11) . ? Cl3A O3C 1.430(11) . ? Cl3A O3B 1.456(11) . ? Cl3B O3H 1.381(12) . ? Cl3B O3E 1.396(12) . ? Cl3B O3G 1.416(12) . ? Cl3B O3F 1.474(13) . ? Cl4 O4B 1.435(6) . ? Cl4 O4C 1.436(6) . ? Cl4 O4A 1.450(7) . ? Cl4 O4D 1.468(6) . ? Cl5 O5D 1.306(8) . ? Cl5 O5C 1.404(7) . ? Cl5 O5A 1.423(6) . ? Cl5 O5B 1.472(9) . ? Cl6 O6B 1.322(9) . ? Cl6 O6E 1.368(9) . ? Cl6 O6D 1.370(9) . ? Cl6 O6G 1.389(5) . ? Cl6 O6C 1.433(9) . ? Cl6 O6A 1.471(10) . ? Cl6 O6F 1.544(9) . ? C0A C1A 1.455(15) . ? C1A N2 1.188(12) . ? C0B C1B 1.436(18) . ? C1B N2 1.128(16) . ? C3 C4 1.420(11) . ? C4 N5 1.152(10) . ? C6 C7 1.37(2) . ? C7 N8 0.99(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N21 Cu1 N81 175.9(2) . . ? N21 Cu1 N11 78.8(2) . . ? N81 Cu1 N11 99.3(2) . . ? N21 Cu1 N71 99.4(2) . . ? N81 Cu1 N71 77.6(2) . . ? N11 Cu1 N71 106.46(18) . . ? N21 Cu1 N31 71.9(2) . . ? N81 Cu1 N31 110.36(19) . . ? N11 Cu1 N31 149.9(2) . . ? N71 Cu1 N31 85.16(16) . . ? N21 Cu1 N91 110.72(18) . . ? N81 Cu1 N91 72.57(18) . . ? N11 Cu1 N91 84.54(16) . . ? N71 Cu1 N91 149.54(19) . . ? N31 Cu1 N91 99.45(15) . . ? C12 N11 C16 119.7(6) . . ? C12 N11 Cu1 129.1(5) . . ? C16 N11 Cu1 111.2(4) . . ? N11 C12 C13 122.6(8) . . ? C14 C13 C12 116.5(8) . . ? C15 C14 C13 121.7(7) . . ? C14 C15 C16 118.2(8) . . ? N11 C16 C15 121.3(7) . . ? N11 C16 C22 115.3(6) . . ? C15 C16 C22 123.4(7) . . ? C25 N21 C22 114.3(6) . . ? C25 N21 Cu1 125.7(4) . . ? C22 N21 Cu1 119.1(5) . . ? N21 C22 C23 109.2(7) . . ? N21 C22 C16 115.1(6) . . ? C23 C22 C16 135.7(7) . . ? C22 C23 S24 113.4(5) . . ? C23 S24 C25 90.6(3) . . ? N21 C25 C32 119.5(6) . . ? N21 C25 S24 112.5(5) . . ? C32 C25 S24 128.0(5) . . ? C36 N31 C32 118.3(5) . . ? C36 N31 Cu1 130.2(4) . . ? C32 N31 Cu1 109.4(4) . . ? N31 C32 C33 121.2(6) . . ? N31 C32 C25 111.3(5) . . ? C33 C32 C25 127.4(6) . . ? C34 C33 C32 120.4(6) . . ? C33 C34 C35 119.3(6) . . ? O300 C35 C34 127.0(6) . . ? O300 C35 C36 115.9(6) . . ? C34 C35 C36 117.0(6) . . ? N31 C36 C35 123.8(6) . . ? N31 C36 C46 116.2(5) . . ? C35 C36 C46 120.0(5) . . ? C76 N71 C72 118.5(5) . . ? C76 N71 Cu1 128.1(5) . . ? C72 N71 Cu1 113.4(4) . . ? N71 C72 C73 121.7(6) . . ? N71 C72 C85 112.9(5) . . ? C73 C72 C85 125.5(7) . . ? C72 C73 C74 118.9(7) . . ? C75 C74 C73 119.1(6) . . ? C76 C75 C74 119.8(7) . . ? N71 C76 C75 122.0(7) . . ? C82 N81 C85 113.9(5) . . ? C82 N81 Cu1 125.5(4) . . ? C85 N81 Cu1 120.4(4) . . ? N81 C82 C92 119.6(6) . . ? N81 C82 S83 112.4(5) . . ? C92 C82 S83 128.0(5) . . ? C82 S83 C84 90.0(3) . . ? C85 C84 S83 110.2(5) . . ? C84 C85 N81 113.4(6) . . ? C84 C85 C72 130.9(6) . . ? N81 C85 C72 115.7(6) . . ? C96 N91 C92 118.6(5) . . ? C96 N91 Cu1 132.7(4) . . ? C92 N91 Cu1 107.8(4) . . ? N91 C92 C93 122.6(6) . . ? N91 C92 C82 113.0(5) . . ? C93 C92 C82 124.3(7) . . ? C92 C93 C94 118.9(7) . . ? C93 C94 C95 119.3(6) . . ? O215 C95 C94 126.9(5) . . ? O215 C95 C96 114.9(6) . . ? C94 C95 C96 118.1(6) . . ? N91 C96 C95 122.3(6) . . ? N91 C96 C102 114.6(5) . . ? C95 C96 C102 122.8(6) . . ? N51 Cu2 N111 178.3(2) . . ? N51 Cu2 N61 78.3(2) . . ? N111 Cu2 N61 101.7(2) . . ? N51 Cu2 N121 100.2(2) . . ? N111 Cu2 N121 78.2(3) . . ? N61 Cu2 N121 105.3(2) . . ? N51 Cu2 N41 71.76(19) . . ? N111 Cu2 N41 108.38(19) . . ? N61 Cu2 N41 149.6(2) . . ? N121 Cu2 N41 85.42(18) . . ? C46 N41 C42 117.3(5) . . ? C46 N41 Cu2 131.5(4) . . ? C42 N41 Cu2 109.4(4) . . ? N41 C42 C43 122.0(6) . . ? N41 C42 C52 112.4(6) . . ? C43 C42 C52 125.6(6) . . ? C44 C43 C42 120.4(7) . . ? C43 C44 C45 117.8(6) . . ? O315 C45 C44 127.8(6) . . ? O315 C45 C46 113.8(6) . . ? C44 C45 C46 118.2(6) . . ? N41 C46 C45 124.3(6) . . ? N41 C46 C36 115.6(5) . . ? C45 C46 C36 120.0(5) . . ? C52 N51 C55 113.9(6) . . ? C52 N51 Cu2 127.1(4) . . ? C55 N51 Cu2 119.0(4) . . ? N51 C52 C42 117.8(6) . . ? N51 C52 S53 112.5(5) . . ? C42 C52 S53 129.6(5) . . ? C52 S53 C54 90.2(3) . . ? C55 C54 S53 111.4(5) . . ? C54 C55 N51 112.0(6) . . ? C54 C55 C62 133.0(6) . . ? N51 C55 C62 115.0(6) . . ? C66 N61 C62 118.2(5) . . ? C66 N61 Cu2 127.6(4) . . ? C62 N61 Cu2 114.0(4) . . ? N61 C62 C63 123.3(6) . . ? N61 C62 C55 113.5(5) . . ? C63 C62 C55 123.1(6) . . ? C62 C63 C64 117.1(6) . . ? C65 C64 C63 120.7(6) . . ? C64 C65 C66 117.9(7) . . ? N61 C66 C65 122.7(7) . . ? C102 N101 C106 118.3(6) . . ? N101 C102 C103 123.6(7) . . ? N101 C102 C96 114.4(5) . . ? C103 C102 C96 121.7(6) . . ? O200 C103 C104 126.0(7) . . ? O200 C103 C102 116.6(7) . . ? C104 C103 C102 117.4(7) . . ? C105 C104 C103 119.6(7) . . ? C104 C105 C106 119.2(7) . . ? N101 C106 C105 121.9(7) . . ? N101 C106 C112 113.9(7) . . ? C105 C106 C112 124.2(7) . . ? C112 N111 C115 113.0(6) . . ? C112 N111 Cu2 128.0(5) . . ? C115 N111 Cu2 119.0(6) . . ? N111 C112 C106 117.9(6) . . ? N111 C112 S113 113.8(6) . . ? C106 C112 S113 128.2(6) . . ? C112 S113 C114 90.0(4) . . ? C115 C114 S113 110.9(7) . . ? N111 C115 C114 112.3(8) . . ? N111 C115 C122 116.6(7) . . ? C114 C115 C122 131.0(8) . . ? C126 N121 C122 118.2(6) . . ? C126 N121 Cu2 129.0(5) . . ? C122 N121 Cu2 112.8(5) . . ? N121 C122 C123 120.2(9) . . ? N121 C122 C115 113.4(6) . . ? C123 C122 C115 126.4(8) . . ? C124 C123 C122 120.0(8) . . ? C125 C124 C123 119.6(8) . . ? C124 C125 C126 116.7(9) . . ? N121 C126 C125 125.3(8) . . ? O4D Na1 O206 126.4(3) . . ? O4D Na1 O209 99.3(2) . . ? O206 Na1 O209 67.90(18) . . ? O4D Na1 N2 132.0(2) . . ? O206 Na1 N2 92.4(2) . . ? O209 Na1 N2 123.1(2) . . ? O4D Na1 O203 87.5(2) . . ? O206 Na1 O203 69.31(19) . . ? O209 Na1 O203 131.02(19) . . ? N2 Na1 O203 81.0(2) . . ? O4D Na1 O212 85.8(2) . . ? O206 Na1 O212 127.1(2) . . ? O209 Na1 O212 66.01(16) . . ? N2 Na1 O212 91.7(2) . . ? O203 Na1 O212 162.63(19) . . ? O4D Na1 Cl4 24.39(16) . . ? O206 Na1 Cl4 102.19(19) . . ? O209 Na1 Cl4 87.30(17) . . ? N2 Na1 Cl4 149.51(19) . . ? O203 Na1 Cl4 79.44(18) . . ? O212 Na1 Cl4 100.22(17) . . ? C103 O200 C201 116.6(6) . . ? O200 C201 C202 108.8(7) . . ? O203 C202 C201 109.4(7) . . ? C202 O203 C204 110.6(6) . . ? C202 O203 Na1 128.9(4) . . ? C204 O203 Na1 107.9(4) . . ? O203 C204 C205 108.4(8) . . ? O206 C205 C204 109.2(7) . . ? C205 O206 C207 111.9(6) . . ? C205 O206 Na1 114.4(5) . . ? C207 O206 Na1 114.5(4) . . ? O206 C207 C208 107.8(7) . . ? O209 C208 C207 108.7(6) . . ? C210 O209 C208 113.8(6) . . ? C210 O209 Na1 118.4(4) . . ? C208 O209 Na1 113.0(4) . . ? O209 C210 C211 108.3(6) . . ? O212 C211 C210 108.3(7) . . ? C213 O212 C211 112.8(5) . . ? C213 O212 Na1 129.9(3) . . ? C211 O212 Na1 105.1(4) . . ? O212 C213 C214 108.1(5) . . ? O215 C214 C213 108.5(6) . . ? C95 O215 C214 115.2(5) . . ? O6A Na2 O309 173.7(4) . . ? O6A Na2 O6B 19.0(4) . . ? O309 Na2 O6B 166.8(3) . . ? O6A Na2 O312 110.0(3) . . ? O309 Na2 O312 70.08(19) . . ? O6B Na2 O312 115.2(3) . . ? O6A Na2 N5 98.8(4) . . ? O309 Na2 N5 87.5(2) . . ? O6B Na2 N5 81.3(4) . . ? O312 Na2 N5 84.1(2) . . ? O6A Na2 O306 107.2(3) . . ? O309 Na2 O306 70.69(18) . . ? O6B Na2 O306 106.6(3) . . ? O312 Na2 O306 137.5(2) . . ? N5 Na2 O306 109.8(2) . . ? O6A Na2 O303 77.5(3) . . ? O309 Na2 O303 96.2(2) . . ? O6B Na2 O303 94.9(4) . . ? O312 Na2 O303 98.31(18) . . ? N5 Na2 O303 176.1(3) . . ? O306 Na2 O303 70.49(16) . . ? O6A Na2 C304 70.3(3) . . ? O309 Na2 C304 104.4(2) . . ? O6B Na2 C304 82.3(4) . . ? O312 Na2 C304 127.2(2) . . ? N5 Na2 C304 148.7(3) . . ? O306 Na2 C304 50.78(17) . . ? O303 Na2 C304 28.86(17) . . ? C35 O300 C301 118.3(6) . . ? O300 C301 C302 110.1(7) . . ? O303 C302 C301 112.2(6) . . ? C302 O303 C304 110.3(5) . . ? C302 O303 Na2 147.4(5) . . ? C304 O303 Na2 95.6(4) . . ? O303 C304 C305 109.8(6) . . ? O303 C304 Na2 55.5(3) . . ? C305 C304 Na2 86.7(4) . . ? O306 C305 C304 107.6(6) . . ? C307 O306 C305 115.6(6) . . ? C307 O306 Na2 110.2(4) . . ? C305 O306 Na2 112.4(4) . . ? O306 C307 C308 111.3(6) . . ? O309 C308 C307 103.7(7) . . ? C310 O309 C308 114.0(7) . . ? C310 O309 Na2 113.8(5) . . ? C308 O309 Na2 112.7(4) . . ? O309 C310 C311 108.1(8) . . ? O312 C311 C310 108.1(6) . . ? C311 O312 C313 110.1(5) . . ? C311 O312 Na2 109.0(4) . . ? C313 O312 Na2 116.4(5) . . ? O312 C313 C314 108.4(5) . . ? O315 C314 C313 106.9(6) . . ? C45 O315 C314 119.2(5) . . ? O1D Cl1 O1C 109.8(4) . . ? O1D Cl1 O1B 109.2(4) . . ? O1C Cl1 O1B 108.6(4) . . ? O1D Cl1 O1A 109.0(3) . . ? O1C Cl1 O1A 109.1(3) . . ? O1B Cl1 O1A 111.1(3) . . ? O2D Cl2 O2C 113.0(4) . . ? O2D Cl2 O2A 110.3(4) . . ? O2C Cl2 O2A 111.1(3) . . ? O2D Cl2 O2B 109.0(5) . . ? O2C Cl2 O2B 105.9(4) . . ? O2A Cl2 O2B 107.2(4) . . ? O3D Cl3A O3A 110.3(9) . . ? O3D Cl3A O3C 116.1(10) . . ? O3A Cl3A O3C 105.4(9) . . ? O3D Cl3A O3B 105.9(9) . . ? O3A Cl3A O3B 106.2(9) . . ? O3C Cl3A O3B 112.6(10) . . ? O3H Cl3B O3E 108.4(11) . . ? O3H Cl3B O3G 105.7(12) . . ? O3E Cl3B O3G 116.6(12) . . ? O3H Cl3B O3F 114.8(12) . . ? O3E Cl3B O3F 106.3(11) . . ? O3G Cl3B O3F 105.4(13) . . ? O4B Cl4 O4C 110.2(5) . . ? O4B Cl4 O4A 109.8(4) . . ? O4C Cl4 O4A 110.0(4) . . ? O4B Cl4 O4D 108.7(4) . . ? O4C Cl4 O4D 108.5(4) . . ? O4A Cl4 O4D 109.6(4) . . ? O4B Cl4 Na1 123.6(4) . . ? O4C Cl4 Na1 123.3(3) . . ? O4A Cl4 Na1 69.2(3) . . ? O4D Cl4 Na1 40.4(3) . . ? Cl4 O4D Na1 115.2(4) . . ? O5D Cl5 O5C 116.0(5) . . ? O5D Cl5 O5A 114.2(4) . . ? O5C Cl5 O5A 112.5(5) . . ? O5D Cl5 O5B 109.0(6) . . ? O5C Cl5 O5B 102.0(5) . . ? O5A Cl5 O5B 101.1(4) . . ? O6B Cl6 O6E 121.1(8) . . ? O6B Cl6 O6D 114.6(7) . . ? O6E Cl6 O6D 55.8(7) . . ? O6B Cl6 O6G 120.6(6) . . ? O6E Cl6 O6G 112.0(5) . . ? O6D Cl6 O6G 116.1(6) . . ? O6B Cl6 O6C 72.8(7) . . ? O6E Cl6 O6C 113.6(7) . . ? O6D Cl6 O6C 59.9(7) . . ? O6G Cl6 O6C 109.2(5) . . ? O6B Cl6 O6A 32.1(6) . . ? O6E Cl6 O6A 111.9(7) . . ? O6D Cl6 O6A 138.6(7) . . ? O6G Cl6 O6A 105.2(5) . . ? O6C Cl6 O6A 104.5(6) . . ? O6B Cl6 O6F 103.0(7) . . ? O6E Cl6 O6F 38.5(6) . . ? O6D Cl6 O6F 94.0(6) . . ? O6G Cl6 O6F 102.2(5) . . ? O6C Cl6 O6F 145.6(6) . . ? O6A Cl6 O6F 79.8(7) . . ? Cl6 O6A Na2 145.6(8) . . ? Cl6 O6B Na2 155.1(8) . . ? N2 C1A C0A 178.2(15) . . ? N2 C1B C0B 170(3) . . ? C1B N2 C1A 27.0(14) . . ? C1B N2 Na1 152.8(15) . . ? C1A N2 Na1 163.1(8) . . ? N5 C4 C3 178.6(9) . . ? C4 N5 Na2 166.5(7) . . ? N8 C7 C6 176(2) . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 70.02 _diffrn_measured_fraction_theta_full 0.889 _refine_diff_density_max 1.742 _refine_diff_density_min -0.908 _refine_diff_density_rms 0.113 data_craig7dm _database_code_depnum_ccdc_archive 'CCDC 270153' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H72 Ba2 Cl8 Cu2 N12 O46 S4' _chemical_formula_weight 2655.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -1.0456 8.4617 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.1100(3) _cell_length_b 19.0281(5) _cell_length_c 19.2925(5) _cell_angle_alpha 73.4950(10) _cell_angle_beta 80.5840(10) _cell_angle_gamma 75.3780(10) _cell_volume 4781.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 4.799 _cell_measurement_theta_max 139.770 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.844 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2652 _exptl_absorpt_coefficient_mu 10.595 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.259761 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; The complex cation features two Cu(II) coordination domains incorporated into a metallo-helical array with 18-crown-6 macrocycles spanning the central bipyrings on each side of the molecule. Ba2+ cations occupy both of the crown ether host cavities, each being stabilised by six Ba-O interactions (with the crown ethers) and axially coordinating water and perchlorate ligands. Although the Cu(II) coordination domains and peripheral crown ethers are well resolved, the two guest Ba2+ ions are each disordered over two positions - one with 0.9:0.1 [Ba(1a) and (1b)] and one with 0.55:0.45 [Ba(2a) and (2b)] site occupancies. The Ba(1a)/(1b) components were refined with ADP restraints (ISOR and DELU). The disorder associated with Ba(2) is coupled with that of a coordinating water molecule [O(40a) and (40b)] and perchlorate anion [ClO4(8a) and (8b)], such that the site occupancies of the latter fragments correspond to those of the Ba(2) positions (ie. 0.55:0.45). Thus, the disordered perchlorate mentioned above [ClO4( ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source '4.8 kW rotating anode' _diffrn_radiation_monochromator 'Osmic ConFocal MaxFlux mirror optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Frames, each covering 0.3 \% in \w' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37734 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 70.21 _reflns_number_total 16319 _reflns_number_gt 13719 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16319 _refine_ls_number_parameters 1368 _refine_ls_number_restraints 232 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1883 _refine_ls_wR_factor_gt 0.1724 _refine_ls_goodness_of_fit_ref 0.797 _refine_ls_restrained_S_all 0.809 _refine_ls_shift/su_max 0.353 _refine_ls_shift/su_mean 0.006 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 0.49392(5) 0.27930(4) 0.77227(3) 0.03728(18) Uani 1 1 d . . . N11 N 0.5215(3) 0.3698(3) 0.8085(2) 0.0446(10) Uani 1 1 d . . . C12 C 0.5378(4) 0.4365(3) 0.7693(3) 0.0465(12) Uani 1 1 d . . . H1 H 0.5216 0.4539 0.7216 0.056 Uiso 1 1 calc R . . C13 C 0.5784(4) 0.4806(4) 0.7975(3) 0.0528(13) Uani 1 1 d . . . H2 H 0.5865 0.5279 0.7698 0.063 Uiso 1 1 calc R . . C14 C 0.6062(4) 0.4538(4) 0.8666(3) 0.0538(14) Uani 1 1 d . . . H3 H 0.6364 0.4816 0.8853 0.065 Uiso 1 1 calc R . . C15 C 0.5893(4) 0.3854(3) 0.9081(3) 0.0498(13) Uani 1 1 d . . . H4 H 0.6073 0.3666 0.9552 0.060 Uiso 1 1 calc R . . C16 C 0.5452(3) 0.3453(3) 0.8784(3) 0.0456(12) Uani 1 1 d . . . N21 N 0.4808(3) 0.2402(3) 0.8766(2) 0.0415(10) Uani 1 1 d . . . C22 C 0.5186(3) 0.2740(3) 0.9167(2) 0.0430(11) Uani 1 1 d . . . C23 C 0.5248(4) 0.2338(4) 0.9877(3) 0.0510(13) Uani 1 1 d . . . H5 H 0.5480 0.2484 1.0227 0.061 Uiso 1 1 calc R . . S24 S 0.48384(10) 0.15315(8) 1.00287(6) 0.0490(3) Uani 1 1 d . . . C25 C 0.4608(3) 0.1753(3) 0.9143(2) 0.0394(11) Uani 1 1 d . . . N31 N 0.4340(3) 0.1557(2) 0.80519(19) 0.0356(8) Uani 1 1 d . . . C32 C 0.4321(3) 0.1274(3) 0.8783(2) 0.0371(10) Uani 1 1 d . . . C33 C 0.4061(3) 0.0603(3) 0.9140(2) 0.0417(11) Uani 1 1 d . . . H6 H 0.4021 0.0446 0.9644 0.050 Uiso 1 1 calc R . . C34 C 0.3858(3) 0.0164(3) 0.8747(2) 0.0402(11) Uani 1 1 d . . . H7 H 0.3671 -0.0287 0.8978 0.048 Uiso 1 1 calc R . . C35 C 0.3943(3) 0.0417(3) 0.7996(2) 0.0372(10) Uani 1 1 d . . . C36 C 0.4140(3) 0.1130(3) 0.7671(2) 0.0352(10) Uani 1 1 d . . . Ba1A Ba 0.57448(4) -0.06802(3) 0.67244(3) 0.03908(14) Uani 0.90 1 d PU . 1 Ba1B Ba 0.5639(4) -0.0640(3) 0.6441(3) 0.0490(11) Uani 0.10 1 d PU . 2 O200 O 0.3835(2) 0.0013(2) 0.75417(17) 0.0427(7) Uani 1 1 d . . . C201 C 0.3329(4) -0.0598(3) 0.7888(3) 0.0510(12) Uani 1 1 d . . . H20A H 0.2693 -0.0403 0.8123 0.061 Uiso 1 1 calc R . . H20B H 0.3712 -0.0967 0.8256 0.061 Uiso 1 1 calc R . . C202 C 0.3193(4) -0.0956(4) 0.7332(3) 0.0533(13) Uani 1 1 d . . . H20C H 0.2753 -0.1298 0.7536 0.064 Uiso 1 1 calc R . . H20D H 0.2907 -0.0576 0.6923 0.064 Uiso 1 1 calc R . . O203 O 0.4137(3) -0.1359(2) 0.7097(2) 0.0499(8) Uani 1 1 d . . . C204 C 0.4097(5) -0.1861(4) 0.6687(4) 0.0592(14) Uani 1 1 d . . . H20E H 0.4020 -0.1590 0.6184 0.071 Uiso 1 1 calc R . . H20F H 0.3540 -0.2095 0.6878 0.071 Uiso 1 1 calc R . . C205 C 0.5048(5) -0.2453(4) 0.6737(3) 0.0597(14) Uani 1 1 d . . . H20G H 0.5114 -0.2735 0.7238 0.072 Uiso 1 1 calc R . . H20H H 0.5047 -0.2800 0.6453 0.072 Uiso 1 1 calc R . . O206 O 0.5838(3) -0.2091(2) 0.6467(2) 0.0542(9) Uani 1 1 d . . . C207 C 0.6762(4) -0.2609(3) 0.6551(3) 0.0530(13) Uani 1 1 d . . . H20I H 0.6772 -0.3026 0.6353 0.064 Uiso 1 1 calc R . . H20J H 0.6853 -0.2806 0.7064 0.064 Uiso 1 1 calc R . . C208 C 0.7566(5) -0.2239(4) 0.6175(3) 0.0556(14) Uani 1 1 d . . . H20K H 0.8190 -0.2600 0.6226 0.067 Uiso 1 1 calc R . . H20L H 0.7481 -0.2046 0.5662 0.067 Uiso 1 1 calc R . . O209 O 0.7574(3) -0.1631(2) 0.64791(18) 0.0468(8) Uani 1 1 d . . . C210 C 0.8394(4) -0.1286(3) 0.6163(3) 0.0485(12) Uani 1 1 d . . . H21A H 0.8381 -0.1109 0.5641 0.058 Uiso 1 1 calc R . . H21B H 0.9007 -0.1650 0.6265 0.058 Uiso 1 1 calc R . . C211 C 0.8329(4) -0.0643(3) 0.6480(3) 0.0494(12) Uani 1 1 d . . . H21C H 0.8314 -0.0813 0.7005 0.059 Uiso 1 1 calc R . . H21D H 0.8894 -0.0417 0.6293 0.059 Uiso 1 1 calc R . . O212 O 0.7435(2) -0.0105(2) 0.62746(18) 0.0426(7) Uani 1 1 d . . . C213 C 0.7419(3) 0.0623(3) 0.6351(3) 0.0416(10) Uani 1 1 d . . . H21E H 0.8010 0.0788 0.6101 0.050 Uiso 1 1 calc R . . H21F H 0.7387 0.0611 0.6860 0.050 Uiso 1 1 calc R . . C214 C 0.6529(3) 0.1147(3) 0.6025(2) 0.0391(10) Uani 1 1 d . . . H21G H 0.6566 0.1662 0.5970 0.047 Uiso 1 1 calc R . . H21H H 0.6498 0.1083 0.5549 0.047 Uiso 1 1 calc R . . O215 O 0.5653(2) 0.0986(2) 0.64984(15) 0.0395(7) Uani 1 1 d . . . N71 N 0.6451(3) 0.2195(3) 0.7599(2) 0.0408(9) Uani 1 1 d . . . C72 C 0.6990(4) 0.1710(3) 0.8118(3) 0.0437(11) Uani 1 1 d . . . H8 H 0.6676 0.1537 0.8576 0.052 Uiso 1 1 calc R . . C73 C 0.7990(4) 0.1458(3) 0.7996(3) 0.0481(12) Uani 1 1 d . . . H9 H 0.8348 0.1127 0.8367 0.058 Uiso 1 1 calc R . . C74 C 0.8452(4) 0.1704(4) 0.7316(3) 0.0532(13) Uani 1 1 d . . . H10 H 0.9126 0.1533 0.7222 0.064 Uiso 1 1 calc R . . C75 C 0.7903(4) 0.2214(3) 0.6765(3) 0.0449(11) Uani 1 1 d . . . H11 H 0.8206 0.2398 0.6305 0.054 Uiso 1 1 calc R . . C76 C 0.6899(4) 0.2434(3) 0.6928(3) 0.0405(10) Uani 1 1 d . . . N81 N 0.5275(3) 0.3150(2) 0.67011(19) 0.0376(8) Uani 1 1 d . . . C82 C 0.6225(4) 0.2963(3) 0.6415(2) 0.0397(10) Uani 1 1 d . . . C83 C 0.6373(4) 0.3310(3) 0.5695(3) 0.0447(11) Uani 1 1 d . . . H12 H 0.6973 0.3244 0.5412 0.054 Uiso 1 1 calc R . . S84 S 0.52975(9) 0.38856(8) 0.53852(6) 0.0461(3) Uani 1 1 d . . . C85 C 0.4703(4) 0.3643(3) 0.6237(2) 0.0391(10) Uani 1 1 d . . . N91 N 0.3445(3) 0.3614(2) 0.72010(19) 0.0370(8) Uani 1 1 d . . . C92 C 0.3680(3) 0.3923(3) 0.6487(2) 0.0374(10) Uani 1 1 d . . . C93 C 0.3022(4) 0.4467(3) 0.6048(2) 0.0412(10) Uani 1 1 d . . . H13 H 0.3210 0.4659 0.5559 0.049 Uiso 1 1 calc R . . C94 C 0.2086(4) 0.4718(3) 0.6349(2) 0.0413(11) Uani 1 1 d . . . H14 H 0.1627 0.5073 0.6062 0.050 Uiso 1 1 calc R . . C95 C 0.1834(3) 0.4435(3) 0.7081(2) 0.0375(10) Uani 1 1 d . A . C96 C 0.2538(3) 0.3866(3) 0.7492(2) 0.0367(10) Uani 1 1 d . . . Ba2A Ba 0.10145(4) 0.58536(3) 0.82793(3) 0.03503(15) Uani 0.55 1 d P A 1 Ba2B Ba 0.07122(5) 0.57394(4) 0.86091(5) 0.03777(17) Uani 0.45 1 d P . 2 O300 O 0.0952(2) 0.4657(2) 0.74447(16) 0.0420(8) Uani 1 1 d . . . C301 C 0.0151(4) 0.5070(3) 0.6999(3) 0.0430(11) Uani 1 1 d . A . H30A H 0.0058 0.4771 0.6694 0.052 Uiso 1 1 calc R . . H30B H 0.0310 0.5532 0.6687 0.052 Uiso 1 1 calc R . . C302 C -0.0757(4) 0.5241(3) 0.7475(3) 0.0495(12) Uani 1 1 d . . . H30C H -0.1326 0.5385 0.7203 0.059 Uiso 1 1 calc R A . H30D H -0.0825 0.4804 0.7871 0.059 Uiso 1 1 calc R . . O303 O -0.0689(3) 0.5845(2) 0.7753(2) 0.0521(9) Uani 1 1 d . A . C304 C -0.1602(4) 0.6210(4) 0.8075(3) 0.0572(15) Uani 1 1 d . . . H30E H -0.1711 0.5951 0.8583 0.069 Uiso 1 1 calc R A 2 H30F H -0.2145 0.6208 0.7826 0.069 Uiso 1 1 calc R A 2 C305 C -0.1527(4) 0.7006(4) 0.8002(4) 0.0647(17) Uani 1 1 d . A . H30G H -0.1403 0.7256 0.7493 0.078 Uiso 1 1 calc R . . H30H H -0.2143 0.7280 0.8194 0.078 Uiso 1 1 calc R . . O306 O -0.0745(3) 0.7001(2) 0.8390(2) 0.0577(10) Uani 1 1 d . . . C307 C -0.0557(6) 0.7734(4) 0.8236(3) 0.0683(18) Uani 1 1 d . A . H30I H -0.1154 0.8084 0.8352 0.082 Uiso 1 1 calc R . . H30J H -0.0348 0.7903 0.7723 0.082 Uiso 1 1 calc R . . C308 C 0.0223(6) 0.7716(4) 0.8674(3) 0.0685(18) Uani 1 1 d . . . H30K H 0.0350 0.8215 0.8576 0.082 Uiso 1 1 calc R A . H30L H 0.0011 0.7555 0.9187 0.082 Uiso 1 1 calc R . . O309 O 0.1106(4) 0.7203(2) 0.8489(2) 0.0619(11) Uani 1 1 d . A . C310 C 0.1904(6) 0.7182(4) 0.8875(3) 0.0691(19) Uani 1 1 d . . . H31A H 0.1727 0.7023 0.9394 0.083 Uiso 1 1 calc R A . H31B H 0.2041 0.7679 0.8764 0.083 Uiso 1 1 calc R . . C311 C 0.2783(5) 0.6653(4) 0.8661(3) 0.0636(17) Uani 1 1 d . A . H31C H 0.2951 0.6802 0.8140 0.076 Uiso 1 1 calc R . . H31D H 0.3336 0.6652 0.8900 0.076 Uiso 1 1 calc R . . O312 O 0.2568(3) 0.5910(2) 0.88702(19) 0.0482(8) Uani 1 1 d . . . C313 C 0.3432(4) 0.5323(4) 0.8873(4) 0.0623(16) Uani 1 1 d . A . H31E H 0.3906 0.5380 0.9153 0.075 Uiso 1 1 calc R . . H31F H 0.3733 0.5340 0.8381 0.075 Uiso 1 1 calc R . . C314 C 0.3128(4) 0.4598(4) 0.9203(3) 0.0530(14) Uani 1 1 d . . . H31G H 0.3702 0.4197 0.9322 0.064 Uiso 1 1 calc R A . H31H H 0.2699 0.4625 0.9647 0.064 Uiso 1 1 calc R . . O315 O 0.2609(3) 0.4448(2) 0.86803(18) 0.0440(8) Uani 1 1 d . A . Cu2 Cu 0.15456(5) 0.21977(4) 0.75729(3) 0.03771(18) Uani 1 1 d . . . N41 N 0.3155(3) 0.1979(2) 0.67704(19) 0.0356(8) Uani 1 1 d . . . C42 C 0.4029(3) 0.1532(3) 0.6886(2) 0.0352(9) Uani 1 1 d . . . C43 C 0.4798(3) 0.1482(3) 0.6325(2) 0.0358(9) Uani 1 1 d . . . C44 C 0.4636(4) 0.1945(3) 0.5633(2) 0.0454(12) Uani 1 1 d . . . H15 H 0.5135 0.1936 0.5253 0.054 Uiso 1 1 calc R . . C45 C 0.3731(3) 0.2414(3) 0.5518(2) 0.0411(11) Uani 1 1 d . . . H16 H 0.3607 0.2728 0.5061 0.049 Uiso 1 1 calc R . . C46 C 0.3002(3) 0.2412(3) 0.6096(2) 0.0400(10) Uani 1 1 d . . . N51 N 0.1378(3) 0.2856(2) 0.66219(19) 0.0356(8) Uani 1 1 d . . . C52 C 0.2009(3) 0.2875(3) 0.6041(2) 0.0388(10) Uani 1 1 d . . . S53 S 0.15226(9) 0.34785(8) 0.52807(6) 0.0467(3) Uani 1 1 d . . . C54 C 0.0415(4) 0.3687(3) 0.5774(3) 0.0462(12) Uani 1 1 d . . . H17 H -0.0143 0.4020 0.5584 0.055 Uiso 1 1 calc R . . C55 C 0.0460(3) 0.3297(3) 0.6486(2) 0.0380(10) Uani 1 1 d . . . N61 N 0.0055(3) 0.2806(2) 0.7736(2) 0.0398(9) Uani 1 1 d . . . C62 C -0.0289(3) 0.3262(3) 0.7105(3) 0.0412(10) Uani 1 1 d . . . C63 C -0.1258(4) 0.3637(3) 0.7056(3) 0.0458(11) Uani 1 1 d . . . H18 H -0.1474 0.3934 0.6613 0.055 Uiso 1 1 calc R . . C64 C -0.1900(4) 0.3562(3) 0.7680(3) 0.0517(13) Uani 1 1 d . . . H19 H -0.2557 0.3810 0.7662 0.062 Uiso 1 1 calc R . . C65 C -0.1561(4) 0.3116(3) 0.8335(3) 0.0498(12) Uani 1 1 d . . . H20 H -0.1979 0.3069 0.8764 0.060 Uiso 1 1 calc R . . C66 C -0.0578(4) 0.2741(3) 0.8332(3) 0.0455(11) Uani 1 1 d . . . H21 H -0.0352 0.2429 0.8766 0.055 Uiso 1 1 calc R . . N101 N 0.2087(3) 0.2805(2) 0.83737(19) 0.0367(8) Uani 1 1 d . . . C102 C 0.2317(3) 0.3472(3) 0.8266(2) 0.0371(10) Uani 1 1 d . A . C103 C 0.2424(3) 0.3748(3) 0.8849(2) 0.0394(10) Uani 1 1 d . . . C104 C 0.2350(4) 0.3302(3) 0.9550(3) 0.0469(12) Uani 1 1 d . A . H22 H 0.2447 0.3464 0.9939 0.056 Uiso 1 1 calc R . . C105 C 0.2127(3) 0.2607(3) 0.9662(2) 0.0432(11) Uani 1 1 d . . . H23 H 0.2077 0.2294 1.0128 0.052 Uiso 1 1 calc R A . C106 C 0.1979(3) 0.2380(3) 0.9068(2) 0.0396(10) Uani 1 1 d . A . N111 N 0.1546(3) 0.1529(2) 0.8535(2) 0.0407(9) Uani 1 1 d . A . C112 C 0.1700(3) 0.1688(3) 0.9126(2) 0.0427(11) Uani 1 1 d . . . S113 S 0.14621(9) 0.10131(8) 0.98975(6) 0.0469(3) Uani 1 1 d . A . C114 C 0.1118(4) 0.0535(3) 0.9391(3) 0.0463(12) Uani 1 1 d . . . H24 H 0.0899 0.0091 0.9582 0.056 Uiso 1 1 calc R A . C115 C 0.1202(3) 0.0883(3) 0.8674(3) 0.0428(11) Uani 1 1 d . A . N121 N 0.1228(3) 0.1192(3) 0.7394(2) 0.0436(9) Uani 1 1 d . A . C122 C 0.0986(3) 0.0710(3) 0.8025(3) 0.0452(11) Uani 1 1 d . . . C123 C 0.0561(4) 0.0123(3) 0.8051(3) 0.0527(13) Uani 1 1 d . A . H25 H 0.0383 -0.0191 0.8494 0.063 Uiso 1 1 calc R . . C124 C 0.0407(4) 0.0012(4) 0.7408(4) 0.0568(14) Uani 1 1 d . . . H26 H 0.0118 -0.0377 0.7411 0.068 Uiso 1 1 calc R A . C125 C 0.0688(4) 0.0486(4) 0.6752(4) 0.0581(14) Uani 1 1 d . A . H27 H 0.0611 0.0409 0.6312 0.070 Uiso 1 1 calc R . . C126 C 0.1085(4) 0.1078(3) 0.6770(3) 0.0480(12) Uani 1 1 d . . . H28 H 0.1257 0.1405 0.6334 0.058 Uiso 1 1 calc R A . Cl1 Cl 0.70177(8) -0.04613(7) 0.84840(5) 0.0423(3) Uani 1 1 d D . . O1A O 0.6467(3) -0.0245(2) 0.78553(18) 0.0518(9) Uani 1 1 d D . . O1B O 0.6510(3) -0.0050(3) 0.8995(2) 0.0606(11) Uani 1 1 d D . . O1C O 0.7993(3) -0.0322(2) 0.8260(2) 0.0526(9) Uani 1 1 d D . . O1D O 0.7095(3) -0.1263(2) 0.8809(2) 0.0545(9) Uani 1 1 d D . . Cl2 Cl 0.28376(10) 0.47325(8) 0.40306(6) 0.0516(3) Uani 1 1 d . . . O2A O 0.3377(5) 0.5309(3) 0.3792(3) 0.0850(15) Uani 1 1 d . . . O2B O 0.1944(4) 0.5015(3) 0.4422(3) 0.098(2) Uani 1 1 d . . . O2C O 0.2674(4) 0.4533(3) 0.3414(3) 0.0790(14) Uani 1 1 d . . . O2D O 0.3381(3) 0.4070(3) 0.4501(2) 0.0652(12) Uani 1 1 d . . . Cl3 Cl 0.42712(9) 0.34740(8) 0.11091(6) 0.0461(3) Uani 1 1 d . . . O3A O 0.4614(3) 0.4049(3) 0.0537(2) 0.0621(11) Uani 1 1 d . . . O3B O 0.5093(3) 0.2853(2) 0.1316(2) 0.0524(9) Uani 1 1 d . . . O3C O 0.3548(3) 0.3208(3) 0.0865(2) 0.0570(10) Uani 1 1 d . . . O3D O 0.3867(3) 0.3755(2) 0.1733(2) 0.0540(9) Uani 1 1 d . . . Cl4A Cl 0.79756(18) 0.14060(15) 0.00557(14) 0.0413(9) Uiso 0.75 1 d PDU B 1 O4A O 0.8191(4) 0.1177(3) 0.0814(3) 0.0503(11) Uiso 0.75 1 d PDU B 1 O4B O 0.8849(4) 0.1265(3) -0.0391(3) 0.0491(12) Uiso 0.75 1 d PDU B 1 O4C O 0.7256(5) 0.1018(4) 0.0004(4) 0.0575(18) Uiso 0.75 1 d PDU B 1 O4D O 0.7515(6) 0.2211(4) -0.0073(5) 0.059(2) Uiso 0.75 1 d PDU B 1 Cl4B Cl 0.7890(5) 0.1491(4) 0.0125(4) 0.037(2) Uiso 0.25 1 d PDU C 2 O4E O 0.7581(14) 0.2229(7) -0.0230(11) 0.046(6) Uiso 0.25 1 d PDU C 2 O4F O 0.7680(18) 0.1237(13) 0.0861(7) 0.085(6) Uiso 0.25 1 d PDU C 2 O4G O 0.7431(12) 0.1013(9) -0.0180(9) 0.044(4) Uiso 0.25 1 d PDU C 2 O4H O 0.8922(11) 0.1301(14) -0.0129(14) 0.094(8) Uiso 0.25 1 d PDU C 2 Cl5 Cl 0.35832(9) 0.02918(9) 0.53877(6) 0.0531(3) Uani 1 1 d . . . O5A O 0.4208(3) 0.0228(3) 0.5918(2) 0.0634(11) Uani 1 1 d . . . O5B O 0.2623(5) 0.0556(8) 0.5630(4) 0.210(7) Uani 1 1 d . . . O5C O 0.3829(4) 0.0786(3) 0.4722(2) 0.0775(14) Uani 1 1 d . . . O5D O 0.3739(10) -0.0401(4) 0.5249(5) 0.162(5) Uani 1 1 d . . . Cl6 Cl -0.06410(11) 0.43940(8) 0.95590(6) 0.0532(3) Uani 1 1 d . . 2 O6A O -0.0337(5) 0.3874(4) 1.0204(3) 0.109(2) Uani 1 1 d . . 2 O6B O 0.0174(3) 0.4492(4) 0.9043(2) 0.0912(19) Uani 1 1 d . D 2 O6C O -0.1024(4) 0.5099(4) 0.9743(5) 0.110(3) Uani 1 1 d . . 2 O6D O -0.1422(4) 0.4247(4) 0.9282(3) 0.0861(16) Uani 1 1 d . E 2 Cl8A Cl 0.32761(18) 0.61471(15) 0.67184(12) 0.0521(5) Uani 0.55 1 d PD A 1 O8A O 0.2689(5) 0.5703(4) 0.7267(3) 0.0516(16) Uani 0.55 1 d PD A 1 O8B O 0.4190(7) 0.6041(7) 0.6969(7) 0.100(4) Uani 0.55 1 d PD A 1 O8C O 0.3295(6) 0.6008(4) 0.5995(3) 0.108(2) Uani 0.55 1 d PD A 1 O8D O 0.2789(9) 0.6934(5) 0.6606(7) 0.084(4) Uani 0.55 1 d PD A 1 Cl8B Cl 0.3760(3) 0.6434(2) 0.62472(16) 0.0624(8) Uani 0.45 1 d PD F 2 O8E O 0.3842(9) 0.7135(6) 0.5757(5) 0.072(3) Uani 0.45 1 d PD F 2 O8F O 0.4677(11) 0.5995(10) 0.6432(10) 0.167(10) Uani 0.45 1 d PD F 2 O8G O 0.3295(6) 0.6008(4) 0.5995(3) 0.108(2) Uani 0.45 1 d PD F 2 O8H O 0.3172(12) 0.6620(10) 0.6885(7) 0.094(5) Uani 0.45 1 d PD F 2 O40A O 0.0764(6) 0.6891(5) 0.6981(4) 0.064(2) Uani 0.55 1 d P A 1 O40B O 0.1368(8) 0.6249(6) 0.7207(5) 0.066(3) Uani 0.45 1 d P G 2 Cl9A Cl 0.9429(4) 0.2836(3) 0.4633(3) 0.0645(13) Uiso 0.35 1 d PDU H 1 O9A O 1.0209(9) 0.2333(8) 0.5058(7) 0.068(3) Uiso 0.35 1 d PDU H 1 O9B O 0.8521(8) 0.2623(8) 0.4979(7) 0.063(3) Uiso 0.35 1 d PDU H 1 O9C O 0.9362(9) 0.3602(6) 0.4595(7) 0.065(3) Uiso 0.35 1 d PDU H 1 O9D O 0.9627(8) 0.2681(6) 0.3945(5) 0.051(2) Uiso 0.35 1 d PDU H 1 Cl9B Cl 0.9408(2) 0.27405(18) 0.48756(19) 0.0672(7) Uiso 0.65 1 d PDU I 2 O9E O 1.0006(7) 0.2259(6) 0.5424(5) 0.092(3) Uiso 0.65 1 d PDU I 2 O9F O 0.8791(10) 0.2354(8) 0.4702(7) 0.131(4) Uiso 0.65 1 d PDU I 2 O9G O 0.8760(7) 0.3328(6) 0.5183(5) 0.101(3) Uiso 0.65 1 d PDU I 2 O9H O 1.0015(7) 0.3096(6) 0.4289(5) 0.091(2) Uiso 0.65 1 d PDU I 2 O400 O 0.5690(3) -0.1571(3) 0.8085(2) 0.0584(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0362(3) 0.0402(4) 0.0338(3) -0.0091(3) -0.0051(2) -0.0046(3) N11 0.0333(19) 0.056(3) 0.0442(19) -0.018(2) -0.0029(15) -0.0031(18) C12 0.041(2) 0.045(3) 0.050(2) -0.011(2) -0.007(2) -0.004(2) C13 0.042(3) 0.047(4) 0.066(3) -0.017(3) -0.005(2) -0.002(2) C14 0.041(3) 0.060(4) 0.070(3) -0.036(3) -0.011(2) -0.002(2) C15 0.045(3) 0.050(4) 0.055(3) -0.023(2) -0.011(2) 0.001(2) C16 0.035(2) 0.056(4) 0.047(2) -0.022(2) -0.0110(18) 0.004(2) N21 0.0347(18) 0.051(3) 0.0346(17) -0.0127(18) -0.0049(14) 0.0012(17) C22 0.037(2) 0.050(3) 0.040(2) -0.017(2) -0.0068(17) 0.003(2) C23 0.050(3) 0.064(4) 0.038(2) -0.016(2) -0.0097(19) -0.004(2) S24 0.0522(7) 0.0556(9) 0.0341(5) -0.0064(5) -0.0121(4) -0.0031(6) C25 0.034(2) 0.045(3) 0.0328(19) -0.008(2) -0.0012(16) -0.0017(19) N31 0.0353(18) 0.036(2) 0.0312(16) -0.0026(15) -0.0060(13) -0.0051(15) C32 0.032(2) 0.040(3) 0.0316(19) -0.0025(18) -0.0054(15) -0.0002(18) C33 0.035(2) 0.047(3) 0.0340(19) 0.001(2) -0.0067(16) -0.003(2) C34 0.035(2) 0.038(3) 0.040(2) 0.0039(19) -0.0031(17) -0.0102(19) C35 0.0298(19) 0.034(3) 0.041(2) -0.0009(19) -0.0056(16) -0.0036(17) C36 0.031(2) 0.038(3) 0.0310(19) -0.0027(18) -0.0047(15) -0.0037(18) Ba1A 0.0391(2) 0.0360(2) 0.0405(3) -0.0078(2) -0.0069(2) -0.00552(15) Ba1B 0.042(2) 0.036(2) 0.055(3) -0.008(2) 0.011(2) 0.0008(14) O200 0.0433(17) 0.039(2) 0.0439(16) -0.0041(14) -0.0060(13) -0.0121(14) C201 0.047(3) 0.044(3) 0.059(3) -0.006(2) -0.002(2) -0.014(2) C202 0.043(3) 0.052(4) 0.065(3) -0.008(3) -0.006(2) -0.017(2) O203 0.0446(18) 0.043(2) 0.063(2) -0.0112(17) -0.0060(16) -0.0120(16) C204 0.062(3) 0.051(4) 0.068(3) -0.015(3) -0.008(3) -0.017(3) C205 0.074(4) 0.045(4) 0.062(3) -0.010(3) -0.014(3) -0.015(3) O206 0.063(2) 0.033(2) 0.064(2) -0.0122(16) -0.0047(18) -0.0068(17) C207 0.064(3) 0.037(3) 0.056(3) -0.014(2) -0.013(2) 0.000(2) C208 0.064(3) 0.050(4) 0.050(3) -0.020(2) -0.010(2) 0.005(3) O209 0.0470(18) 0.042(2) 0.0457(17) -0.0126(15) -0.0040(14) 0.0013(15) C210 0.044(2) 0.047(3) 0.049(2) -0.011(2) -0.003(2) -0.001(2) C211 0.043(3) 0.050(3) 0.051(2) -0.016(2) -0.007(2) 0.002(2) O212 0.0371(16) 0.042(2) 0.0463(16) -0.0111(14) -0.0051(13) -0.0037(14) C213 0.037(2) 0.045(3) 0.044(2) -0.010(2) -0.0046(17) -0.011(2) C214 0.041(2) 0.038(3) 0.0351(19) -0.0066(18) 0.0031(17) -0.011(2) O215 0.0363(15) 0.042(2) 0.0328(13) -0.0039(13) -0.0007(11) -0.0035(13) N71 0.0392(19) 0.040(2) 0.0442(19) -0.0120(17) -0.0038(16) -0.0091(17) C72 0.044(2) 0.042(3) 0.042(2) -0.007(2) -0.0060(18) -0.006(2) C73 0.047(3) 0.045(3) 0.052(3) -0.013(2) -0.014(2) -0.002(2) C74 0.044(3) 0.052(4) 0.064(3) -0.021(3) -0.009(2) -0.002(2) C75 0.045(3) 0.040(3) 0.048(2) -0.008(2) -0.005(2) -0.011(2) C76 0.043(2) 0.034(3) 0.046(2) -0.012(2) -0.0072(19) -0.009(2) N81 0.0359(18) 0.037(2) 0.0379(17) -0.0100(16) -0.0032(14) -0.0048(16) C82 0.042(2) 0.041(3) 0.037(2) -0.0075(19) -0.0002(17) -0.013(2) C83 0.045(2) 0.043(3) 0.044(2) -0.007(2) 0.0024(19) -0.015(2) S84 0.0480(6) 0.0438(8) 0.0388(5) -0.0006(5) -0.0022(4) -0.0086(5) C85 0.045(2) 0.038(3) 0.0312(18) -0.0036(17) -0.0062(17) -0.008(2) N91 0.0393(19) 0.036(2) 0.0345(16) -0.0055(15) -0.0089(14) -0.0067(16) C92 0.042(2) 0.035(3) 0.0345(19) -0.0072(17) -0.0050(17) -0.0078(19) C93 0.049(3) 0.041(3) 0.0323(19) -0.0078(18) -0.0091(17) -0.006(2) C94 0.045(2) 0.037(3) 0.036(2) -0.0030(18) -0.0148(18) 0.002(2) C95 0.037(2) 0.032(3) 0.040(2) -0.0066(18) -0.0077(17) -0.0032(18) C96 0.042(2) 0.034(3) 0.035(2) -0.0061(18) -0.0085(17) -0.0092(19) Ba2A 0.0343(3) 0.0354(3) 0.0330(3) -0.0050(2) -0.0039(2) -0.0072(2) Ba2B 0.0390(4) 0.0342(4) 0.0385(4) -0.0058(3) -0.0066(3) -0.0072(3) O300 0.0379(16) 0.047(2) 0.0384(14) -0.0101(14) -0.0103(12) -0.0007(14) C301 0.046(3) 0.042(3) 0.042(2) -0.0104(19) -0.0157(19) -0.004(2) C302 0.042(3) 0.055(4) 0.051(3) -0.012(2) -0.010(2) -0.008(2) O303 0.0347(17) 0.061(3) 0.063(2) -0.0254(18) -0.0115(15) 0.0009(16) C304 0.041(3) 0.049(4) 0.064(3) -0.004(3) 0.004(2) 0.003(2) C305 0.051(3) 0.052(4) 0.070(3) -0.003(3) 0.002(3) 0.007(3) O306 0.070(2) 0.038(2) 0.0539(19) -0.0050(16) -0.0094(17) 0.0024(18) C307 0.097(5) 0.039(4) 0.056(3) -0.004(3) 0.002(3) -0.007(3) C308 0.105(5) 0.039(4) 0.054(3) -0.015(3) 0.005(3) -0.007(3) O309 0.093(3) 0.043(2) 0.0463(18) -0.0126(16) -0.0065(19) -0.007(2) C310 0.118(6) 0.043(4) 0.053(3) -0.006(3) -0.009(3) -0.039(4) C311 0.081(4) 0.069(5) 0.055(3) -0.022(3) 0.007(3) -0.043(4) O312 0.0474(18) 0.050(2) 0.0528(18) -0.0182(16) 0.0034(15) -0.0194(16) C313 0.042(3) 0.076(5) 0.087(4) -0.046(4) -0.003(3) -0.018(3) C314 0.040(2) 0.065(4) 0.061(3) -0.028(3) -0.020(2) 0.000(2) O315 0.0443(17) 0.046(2) 0.0448(16) -0.0090(15) -0.0111(13) -0.0145(15) Cu2 0.0367(3) 0.0335(4) 0.0374(3) -0.0016(3) -0.0078(2) -0.0035(3) N41 0.0355(18) 0.035(2) 0.0349(16) -0.0037(15) -0.0068(14) -0.0086(15) C42 0.041(2) 0.030(3) 0.0333(19) -0.0072(17) -0.0029(16) -0.0072(18) C43 0.039(2) 0.033(3) 0.0335(19) -0.0077(17) -0.0018(16) -0.0071(18) C44 0.043(2) 0.051(3) 0.033(2) -0.004(2) 0.0023(17) -0.005(2) C45 0.043(2) 0.045(3) 0.0267(17) 0.0007(17) -0.0033(16) -0.006(2) C46 0.039(2) 0.042(3) 0.036(2) -0.0063(19) -0.0070(17) -0.007(2) N51 0.0340(18) 0.032(2) 0.0367(17) -0.0023(15) -0.0073(14) -0.0059(15) C52 0.040(2) 0.037(3) 0.0339(19) -0.0051(18) -0.0065(17) -0.0017(19) S53 0.0497(6) 0.0475(8) 0.0344(5) -0.0011(5) -0.0104(4) -0.0018(5) C54 0.046(3) 0.045(3) 0.043(2) -0.007(2) -0.0159(19) 0.000(2) C55 0.039(2) 0.030(3) 0.040(2) -0.0039(18) -0.0110(17) -0.0010(18) N61 0.0385(19) 0.037(2) 0.0428(19) -0.0073(16) -0.0065(15) -0.0073(16) C62 0.038(2) 0.036(3) 0.048(2) -0.007(2) -0.0144(19) -0.0027(19) C63 0.043(3) 0.037(3) 0.053(3) -0.006(2) -0.008(2) -0.005(2) C64 0.039(2) 0.042(3) 0.071(3) -0.016(3) -0.009(2) 0.000(2) C65 0.046(3) 0.045(3) 0.059(3) -0.019(2) 0.000(2) -0.009(2) C66 0.050(3) 0.039(3) 0.043(2) -0.003(2) -0.004(2) -0.010(2) N101 0.0360(18) 0.037(2) 0.0317(16) -0.0053(15) -0.0058(13) -0.0013(16) C102 0.032(2) 0.038(3) 0.038(2) -0.0047(19) -0.0076(16) -0.0037(18) C103 0.035(2) 0.047(3) 0.035(2) -0.0114(19) -0.0070(16) -0.0032(19) C104 0.043(2) 0.057(4) 0.039(2) -0.014(2) -0.0089(18) -0.002(2) C105 0.041(2) 0.051(3) 0.0319(19) -0.0075(19) -0.0091(17) -0.001(2) C106 0.036(2) 0.040(3) 0.037(2) -0.0047(19) -0.0057(16) -0.0033(19) N111 0.0384(19) 0.033(2) 0.0431(19) 0.0001(17) -0.0079(15) -0.0038(16) C112 0.039(2) 0.043(3) 0.035(2) 0.0026(19) -0.0112(17) 0.000(2) S113 0.0445(6) 0.0447(8) 0.0398(5) 0.0021(5) -0.0027(4) -0.0048(5) C114 0.038(2) 0.041(3) 0.051(2) -0.001(2) -0.0040(19) -0.004(2) C115 0.035(2) 0.039(3) 0.050(2) -0.007(2) -0.0073(18) -0.0028(19) N121 0.0348(19) 0.042(3) 0.049(2) -0.0057(18) -0.0034(16) -0.0062(17) C122 0.034(2) 0.044(3) 0.052(2) -0.010(2) -0.0076(19) 0.000(2) C123 0.048(3) 0.040(3) 0.063(3) 0.002(2) -0.009(2) -0.010(2) C124 0.050(3) 0.043(4) 0.081(4) -0.016(3) -0.010(3) -0.013(2) C125 0.046(3) 0.064(4) 0.069(3) -0.026(3) -0.009(2) -0.007(3) C126 0.042(2) 0.050(3) 0.051(3) -0.016(2) 0.000(2) -0.008(2) Cl1 0.0440(5) 0.0421(7) 0.0372(5) -0.0031(4) -0.0071(4) -0.0087(5) O1A 0.060(2) 0.049(2) 0.0419(16) 0.0007(15) -0.0165(15) -0.0102(18) O1B 0.060(2) 0.066(3) 0.0475(19) -0.0118(18) -0.0054(16) -0.003(2) O1C 0.0477(19) 0.058(3) 0.0514(18) -0.0081(17) -0.0024(15) -0.0183(17) O1D 0.056(2) 0.043(2) 0.059(2) 0.0054(17) -0.0186(17) -0.0130(17) Cl2 0.0640(7) 0.0457(8) 0.0398(5) -0.0011(5) -0.0105(5) -0.0102(6) O2A 0.099(4) 0.067(4) 0.096(4) -0.025(3) 0.013(3) -0.039(3) O2B 0.093(4) 0.071(4) 0.076(3) 0.015(3) 0.016(3) 0.022(3) O2C 0.090(3) 0.073(3) 0.078(3) -0.020(2) -0.046(3) 0.000(3) O2D 0.065(2) 0.068(3) 0.0467(19) 0.0068(18) -0.0173(17) -0.004(2) Cl3 0.0448(6) 0.0522(8) 0.0445(5) -0.0130(5) -0.0079(4) -0.0133(5) O3A 0.074(3) 0.064(3) 0.0482(19) -0.0075(18) -0.0024(18) -0.024(2) O3B 0.0449(18) 0.060(3) 0.0563(19) -0.0208(17) -0.0122(15) -0.0081(17) O3C 0.048(2) 0.065(3) 0.063(2) -0.0185(19) -0.0200(17) -0.0090(18) O3D 0.053(2) 0.058(3) 0.0527(19) -0.0168(17) -0.0034(16) -0.0132(18) Cl5 0.0438(6) 0.0670(9) 0.0419(5) -0.0075(5) -0.0077(4) -0.0053(6) O5A 0.075(3) 0.067(3) 0.0470(19) -0.0124(18) -0.0162(18) -0.008(2) O5B 0.067(4) 0.403(18) 0.065(3) -0.004(6) 0.003(3) 0.050(6) O5C 0.088(3) 0.083(4) 0.050(2) 0.006(2) -0.016(2) -0.018(3) O5D 0.294(13) 0.072(5) 0.153(7) -0.001(4) -0.137(8) -0.060(6) Cl6 0.0653(8) 0.0608(9) 0.0392(5) -0.0075(5) -0.0054(5) -0.0298(6) O6A 0.111(5) 0.112(5) 0.096(4) 0.046(4) -0.050(3) -0.067(4) O6B 0.053(2) 0.161(6) 0.051(2) -0.029(3) 0.0004(18) -0.010(3) O6C 0.063(3) 0.111(5) 0.183(7) -0.099(5) -0.046(4) 0.022(3) O6D 0.084(3) 0.093(4) 0.092(3) -0.014(3) -0.038(3) -0.029(3) Cl8A 0.0591(13) 0.0504(16) 0.0450(11) -0.0069(10) 0.0066(10) -0.0219(11) O8A 0.062(4) 0.050(4) 0.041(3) -0.007(3) 0.007(3) -0.022(3) O8B 0.060(5) 0.085(8) 0.130(9) 0.018(7) -0.014(6) -0.019(5) O8C 0.174(7) 0.110(5) 0.066(3) -0.036(3) 0.027(4) -0.086(5) O8D 0.078(7) 0.070(8) 0.095(8) 0.008(6) -0.019(6) -0.026(5) Cl8B 0.0710(19) 0.070(2) 0.0479(14) -0.0158(14) -0.0005(13) -0.0203(16) O8E 0.092(7) 0.076(8) 0.054(5) -0.016(5) -0.005(5) -0.030(6) O8F 0.182(18) 0.114(14) 0.114(12) -0.002(10) -0.017(12) 0.098(14) O8G 0.174(7) 0.110(5) 0.066(3) -0.036(3) 0.027(4) -0.086(5) O8H 0.125(14) 0.109(13) 0.074(8) -0.057(9) 0.020(8) -0.055(11) O40A 0.066(5) 0.069(6) 0.051(4) 0.005(3) -0.019(3) -0.019(4) O40B 0.083(7) 0.071(7) 0.045(4) -0.013(4) 0.003(4) -0.029(6) O400 0.064(2) 0.053(3) 0.062(2) -0.0094(18) -0.0155(18) -0.0175(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N81 1.915(4) . ? Cu1 N21 1.933(4) . ? Cu1 N71 2.160(4) . ? Cu1 N11 2.172(5) . ? Cu1 N91 2.457(4) . ? N11 C12 1.334(8) . ? N11 C16 1.364(6) . ? C12 C13 1.391(8) . ? C13 C14 1.369(8) . ? C14 C15 1.376(9) . ? C15 C16 1.380(8) . ? C16 C22 1.458(9) . ? N21 C25 1.317(7) . ? N21 C22 1.375(7) . ? C22 C23 1.370(7) . ? C23 S24 1.706(7) . ? S24 C25 1.704(4) . ? C25 C32 1.454(7) . ? N31 C36 1.343(6) . ? N31 C32 1.358(5) . ? C32 C33 1.376(8) . ? C33 C34 1.381(8) . ? C34 C35 1.385(6) . ? C35 O200 1.368(6) . ? C35 C36 1.399(7) . ? C36 C42 1.504(5) . ? Ba1A O400 2.691(4) . ? Ba1A O212 2.783(4) . ? Ba1A O203 2.784(4) . ? Ba1A O5A 2.792(4) . ? Ba1A O209 2.809(3) . ? Ba1A O5C 2.810(5) 2_656 ? Ba1A O206 2.833(4) . ? Ba1A O1A 2.944(4) . ? Ba1A O215 3.047(4) . ? Ba1A O200 3.079(3) . ? Ba1B O5C 2.318(7) 2_656 ? Ba1B O5A 2.421(7) . ? Ba1B O206 2.691(7) . ? Ba1B O203 2.752(7) . ? Ba1B O209 2.900(6) . ? Ba1B O212 2.901(7) . ? Ba1B O215 3.132(6) . ? Ba1B O400 3.165(7) . ? Ba1B O200 3.265(6) . ? Ba1B Cl5 3.444(5) 2_656 ? Ba1B Cl5 3.602(6) . ? O200 C201 1.459(7) . ? C201 C202 1.485(8) . ? C202 O203 1.432(7) . ? O203 C204 1.418(7) . ? C204 C205 1.517(9) . ? C205 O206 1.407(8) . ? O206 C207 1.424(7) . ? C207 C208 1.467(9) . ? C208 O209 1.439(7) . ? O209 C210 1.437(7) . ? C210 C211 1.494(8) . ? C211 O212 1.441(6) . ? O212 C213 1.427(7) . ? C213 C214 1.495(7) . ? C214 O215 1.455(5) . ? O215 C43 1.355(5) . ? N71 C72 1.343(6) . ? N71 C76 1.351(6) . ? C72 C73 1.375(7) . ? C73 C74 1.374(8) . ? C74 C75 1.406(8) . ? C75 C76 1.383(7) . ? C76 C82 1.469(7) . ? N81 C85 1.308(6) . ? N81 C82 1.363(6) . ? C82 C83 1.365(6) . ? C83 S84 1.716(5) . ? S84 C85 1.711(4) . ? C85 C92 1.460(6) . ? N91 C96 1.338(6) . ? N91 C92 1.357(6) . ? C92 C93 1.387(6) . ? C93 C94 1.378(7) . ? C94 C95 1.382(6) . ? C95 O300 1.355(5) . ? C95 C96 1.420(6) . ? C96 C102 1.490(6) . ? Ba2A O312 2.669(4) . ? Ba2A O40A 2.725(7) . ? Ba2A O309 2.748(5) . ? Ba2A O303 2.763(4) . ? Ba2A O8A 2.818(6) . ? Ba2A O306 2.887(4) . ? Ba2A O315 3.027(4) . ? Ba2A O300 3.165(4) . ? Ba2B O6A 2.536(8) 2_567 ? Ba2B O6B 2.547(8) . ? Ba2B O40B 2.694(9) . ? Ba2B O303 2.712(4) . ? Ba2B O306 2.718(4) . ? Ba2B O312 2.859(4) . ? Ba2B O309 2.915(5) . ? Ba2B O315 3.134(4) . ? Ba2B O6C 3.173(9) 2_567 ? Ba2B O6C 3.242(9) . ? Ba2B C304 3.409(6) . ? Ba2B Cl6 3.4573(14) 2_567 ? O300 C301 1.456(5) . ? C301 C302 1.472(7) . ? C302 O303 1.428(7) . ? O303 C304 1.434(6) . ? C304 C305 1.510(11) . ? C305 O306 1.427(9) . ? O306 C307 1.425(9) . ? C307 C308 1.482(11) . ? C308 O309 1.438(8) . ? O309 C310 1.435(9) . ? C310 C311 1.469(11) . ? C311 O312 1.451(8) . ? O312 C313 1.430(7) . ? C313 C314 1.483(10) . ? C314 O315 1.465(6) . ? O315 C103 1.361(7) . ? Cu2 N51 1.918(4) . ? Cu2 N111 1.929(4) . ? Cu2 N61 2.150(4) . ? Cu2 N121 2.201(5) . ? N41 C42 1.321(6) . ? N41 C46 1.346(6) . ? C42 C43 1.407(6) . ? C43 C44 1.394(6) . ? C44 C45 1.371(7) . ? C45 C46 1.387(6) . ? C46 C52 1.457(6) . ? N51 C52 1.311(6) . ? N51 C55 1.373(6) . ? C52 S53 1.708(4) . ? S53 C54 1.709(5) . ? C54 C55 1.368(6) . ? C55 C62 1.458(7) . ? N61 C66 1.331(6) . ? N61 C62 1.361(6) . ? C62 C63 1.378(7) . ? C63 C64 1.378(8) . ? C64 C65 1.390(8) . ? C65 C66 1.390(7) . ? N101 C102 1.340(7) . ? N101 C106 1.360(6) . ? C102 C103 1.411(6) . ? C103 C104 1.381(7) . ? C104 C105 1.385(9) . ? C105 C106 1.395(7) . ? C106 C112 1.437(8) . ? N111 C112 1.323(7) . ? N111 C115 1.374(7) . ? C112 S113 1.716(5) . ? S113 C114 1.704(6) . ? C114 C115 1.352(7) . ? C115 C122 1.476(7) . ? N121 C126 1.336(7) . ? N121 C122 1.352(7) . ? C122 C123 1.381(8) . ? C123 C124 1.375(9) . ? C124 C125 1.393(10) . ? C125 C126 1.390(9) . ? Cl1 O1B 1.423(4) . ? Cl1 O1C 1.441(4) . ? Cl1 O1A 1.451(3) . ? Cl1 O1D 1.458(4) . ? Cl2 O2C 1.416(5) . ? Cl2 O2A 1.419(6) . ? Cl2 O2B 1.423(5) . ? Cl2 O2D 1.446(4) . ? Cl3 O3D 1.430(4) . ? Cl3 O3A 1.433(4) . ? Cl3 O3C 1.440(4) . ? Cl3 O3B 1.446(4) . ? Cl4A O4B 1.396(5) . ? Cl4A O4C 1.429(6) . ? Cl4A O4A 1.463(5) . ? Cl4A O4D 1.471(7) . ? Cl4B O4E 1.369(12) . ? Cl4B O4F 1.372(13) . ? Cl4B O4H 1.447(13) . ? Cl4B O4G 1.523(11) . ? Cl5 O5B 1.375(6) . ? Cl5 O5D 1.376(8) . ? Cl5 O5C 1.410(5) . ? Cl5 O5A 1.417(4) . ? Cl5 Ba1B 3.444(5) 2_656 ? O5C Ba1B 2.318(7) 2_656 ? O5C Ba1A 2.810(5) 2_656 ? Cl6 O6A 1.404(5) . ? Cl6 O6B 1.406(5) . ? Cl6 O6D 1.419(5) . ? Cl6 O6C 1.436(6) . ? Cl6 Ba2B 3.4573(14) 2_567 ? O6A Ba2B 2.536(8) 2_567 ? O6C Ba2B 3.173(9) 2_567 ? Cl8A O8B 1.398(9) . ? Cl8A O8A 1.442(6) . ? Cl8A O8D 1.452(10) . ? Cl8A O8C 1.487(5) . ? Cl8B O8F 1.391(11) . ? Cl8B O8E 1.418(9) . ? Cl8B O8H 1.447(10) . ? Cl9A O9D 1.410(10) . ? Cl9A O9C 1.416(10) . ? Cl9A O9B 1.443(10) . ? Cl9A O9A 1.455(11) . ? Cl9B O9F 1.402(10) . ? Cl9B O9H 1.419(8) . ? Cl9B O9E 1.423(9) . ? Cl9B O9G 1.455(9) . ? 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 N81 Cu1 N21 171.46(17) . . ? N81 Cu1 N71 78.54(16) . . ? N21 Cu1 N71 93.63(16) . . ? N81 Cu1 N11 98.99(17) . . ? N21 Cu1 N11 78.44(18) . . ? N71 Cu1 N11 97.25(16) . . ? N81 Cu1 N91 72.63(14) . . ? N21 Cu1 N91 115.36(14) . . ? N71 Cu1 N91 150.94(14) . . ? N11 Cu1 N91 90.88(15) . . ? C12 N11 C16 118.2(5) . . ? C12 N11 Cu1 129.2(3) . . ? C16 N11 Cu1 111.0(4) . . ? N11 C12 C13 122.0(5) . . ? C14 C13 C12 119.2(6) . . ? C13 C14 C15 119.6(6) . . ? C14 C15 C16 118.8(5) . . ? N11 C16 C15 122.1(6) . . ? N11 C16 C22 112.9(5) . . ? C15 C16 C22 124.9(5) . . ? C25 N21 C22 112.9(4) . . ? C25 N21 Cu1 128.2(4) . . ? C22 N21 Cu1 117.0(4) . . ? C23 C22 N21 113.1(5) . . ? C23 C22 C16 130.6(5) . . ? N21 C22 C16 116.4(4) . . ? C22 C23 S24 110.5(4) . . ? C25 S24 C23 90.6(3) . . ? N21 C25 C32 120.2(4) . . ? N21 C25 S24 112.9(4) . . ? C32 C25 S24 126.6(4) . . ? C36 N31 C32 116.9(4) . . ? N31 C32 C33 123.1(5) . . ? N31 C32 C25 112.9(4) . . ? C33 C32 C25 124.0(4) . . ? C32 C33 C34 119.8(4) . . ? C33 C34 C35 117.9(5) . . ? O200 C35 C34 123.8(5) . . ? O200 C35 C36 116.9(4) . . ? C34 C35 C36 119.3(5) . . ? N31 C36 C35 122.7(4) . . ? N31 C36 C42 113.0(4) . . ? C35 C36 C42 123.9(4) . . ? O400 Ba1A O212 114.39(12) . . ? O400 Ba1A O203 66.75(12) . . ? O212 Ba1A O203 174.40(11) . . ? O400 Ba1A O5A 129.98(14) . . ? O212 Ba1A O5A 110.30(13) . . ? O203 Ba1A O5A 71.01(13) . . ? O400 Ba1A O209 85.83(12) . . ? O212 Ba1A O209 59.59(11) . . ? O203 Ba1A O209 115.60(12) . . ? O5A Ba1A O209 137.61(11) . . ? O400 Ba1A O5C 140.00(15) . 2_656 ? O212 Ba1A O5C 77.55(14) . 2_656 ? O203 Ba1A O5C 98.08(15) . 2_656 ? O5A Ba1A O5C 70.50(14) . 2_656 ? O209 Ba1A O5C 67.12(13) . 2_656 ? O400 Ba1A O206 78.37(13) . . ? O212 Ba1A O206 116.21(11) . . ? O203 Ba1A O206 58.32(12) . . ? O5A Ba1A O206 101.22(13) . . ? O209 Ba1A O206 59.67(12) . . ? O5C Ba1A O206 62.81(14) 2_656 . ? O400 Ba1A O1A 61.61(12) . . ? O212 Ba1A O1A 65.42(10) . . ? O203 Ba1A O1A 118.75(11) . . ? O5A Ba1A O1A 123.29(12) . . ? O209 Ba1A O1A 91.51(11) . . ? O5C Ba1A O1A 142.93(14) 2_656 . ? O206 Ba1A O1A 132.66(11) . . ? O400 Ba1A O215 119.15(11) . . ? O212 Ba1A O215 59.17(9) . . ? O203 Ba1A O215 125.58(10) . . ? O5A Ba1A O215 67.76(12) . . ? O209 Ba1A O215 118.75(10) . . ? O5C Ba1A O215 99.99(13) 2_656 . ? O206 Ba1A O215 162.47(10) . . ? O1A Ba1A O215 62.98(9) . . ? O400 Ba1A O200 73.99(11) . . ? O212 Ba1A O200 126.85(10) . . ? O203 Ba1A O200 58.70(11) . . ? O5A Ba1A O200 61.62(11) . . ? O209 Ba1A O200 159.66(9) . . ? O5C Ba1A O200 131.19(13) 2_656 . ? O206 Ba1A O200 116.85(11) . . ? O1A Ba1A O200 76.92(10) . . ? O215 Ba1A O200 70.98(9) . . ? O5C Ba1B O5A 86.0(3) 2_656 . ? O5C Ba1B O206 71.5(2) 2_656 . ? O5A Ba1B O206 116.5(3) . . ? O5C Ba1B O203 112.6(3) 2_656 . ? O5A Ba1B O203 77.2(2) . . ? O206 Ba1B O203 60.38(17) . . ? O5C Ba1B O209 72.10(19) 2_656 . ? O5A Ba1B O209 157.9(3) . . ? O206 Ba1B O209 60.15(16) . . ? O203 Ba1B O209 113.7(2) . . ? O5C Ba1B O212 83.5(2) 2_656 . ? O5A Ba1B O212 118.3(2) . . ? O206 Ba1B O212 117.0(2) . . ? O203 Ba1B O212 159.3(3) . . ? O209 Ba1B O212 57.24(15) . . ? O5C Ba1B O215 110.0(2) 2_656 . ? O5A Ba1B O215 70.63(18) . . ? O206 Ba1B O215 172.9(3) . . ? O203 Ba1B O215 123.57(19) . . ? O209 Ba1B O215 113.3(2) . . ? O212 Ba1B O215 57.03(14) . . ? O5C Ba1B O400 140.5(2) 2_656 . ? O5A Ba1B O400 125.1(2) . . ? O206 Ba1B O400 72.70(16) . . ? O203 Ba1B O400 60.75(15) . . ? O209 Ba1B O400 76.14(16) . . ? O212 Ba1B O400 98.6(2) . . ? O215 Ba1B O400 103.7(2) . . ? O5C Ba1B O200 147.3(3) 2_656 . ? O5A Ba1B O200 62.02(15) . . ? O206 Ba1B O200 115.2(2) . . ? O203 Ba1B O200 56.54(14) . . ? O209 Ba1B O200 140.1(2) . . ? O212 Ba1B O200 116.4(2) . . ? O215 Ba1B O200 67.52(13) . . ? O400 Ba1B O200 65.63(14) . . ? O5C Ba1B Cl5 17.27(15) 2_656 2_656 ? O5A Ba1B Cl5 78.23(17) . 2_656 ? O206 Ba1B Cl5 88.72(17) . 2_656 ? O203 Ba1B Cl5 124.5(2) . 2_656 ? O209 Ba1B Cl5 79.82(13) . 2_656 ? O212 Ba1B Cl5 74.36(13) . 2_656 ? O215 Ba1B Cl5 92.82(14) . 2_656 ? O400 Ba1B Cl5 154.75(18) . 2_656 ? O200 Ba1B Cl5 139.40(18) . 2_656 ? O5C Ba1B Cl5 74.2(2) 2_656 . ? O5A Ba1B Cl5 15.24(13) . . ? O206 Ba1B Cl5 102.9(2) . . ? O203 Ba1B Cl5 73.99(16) . . ? O209 Ba1B Cl5 145.7(2) . . ? O212 Ba1B Cl5 124.68(17) . . ? O215 Ba1B Cl5 84.12(13) . . ? O400 Ba1B Cl5 130.30(18) . . ? O200 Ba1B Cl5 73.15(12) . . ? Cl5 Ba1B Cl5 69.64(11) 2_656 . ? C35 O200 C201 114.6(4) . . ? C35 O200 Ba1A 115.9(3) . . ? C201 O200 Ba1A 106.2(3) . . ? C35 O200 Ba1B 123.2(3) . . ? C201 O200 Ba1B 106.2(3) . . ? Ba1A O200 Ba1B 9.74(10) . . ? O200 C201 C202 109.4(4) . . ? O203 C202 C201 108.2(4) . . ? C204 O203 C202 114.2(5) . . ? C204 O203 Ba1B 107.6(3) . . ? C202 O203 Ba1B 121.6(3) . . ? C204 O203 Ba1A 116.1(3) . . ? C202 O203 Ba1A 120.4(3) . . ? Ba1B O203 Ba1A 11.79(12) . . ? O203 C204 C205 108.2(5) . . ? O206 C205 C204 108.4(5) . . ? C205 O206 C207 111.5(5) . . ? C205 O206 Ba1B 120.9(4) . . ? C207 O206 Ba1B 121.3(4) . . ? C205 O206 Ba1A 119.8(3) . . ? C207 O206 Ba1A 115.4(3) . . ? Ba1B O206 Ba1A 11.46(12) . . ? O206 C207 C208 110.4(5) . . ? O209 C208 C207 110.0(5) . . ? C210 O209 C208 111.9(4) . . ? C210 O209 Ba1A 117.5(3) . . ? C208 O209 Ba1A 116.5(3) . . ? C210 O209 Ba1B 116.5(3) . . ? C208 O209 Ba1B 108.8(3) . . ? Ba1A O209 Ba1B 11.30(11) . . ? O209 C210 C211 108.9(4) . . ? O212 C211 C210 107.2(4) . . ? C213 O212 C211 112.9(4) . . ? C213 O212 Ba1A 119.0(3) . . ? C211 O212 Ba1A 113.9(3) . . ? C213 O212 Ba1B 121.5(3) . . ? C211 O212 Ba1B 118.6(3) . . ? Ba1A O212 Ba1B 11.25(10) . . ? O212 C213 C214 107.4(4) . . ? O215 C214 C213 109.1(4) . . ? C43 O215 C214 115.7(3) . . ? C43 O215 Ba1A 118.6(3) . . ? C214 O215 Ba1A 106.5(3) . . ? C43 O215 Ba1B 112.7(3) . . ? C214 O215 Ba1B 103.5(3) . . ? Ba1A O215 Ba1B 10.46(10) . . ? C72 N71 C76 119.2(4) . . ? C72 N71 Cu1 127.8(3) . . ? C76 N71 Cu1 112.5(3) . . ? N71 C72 C73 122.3(5) . . ? C74 C73 C72 118.9(5) . . ? C73 C74 C75 119.9(5) . . ? C76 C75 C74 117.7(5) . . ? N71 C76 C75 122.0(5) . . ? N71 C76 C82 113.5(4) . . ? C75 C76 C82 124.5(4) . . ? C85 N81 C82 113.5(4) . . ? C85 N81 Cu1 126.4(3) . . ? C82 N81 Cu1 119.6(3) . . ? N81 C82 C83 113.1(4) . . ? N81 C82 C76 115.1(4) . . ? C83 C82 C76 131.8(5) . . ? C82 C83 S84 110.5(4) . . ? C85 S84 C83 89.9(2) . . ? N81 C85 C92 118.9(4) . . ? N81 C85 S84 112.9(4) . . ? C92 C85 S84 128.2(3) . . ? C96 N91 C92 117.6(4) . . ? C96 N91 Cu1 133.2(3) . . ? C92 N91 Cu1 108.6(3) . . ? N91 C92 C93 123.3(4) . . ? N91 C92 C85 113.1(4) . . ? C93 C92 C85 123.6(4) . . ? C94 C93 C92 118.9(4) . . ? C93 C94 C95 119.3(4) . . ? O300 C95 C94 124.9(4) . . ? O300 C95 C96 116.5(4) . . ? C94 C95 C96 118.6(4) . . ? N91 C96 C95 122.2(4) . . ? N91 C96 C102 114.5(4) . . ? C95 C96 C102 123.2(4) . . ? O312 Ba2A O40A 112.1(2) . . ? O312 Ba2A O309 61.85(13) . . ? O40A Ba2A O309 73.2(2) . . ? O312 Ba2A O303 175.37(11) . . ? O40A Ba2A O303 69.4(2) . . ? O309 Ba2A O303 115.29(14) . . ? O312 Ba2A O8A 71.28(17) . . ? O40A Ba2A O8A 67.4(2) . . ? O309 Ba2A O8A 97.74(18) . . ? O303 Ba2A O8A 113.14(17) . . ? O312 Ba2A O306 116.99(13) . . ? O40A Ba2A O306 69.2(2) . . ? O309 Ba2A O306 59.04(14) . . ? O303 Ba2A O306 59.06(13) . . ? O8A Ba2A O306 135.27(16) . . ? O312 Ba2A O315 60.64(11) . . ? O40A Ba2A O315 129.8(2) . . ? O309 Ba2A O315 122.49(12) . . ? O303 Ba2A O315 122.12(11) . . ? O8A Ba2A O315 63.45(16) . . ? O306 Ba2A O315 160.96(10) . . ? O312 Ba2A O300 125.59(10) . . ? O40A Ba2A O300 86.2(2) . . ? O309 Ba2A O300 159.01(10) . . ? O303 Ba2A O300 58.46(10) . . ? O8A Ba2A O300 70.07(16) . . ? O306 Ba2A O300 117.41(11) . . ? O315 Ba2A O300 68.38(9) . . ? O6A Ba2B O6B 98.72(17) 2_567 . ? O6A Ba2B O40B 140.7(3) 2_567 . ? O6B Ba2B O40B 120.6(3) . . ? O6A Ba2B O303 123.45(17) 2_567 . ? O6B Ba2B O303 74.17(15) . . ? O40B Ba2B O303 70.7(3) . . ? O6A Ba2B O306 73.79(17) 2_567 . ? O6B Ba2B O306 116.55(16) . . ? O40B Ba2B O306 86.0(3) . . ? O303 Ba2B O306 61.76(13) . . ? O6A Ba2B O312 76.42(16) 2_567 . ? O6B Ba2B O312 122.73(14) . . ? O40B Ba2B O312 83.3(2) . . ? O303 Ba2B O312 153.99(12) . . ? O306 Ba2B O312 116.33(13) . . ? O6A Ba2B O309 66.49(15) 2_567 . ? O6B Ba2B O309 165.08(13) . . ? O40B Ba2B O309 74.2(2) . . ? O303 Ba2B O309 111.63(13) . . ? O306 Ba2B O309 59.00(14) . . ? O312 Ba2B O309 57.67(13) . . ? O6A Ba2B O315 109.58(16) 2_567 . ? O6B Ba2B O315 72.09(13) . . ? O40B Ba2B O315 86.2(3) . . ? O303 Ba2B O315 120.07(11) . . ? O306 Ba2B O315 170.60(12) . . ? O312 Ba2B O315 57.49(10) . . ? O309 Ba2B O315 113.67(12) . . ? O6A Ba2B O6C 45.06(17) 2_567 2_567 ? O6B Ba2B O6C 65.91(16) . 2_567 ? O40B Ba2B O6C 153.0(3) . 2_567 ? O303 Ba2B O6C 132.72(15) . 2_567 ? O306 Ba2B O6C 115.60(13) . 2_567 ? O312 Ba2B O6C 72.82(14) . 2_567 ? O309 Ba2B O6C 102.22(14) . 2_567 ? O315 Ba2B O6C 70.59(11) . 2_567 ? O6A Ba2B O6C 63.42(17) 2_567 . ? O6B Ba2B O6C 44.29(15) . . ? O40B Ba2B O6C 146.6(3) . . ? O303 Ba2B O6C 76.04(14) . . ? O306 Ba2B O6C 80.80(15) . . ? O312 Ba2B O6C 129.96(13) . . ? O309 Ba2B O6C 122.31(13) . . ? O315 Ba2B O6C 108.59(13) . . ? O6C Ba2B O6C 57.91(17) 2_567 . ? O6A Ba2B C304 99.76(18) 2_567 . ? O6B Ba2B C304 77.59(16) . . ? O40B Ba2B C304 87.7(3) . . ? O303 Ba2B C304 23.77(13) . . ? O306 Ba2B C304 44.43(16) . . ? O312 Ba2B C304 159.56(14) . . ? O309 Ba2B C304 102.20(15) . . ? O315 Ba2B C304 140.27(14) . . ? O6C Ba2B C304 118.87(15) 2_567 . ? O6C Ba2B C304 61.57(15) . . ? O6A Ba2B Cl6 20.62(15) 2_567 2_567 ? O6B Ba2B Cl6 84.48(11) . 2_567 ? O40B Ba2B Cl6 152.2(2) . 2_567 ? O303 Ba2B Cl6 132.72(9) . 2_567 ? O306 Ba2B Cl6 93.46(9) . 2_567 ? O312 Ba2B Cl6 72.00(7) . 2_567 ? O309 Ba2B Cl6 81.71(8) . 2_567 ? O315 Ba2B Cl6 91.06(7) . 2_567 ? O6C Ba2B Cl6 24.54(10) 2_567 2_567 ? O6C Ba2B Cl6 59.77(11) . 2_567 ? C304 Ba2B Cl6 111.15(10) . 2_567 ? C95 O300 C301 116.0(3) . . ? C95 O300 Ba2A 112.0(3) . . ? C301 O300 Ba2A 100.4(3) . . ? O300 C301 C302 109.1(4) . . ? O303 C302 C301 107.6(5) . . ? C302 O303 C304 114.7(5) . . ? C302 O303 Ba2B 123.2(3) . . ? C304 O303 Ba2B 106.5(3) . . ? C302 O303 Ba2A 121.3(3) . . ? C304 O303 Ba2A 117.1(4) . . ? Ba2B O303 Ba2A 15.00(2) . . ? O303 C304 C305 107.0(5) . . ? O303 C304 Ba2B 49.7(3) . . ? C305 C304 Ba2B 84.5(4) . . ? O306 C305 C304 109.8(5) . . ? C307 O306 C305 110.8(5) . . ? C307 O306 Ba2B 122.4(4) . . ? C305 O306 Ba2B 116.8(4) . . ? C307 O306 Ba2A 113.3(4) . . ? C305 O306 Ba2A 115.7(3) . . ? Ba2B O306 Ba2A 14.28(3) . . ? O306 C307 C308 109.3(5) . . ? O309 C308 C307 109.2(5) . . ? C310 O309 C308 112.0(5) . . ? C310 O309 Ba2A 115.5(4) . . ? C308 O309 Ba2A 120.6(4) . . ? C310 O309 Ba2B 114.6(3) . . ? C308 O309 Ba2B 111.0(4) . . ? Ba2A O309 Ba2B 14.15(3) . . ? O309 C310 C311 109.3(5) . . ? O312 C311 C310 108.3(5) . . ? C313 O312 C311 113.1(5) . . ? C313 O312 Ba2A 118.8(3) . . ? C311 O312 Ba2A 112.8(4) . . ? C313 O312 Ba2B 121.5(3) . . ? C311 O312 Ba2B 119.2(4) . . ? Ba2A O312 Ba2B 14.37(2) . . ? O312 C313 C314 107.6(5) . . ? O315 C314 C313 108.4(5) . . ? C103 O315 C314 115.8(4) . . ? C103 O315 Ba2A 122.2(3) . . ? C314 O315 Ba2A 104.3(3) . . ? C103 O315 Ba2B 114.1(3) . . ? C314 O315 Ba2B 101.3(3) . . ? Ba2A O315 Ba2B 13.21(2) . . ? N51 Cu2 N111 172.91(17) . . ? N51 Cu2 N61 79.34(15) . . ? N111 Cu2 N61 94.94(16) . . ? N51 Cu2 N121 99.03(17) . . ? N111 Cu2 N121 77.52(18) . . ? N61 Cu2 N121 98.36(16) . . ? C42 N41 C46 118.9(4) . . ? N41 C42 C43 122.2(4) . . ? N41 C42 C36 114.0(4) . . ? C43 C42 C36 123.7(4) . . ? O215 C43 C44 124.3(4) . . ? O215 C43 C42 117.4(4) . . ? C44 C43 C42 118.3(4) . . ? C45 C44 C43 119.2(4) . . ? C44 C45 C46 118.9(4) . . ? N41 C46 C45 122.5(4) . . ? N41 C46 C52 113.4(4) . . ? C45 C46 C52 124.1(4) . . ? C52 N51 C55 113.7(4) . . ? C52 N51 Cu2 127.5(3) . . ? C55 N51 Cu2 118.2(3) . . ? N51 C52 C46 119.9(4) . . ? N51 C52 S53 112.5(3) . . ? C46 C52 S53 127.6(3) . . ? C52 S53 C54 90.5(2) . . ? C55 C54 S53 110.6(4) . . ? C54 C55 N51 112.6(4) . . ? C54 C55 C62 131.3(4) . . ? N51 C55 C62 116.1(4) . . ? C66 N61 C62 117.6(4) . . ? C66 N61 Cu2 129.6(3) . . ? C62 N61 Cu2 112.3(3) . . ? N61 C62 C63 123.0(5) . . ? N61 C62 C55 113.4(4) . . ? C63 C62 C55 123.6(4) . . ? C62 C63 C64 118.3(5) . . ? C63 C64 C65 119.8(5) . . ? C64 C65 C66 118.1(5) . . ? N61 C66 C65 123.1(5) . . ? C102 N101 C106 118.1(4) . . ? N101 C102 C103 122.1(4) . . ? N101 C102 C96 115.3(4) . . ? C103 C102 C96 122.5(5) . . ? O315 C103 C104 123.4(5) . . ? O315 C103 C102 117.2(4) . . ? C104 C103 C102 119.4(5) . . ? C103 C104 C105 118.6(5) . . ? C104 C105 C106 119.4(4) . . ? N101 C106 C105 122.3(5) . . ? N101 C106 C112 113.8(4) . . ? C105 C106 C112 123.9(4) . . ? C112 N111 C115 113.7(4) . . ? C112 N111 Cu2 125.3(4) . . ? C115 N111 Cu2 120.0(3) . . ? N111 C112 C106 119.8(4) . . ? N111 C112 S113 111.8(4) . . ? C106 C112 S113 128.4(4) . . ? C114 S113 C112 90.4(3) . . ? C115 C114 S113 111.5(4) . . ? C114 C115 N111 112.6(5) . . ? C114 C115 C122 132.6(5) . . ? N111 C115 C122 114.8(4) . . ? C126 N121 C122 118.8(5) . . ? C126 N121 Cu2 128.1(4) . . ? C122 N121 Cu2 112.0(4) . . ? N121 C122 C123 122.5(5) . . ? N121 C122 C115 113.6(5) . . ? C123 C122 C115 123.9(5) . . ? C124 C123 C122 118.5(5) . . ? C123 C124 C125 119.6(6) . . ? C126 C125 C124 118.5(6) . . ? N121 C126 C125 122.0(5) . . ? O1B Cl1 O1C 110.9(3) . . ? O1B Cl1 O1A 109.3(2) . . ? O1C Cl1 O1A 109.7(2) . . ? O1B Cl1 O1D 109.8(3) . . ? O1C Cl1 O1D 108.9(2) . . ? O1A Cl1 O1D 108.3(2) . . ? Cl1 O1A Ba1A 149.0(2) . . ? O2C Cl2 O2A 108.4(4) . . ? O2C Cl2 O2B 112.4(4) . . ? O2A Cl2 O2B 107.6(4) . . ? O2C Cl2 O2D 108.1(3) . . ? O2A Cl2 O2D 111.2(4) . . ? O2B Cl2 O2D 109.2(3) . . ? O3D Cl3 O3A 110.2(3) . . ? O3D Cl3 O3C 110.5(2) . . ? O3A Cl3 O3C 110.2(3) . . ? O3D Cl3 O3B 108.0(2) . . ? O3A Cl3 O3B 109.1(3) . . ? O3C Cl3 O3B 108.8(3) . . ? O4B Cl4A O4C 114.1(4) . . ? O4B Cl4A O4A 109.4(4) . . ? O4C Cl4A O4A 107.3(4) . . ? O4B Cl4A O4D 112.7(4) . . ? O4C Cl4A O4D 108.2(4) . . ? O4A Cl4A O4D 104.5(4) . . ? O4E Cl4B O4F 121.5(14) . . ? O4E Cl4B O4H 104.7(12) . . ? O4F Cl4B O4H 114.4(14) . . ? O4E Cl4B O4G 108.6(11) . . ? O4F Cl4B O4G 102.9(12) . . ? O4H Cl4B O4G 103.1(12) . . ? O5B Cl5 O5D 113.2(9) . . ? O5B Cl5 O5C 108.7(5) . . ? O5D Cl5 O5C 106.0(5) . . ? O5B Cl5 O5A 109.6(5) . . ? O5D Cl5 O5A 107.8(4) . . ? O5C Cl5 O5A 111.5(3) . . ? O5B Cl5 Ba1B 121.0(3) . 2_656 ? O5D Cl5 Ba1B 76.8(4) . 2_656 ? O5C Cl5 Ba1B 29.2(3) . 2_656 ? O5A Cl5 Ba1B 122.4(2) . 2_656 ? O5B Cl5 Ba1B 128.3(3) . . ? O5D Cl5 Ba1B 82.0(4) . . ? O5C Cl5 Ba1B 113.7(2) . . ? O5A Cl5 Ba1B 26.7(2) . . ? Ba1B Cl5 Ba1B 110.36(11) 2_656 . ? Cl5 O5A Ba1B 138.1(3) . . ? Cl5 O5A Ba1A 146.3(3) . . ? Ba1B O5A Ba1A 9.52(13) . . ? Cl5 O5C Ba1B 133.5(4) . 2_656 ? Cl5 O5C Ba1A 134.4(4) . 2_656 ? Ba1B O5C Ba1A 6.43(15) 2_656 2_656 ? O6A Cl6 O6B 110.3(4) . . ? O6A Cl6 O6D 114.6(4) . . ? O6B Cl6 O6D 113.3(3) . . ? O6A Cl6 O6C 105.8(5) . . ? O6B Cl6 O6C 106.3(5) . . ? O6D Cl6 O6C 105.8(4) . . ? O6A Cl6 Ba2B 39.5(4) . 2_567 ? O6B Cl6 Ba2B 125.5(2) . 2_567 ? O6D Cl6 Ba2B 120.7(3) . 2_567 ? O6C Cl6 Ba2B 66.6(3) . 2_567 ? O6A Cl6 Ba2B 120.8(3) . . ? O6B Cl6 Ba2B 38.4(3) . . ? O6D Cl6 Ba2B 123.9(3) . . ? O6C Cl6 Ba2B 68.0(3) . . ? Ba2B Cl6 Ba2B 107.68(4) 2_567 . ? Cl6 O6A Ba2B 119.9(5) . 2_567 ? Cl6 O6B Ba2B 121.6(4) . . ? Cl6 O6C Ba2B 88.9(4) . 2_567 ? Cl6 O6C Ba2B 87.8(3) . . ? Ba2B O6C Ba2B 122.09(17) 2_567 . ? O8B Cl8A O8A 108.5(6) . . ? O8B Cl8A O8D 108.7(7) . . ? O8A Cl8A O8D 108.9(6) . . ? O8B Cl8A O8C 116.3(7) . . ? O8A Cl8A O8C 111.2(4) . . ? O8D Cl8A O8C 102.8(6) . . ? Cl8A O8A Ba2A 141.2(4) . . ? O8F Cl8B O8E 111.5(10) . . ? O8F Cl8B O8H 109.8(10) . . ? O8E Cl8B O8H 105.1(9) . . ? O9D Cl9A O9C 112.8(8) . . ? O9D Cl9A O9B 108.7(8) . . ? O9C Cl9A O9B 109.7(8) . . ? O9D Cl9A O9A 105.7(8) . . ? O9C Cl9A O9A 112.8(8) . . ? O9B Cl9A O9A 106.8(8) . . ? O9F Cl9B O9H 116.4(7) . . ? O9F Cl9B O9E 110.6(7) . . ? O9H Cl9B O9E 109.1(6) . . ? O9F Cl9B O9G 106.1(8) . . ? O9H Cl9B O9G 107.1(6) . . ? O9E Cl9B O9G 107.2(6) . . ? Ba1A O400 Ba1B 6.18(12) . . ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 70.21 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 1.603 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.116 data_holidaym _database_code_depnum_ccdc_archive 'CCDC 270154' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H83 Cl6 Cu2 Li2 N17 O36 S4' _chemical_formula_weight 2364.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 '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)/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 18.9494(16) _cell_length_b 25.4504(18) _cell_length_c 22.770(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.518(5) _cell_angle_gamma 90.00 _cell_volume 10144.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(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 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4848 _exptl_absorpt_coefficient_mu 3.532 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.579351 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The complex cation features two Cu(II) coordination domains incorporated into a metallo-helical array with 18-crown-6 macrocycles spanning the central bipy rings on each side of the molecule. Li+ cations occupy both of the crown ether host cavities, each being stabilised by up to four Li-O interactions (with the crown ethers) and coordinating acetonitrile and perchlorate ligands. The Cu(II) coordination domains and four of the six expected anions are well resolved. However, both crown ethers, the Li+ cations, and the Li-bound perchlorate ClO4(6), presented significant refinement problems owing to extensive disorder. Accordingly, the disordered crown ethers were (tentatively) resolved into two components, each component being refined with geometric similarity restraints (SADI), ADP restraints (SIMU) and a number of atoms with isotropic displacement paramters [C(30a), C(30b) and all atoms from C(20a)/C(20b) to C(24a)/C(24b)]. The Li-bound perchlorate, ClO4(6), and non-coordinated, ClO4(5), were also disordere ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65632 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 70.25 _reflns_number_total 18563 _reflns_number_gt 15741 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHEXTL' _computing_publication_material 'Bruker SHEXTL' _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^)+(0.1214P)^2^+13.9840P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18563 _refine_ls_number_parameters 1314 _refine_ls_number_restraints 182 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.2307 _refine_ls_wR_factor_gt 0.2228 _refine_ls_goodness_of_fit_ref 1.221 _refine_ls_restrained_S_all 1.261 _refine_ls_shift/su_max 0.047 _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 0.29710(3) 0.94418(2) 0.35835(3) 0.02874(16) Uani 1 1 d . . . Cu2 Cu 0.17772(4) 0.83941(2) 0.15681(3) 0.03624(18) Uani 1 1 d . . . Li1 Li -0.1107(10) 0.8095(8) 0.3469(8) 0.118(7) Uani 1 1 d . . . Li2 Li 0.5794(8) 1.0420(6) 0.1396(7) 0.089(4) Uani 1 1 d . . . N11 N 0.40022(19) 0.98948(14) 0.38662(17) 0.0334(7) Uani 1 1 d . . . C12 C 0.4642(2) 0.96163(18) 0.4179(2) 0.0375(9) Uani 1 1 d . . . C13 C 0.5362(3) 0.9845(2) 0.4401(2) 0.0467(11) Uani 1 1 d . . . H105 H 0.5806 0.9642 0.4620 0.056 Uiso 1 1 calc R . . C14 C 0.5418(3) 1.0374(2) 0.4296(3) 0.0525(13) Uani 1 1 d . . . H104 H 0.5904 1.0540 0.4442 0.063 Uiso 1 1 calc R . . C15 C 0.4765(3) 1.0663(2) 0.3980(3) 0.0504(12) Uani 1 1 d . . . H103 H 0.4796 1.1028 0.3905 0.060 Uiso 1 1 calc R . . C16 C 0.4064(3) 1.04092(18) 0.3774(2) 0.0403(10) Uani 1 1 d . . . H102 H 0.3612 1.0607 0.3561 0.048 Uiso 1 1 calc R . . N21 N 0.3746(2) 0.89168(14) 0.39886(17) 0.0329(7) Uani 1 1 d . . . C22 C 0.3633(2) 0.84152(16) 0.4064(2) 0.0341(9) Uani 1 1 d . . . S23 S 0.44653(7) 0.80888(5) 0.44850(6) 0.0488(3) Uani 1 1 d . . . C24 C 0.4970(3) 0.8656(2) 0.4549(2) 0.0475(11) Uani 1 1 d . . . H108 H 0.5509 0.8686 0.4760 0.057 Uiso 1 1 calc R . . C25 C 0.4497(2) 0.90570(18) 0.4257(2) 0.0380(9) Uani 1 1 d . . . N31 N 0.2353(2) 0.85706(13) 0.34223(16) 0.0306(7) Uani 1 1 d . . . C32 C 0.1626(2) 0.84366(15) 0.3151(2) 0.0327(9) Uani 1 1 d . . . C33 C 0.1353(3) 0.79361(16) 0.3226(2) 0.0360(9) Uani 1 1 d . . . C34 C 0.1874(3) 0.75666(16) 0.3604(2) 0.0387(10) Uani 1 1 d . . . H114 H 0.1710 0.7226 0.3667 0.046 Uiso 1 1 calc R . . C35 C 0.2633(3) 0.77091(16) 0.3882(2) 0.0362(9) Uani 1 1 d . . . H113 H 0.3002 0.7465 0.4137 0.043 Uiso 1 1 calc R . . C36 C 0.2854(2) 0.82093(16) 0.37883(19) 0.0326(8) Uani 1 1 d . . . N41 N 0.1213(2) 0.89398(13) 0.22005(17) 0.0333(8) Uani 1 1 d . . . C42 C 0.1102(2) 0.88354(15) 0.2724(2) 0.0344(9) Uani 1 1 d . . . C43 C 0.0545(3) 0.90950(17) 0.2885(2) 0.0396(10) Uani 1 1 d . . . C44 C 0.0101(3) 0.94811(17) 0.2469(2) 0.0431(11) Uani 1 1 d . . . H135 H -0.0277 0.9666 0.2564 0.052 Uiso 1 1 calc R . . C45 C 0.0219(3) 0.95890(17) 0.1922(2) 0.0401(10) Uani 1 1 d . . . H136 H -0.0081 0.9846 0.1632 0.048 Uiso 1 1 calc R . . C46 C 0.0782(2) 0.93176(15) 0.1800(2) 0.0355(9) Uani 1 1 d . . . N51 N 0.1401(2) 0.90438(14) 0.11220(17) 0.0378(8) Uani 1 1 d . . . C52 C 0.0967(3) 0.93854(17) 0.1248(2) 0.0386(10) Uani 1 1 d . . . S53 S 0.06970(7) 0.98876(4) 0.06978(6) 0.0430(3) Uani 1 1 d . . . C54 C 0.1187(3) 0.96044(19) 0.0287(2) 0.0453(11) Uani 1 1 d . . . H142 H 0.1210 0.9740 -0.0094 0.054 Uiso 1 1 calc R . . C55 C 0.1540(3) 0.91580(18) 0.0583(2) 0.0409(10) Uani 1 1 d . . . N61 N 0.2299(2) 0.83931(14) 0.08762(18) 0.0412(9) Uani 1 1 d . . . C62 C 0.2054(3) 0.87916(18) 0.0449(2) 0.0414(10) Uani 1 1 d . . . C63 C 0.2296(3) 0.8841(2) -0.0054(2) 0.0492(12) Uani 1 1 d . . . H146 H 0.2107 0.9118 -0.0354 0.059 Uiso 1 1 calc R . . C64 C 0.2807(4) 0.8487(2) -0.0112(3) 0.0564(13) Uani 1 1 d . . . H147 H 0.2976 0.8515 -0.0453 0.068 Uiso 1 1 calc R . . C65 C 0.3076(4) 0.8090(2) 0.0328(3) 0.0546(13) Uani 1 1 d . . . H148 H 0.3442 0.7846 0.0302 0.066 Uiso 1 1 calc R . . C66 C 0.2803(3) 0.80523(19) 0.0811(2) 0.0470(11) Uani 1 1 d . . . H149 H 0.2982 0.7773 0.1109 0.056 Uiso 1 1 calc R . . N71 N 0.24160(19) 0.95377(13) 0.42519(16) 0.0298(7) Uani 1 1 d . . . C72 C 0.1905(2) 0.99338(16) 0.4105(2) 0.0325(8) Uani 1 1 d . . . C73 C 0.1517(3) 1.00767(18) 0.4484(2) 0.0410(10) Uani 1 1 d . . . H246 H 0.1162 1.0359 0.4366 0.049 Uiso 1 1 calc R . . C74 C 0.1656(3) 0.98003(19) 0.5038(2) 0.0453(11) Uani 1 1 d . . . H247 H 0.1407 0.9895 0.5314 0.054 Uiso 1 1 calc R . . C75 C 0.2161(3) 0.93850(19) 0.5186(2) 0.0430(10) Uani 1 1 d . . . H248 H 0.2248 0.9181 0.5557 0.052 Uiso 1 1 calc R . . C76 C 0.2540(3) 0.92682(17) 0.4787(2) 0.0353(9) Uani 1 1 d . . . H249 H 0.2899 0.8988 0.4898 0.042 Uiso 1 1 calc R . . N81 N 0.22322(18) 0.99921(13) 0.31896(16) 0.0291(7) Uani 1 1 d . . . C82 C 0.2108(2) 1.02235(15) 0.26454(19) 0.0294(8) Uani 1 1 d . . . S83 S 0.14123(6) 1.06957(4) 0.24626(5) 0.0362(2) Uani 1 1 d . . . C84 C 0.1292(3) 1.05667(16) 0.3159(2) 0.0377(10) Uani 1 1 d . . . H242 H 0.0934 1.0738 0.3293 0.045 Uiso 1 1 calc R . . C85 C 0.1782(2) 1.01864(15) 0.3489(2) 0.0319(8) Uani 1 1 d . . . N91 N 0.29012(18) 0.95908(12) 0.24679(15) 0.0280(7) Uani 1 1 d . . . C92 C 0.3306(2) 0.93910(15) 0.21586(19) 0.0298(8) Uani 1 1 d . . . C93 C 0.3378(2) 0.96528(18) 0.1636(2) 0.0355(9) Uani 1 1 d . . . C94 C 0.2983(2) 1.01129(17) 0.1421(2) 0.0370(9) Uani 1 1 d . . . H235 H 0.3009 1.0288 0.1062 0.044 Uiso 1 1 calc R . . C95 C 0.2548(2) 1.03172(17) 0.1735(2) 0.0342(9) Uani 1 1 d . . . H236 H 0.2268 1.0634 0.1594 0.041 Uiso 1 1 calc R . . C96 C 0.2528(2) 1.00488(15) 0.22601(19) 0.0296(8) Uani 1 1 d . . . N101 N 0.3141(2) 0.84751(13) 0.22989(16) 0.0313(7) Uani 1 1 d . . . C102 C 0.3637(2) 0.88618(16) 0.23870(19) 0.0320(8) Uani 1 1 d . . . C103 C 0.4426(3) 0.87930(17) 0.2709(2) 0.0365(9) Uani 1 1 d . . . C104 C 0.4701(3) 0.82911(19) 0.2932(2) 0.0438(10) Uani 1 1 d . . . H214 H 0.5233 0.8230 0.3149 0.053 Uiso 1 1 calc R . . C105 C 0.4181(3) 0.78874(17) 0.2827(2) 0.0418(10) Uani 1 1 d . . . H213 H 0.4352 0.7542 0.2970 0.050 Uiso 1 1 calc R . . C106 C 0.3408(3) 0.79875(16) 0.2513(2) 0.0348(9) Uani 1 1 d . . . N111 N 0.2105(2) 0.77278(13) 0.19930(17) 0.0358(8) Uani 1 1 d . . . C112 C 0.2802(3) 0.75990(16) 0.2364(2) 0.0369(9) Uani 1 1 d . . . S113 S 0.28586(7) 0.69582(4) 0.26205(6) 0.0445(3) Uani 1 1 d . . . C114 C 0.1894(3) 0.68818(17) 0.2207(2) 0.0451(11) Uani 1 1 d . . . H208 H 0.1617 0.6569 0.2197 0.054 Uiso 1 1 calc R . . C115 C 0.1585(3) 0.73311(16) 0.1897(2) 0.0395(10) Uani 1 1 d . . . N121 N 0.0708(2) 0.79777(15) 0.12974(19) 0.0416(9) Uani 1 1 d . . . C122 C 0.0796(3) 0.74709(17) 0.1498(2) 0.0433(10) Uani 1 1 d . . . C123 C 0.0185(3) 0.7129(2) 0.1333(3) 0.0548(13) Uani 1 1 d . . . H205 H 0.0255 0.6773 0.1469 0.066 Uiso 1 1 calc R . . C124 C -0.0534(3) 0.7319(2) 0.0962(3) 0.0637(15) Uani 1 1 d . . . H204 H -0.0963 0.7091 0.0839 0.076 Uiso 1 1 calc R . . C125 C -0.0631(3) 0.7829(2) 0.0772(3) 0.0589(14) Uani 1 1 d . . . H203 H -0.1125 0.7961 0.0525 0.071 Uiso 1 1 calc R . . C126 C 0.0008(3) 0.8155(2) 0.0946(2) 0.0493(12) Uani 1 1 d . . . H202 H -0.0055 0.8511 0.0811 0.059 Uiso 1 1 calc R . . O200 O 0.06029(19) 0.78658(12) 0.28947(18) 0.0492(8) Uani 1 1 d D . . C201 C 0.0246(3) 0.74042(19) 0.3025(3) 0.0497(12) Uani 1 1 d D . . H11A H 0.0269 0.7412 0.3467 0.060 Uiso 1 1 calc R . . H11B H 0.0505 0.7082 0.2967 0.060 Uiso 1 1 calc R . . C202 C -0.0566(3) 0.7417(2) 0.2560(3) 0.0622(15) Uani 1 1 d D . . H12A H -0.0576 0.7409 0.2123 0.075 Uiso 1 1 calc R A . H12B H -0.0834 0.7099 0.2619 0.075 Uiso 1 1 calc R . . O203 O -0.0956(3) 0.7864(2) 0.2632(2) 0.0817(14) Uani 1 1 d D A . C20A C -0.1291(9) 0.8224(6) 0.2141(7) 0.083(4) Uiso 0.50 1 d PDU A 1 H12C H -0.1344 0.8072 0.1726 0.100 Uiso 0.50 1 calc PR A 1 H12D H -0.0985 0.8550 0.2214 0.100 Uiso 0.50 1 calc PR A 1 C21A C -0.2073(10) 0.8332(9) 0.2163(8) 0.109(6) Uiso 0.50 1 d PDU A 1 H12E H -0.2361 0.8003 0.2142 0.131 Uiso 0.50 1 calc PR A 1 H12F H -0.2382 0.8571 0.1817 0.131 Uiso 0.50 1 calc PR A 1 O22A O -0.1828(5) 0.8597(4) 0.2824(4) 0.073(2) Uiso 0.50 1 d PDU A 1 C23A C -0.2555(7) 0.8536(7) 0.2924(7) 0.076(4) Uiso 0.50 1 d PDU A 1 H12G H -0.2717 0.8164 0.2893 0.091 Uiso 0.50 1 calc PR A 1 H12H H -0.2971 0.8749 0.2619 0.091 Uiso 0.50 1 calc PR A 1 C24A C -0.2312(10) 0.8747(6) 0.3610(6) 0.088(4) Uiso 0.50 1 d PDU A 1 H12I H -0.2040 0.9087 0.3664 0.105 Uiso 0.50 1 calc PR A 1 H12J H -0.2754 0.8786 0.3736 0.105 Uiso 0.50 1 calc PR A 1 C20B C -0.1624(8) 0.8002(6) 0.2056(6) 0.080(4) Uiso 0.50 1 d PDU A 2 H12K H -0.2037 0.7740 0.1974 0.096 Uiso 0.50 1 calc PR A 2 H12L H -0.1482 0.8018 0.1680 0.096 Uiso 0.50 1 calc PR A 2 C21B C -0.1878(8) 0.8542(5) 0.2196(6) 0.061(3) Uiso 0.50 1 d PDU A 2 H12M H -0.2287 0.8702 0.1826 0.073 Uiso 0.50 1 calc PR A 2 H12N H -0.1449 0.8791 0.2388 0.073 Uiso 0.50 1 calc PR A 2 O22B O -0.2169(10) 0.8299(6) 0.2682(8) 0.137(5) Uiso 0.50 1 d PDU A 2 C23B C -0.2394(11) 0.8775(6) 0.2962(8) 0.084(4) Uiso 0.50 1 d PDU A 2 H12O H -0.2856 0.8950 0.2658 0.100 Uiso 0.50 1 calc PR A 2 H12P H -0.1973 0.9032 0.3136 0.100 Uiso 0.50 1 calc PR A 2 C24B C -0.2551(9) 0.8471(9) 0.3487(8) 0.112(6) Uiso 0.50 1 d PDU A 2 H12Q H -0.2831 0.8696 0.3680 0.135 Uiso 0.50 1 calc PR A 2 H12R H -0.2862 0.8154 0.3308 0.135 Uiso 0.50 1 calc PR A 2 O214 O -0.1796(4) 0.8322(3) 0.3967(3) 0.122(2) Uani 1 1 d D A . C215 C -0.1277(6) 0.8583(4) 0.4558(5) 0.107(3) Uani 1 1 d . . . H12S H -0.1295 0.8969 0.4500 0.129 Uiso 1 1 calc R A . H12T H -0.1431 0.8499 0.4917 0.129 Uiso 1 1 calc R . . C216 C -0.0523(6) 0.8391(3) 0.4685(5) 0.094(3) Uani 1 1 d . A . H12U H -0.0154 0.8557 0.5075 0.113 Uiso 1 1 calc R . . H12V H -0.0505 0.8006 0.4751 0.113 Uiso 1 1 calc R . . O217 O -0.0328(3) 0.85141(18) 0.4155(3) 0.0831(14) Uani 1 1 d . A . C218 C -0.0029(5) 0.9044(3) 0.4215(3) 0.0745(18) Uani 1 1 d . . . H13A H -0.0334 0.9280 0.4372 0.089 Uiso 1 1 calc R A . H13B H 0.0506 0.9049 0.4527 0.089 Uiso 1 1 calc R . . C219 C -0.0055(4) 0.9232(2) 0.3608(3) 0.0603(14) Uani 1 1 d . A . H13C H 0.0052 0.9614 0.3633 0.072 Uiso 1 1 calc R . . H13D H -0.0570 0.9173 0.3278 0.072 Uiso 1 1 calc R . . O220 O 0.0509(2) 0.89536(13) 0.34426(17) 0.0488(8) Uani 1 1 d . . . O300 O 0.3827(2) 0.94084(13) 0.13742(16) 0.0453(8) Uani 1 1 d . . . C301 C 0.3893(4) 0.9669(3) 0.0830(3) 0.0616(15) Uani 1 1 d . . . H23C H 0.4038 1.0041 0.0936 0.074 Uiso 1 1 calc R . . H23D H 0.3393 0.9661 0.0467 0.074 Uiso 1 1 calc R . . C302 C 0.4475(5) 0.9404(4) 0.0651(4) 0.093(3) Uani 1 1 d D . . H23A H 0.4484 0.9024 0.0747 0.112 Uiso 1 1 calc R E . H23B H 0.4344 0.9444 0.0188 0.112 Uiso 1 1 calc R . . O303 O 0.5203(3) 0.9626(3) 0.0992(3) 0.118(2) Uani 1 1 d D B . C30A C 0.5816(8) 0.9303(8) 0.1196(10) 0.21(2) Uani 0.30 1 d PDU B 1 H22M H 0.5672 0.8960 0.0977 0.255 Uiso 0.30 1 calc PR B 1 H22N H 0.5970 0.9241 0.1658 0.255 Uiso 0.30 1 calc PR B 1 C30B C 0.5685(6) 0.9335(6) 0.0734(6) 0.122(6) Uani 0.70 1 d PDU B 2 H22K H 0.5646 0.8953 0.0794 0.146 Uiso 0.70 1 calc PR B 2 H22L H 0.5530 0.9408 0.0275 0.146 Uiso 0.70 1 calc PR B 2 C306 C 0.6450(6) 0.9514(3) 0.1080(6) 0.108(3) Uani 1 1 d D . . H22O H 0.6922 0.9409 0.1439 0.130 Uiso 0.50 1 calc PR B 1 H22P H 0.6461 0.9342 0.0694 0.130 Uiso 0.50 1 calc PR B 1 H22Q H 0.6789 0.9345 0.0896 0.130 Uiso 0.50 1 d PR B 2 H22R H 0.6658 0.9435 0.1541 0.130 Uiso 0.50 1 d PR B 2 O307 O 0.6485(3) 1.0065(2) 0.0999(2) 0.0777(13) Uani 1 1 d D B . C308 C 0.7215(4) 1.0254(3) 0.1327(4) 0.080(2) Uani 1 1 d . . . H22I H 0.7253 1.0613 0.1173 0.095 Uiso 1 1 calc R B . H22J H 0.7584 1.0028 0.1232 0.095 Uiso 1 1 calc R . . C309 C 0.7431(4) 1.0271(4) 0.2030(4) 0.091(2) Uani 1 1 d . B . H22G H 0.7558 0.9915 0.2214 0.109 Uiso 1 1 calc R . . H22H H 0.7880 1.0502 0.2232 0.109 Uiso 1 1 calc R . . O310 O 0.6778(3) 1.0476(2) 0.2128(2) 0.0727(12) Uani 1 1 d D B . C311 C 0.6933(5) 1.0568(3) 0.2785(3) 0.079(2) Uani 1 1 d D . . H22E H 0.7348 1.0831 0.2947 0.095 Uiso 1 1 calc R E . H22F H 0.6472 1.0724 0.2819 0.095 Uiso 1 1 calc R . . C312 C 0.7148(4) 1.0116(4) 0.3189(4) 0.091(3) Uani 1 1 d D . . H22C H 0.7676 1.0018 0.3248 0.109 Uiso 1 1 calc R . . H22D H 0.7153 1.0215 0.3611 0.109 Uiso 1 1 calc R . . O313 O 0.6669(3) 0.9665(2) 0.2967(3) 0.0800(13) Uani 1 1 d . . . C314 C 0.5953(4) 0.9722(3) 0.2951(4) 0.077(2) Uani 1 1 d D . . H22A H 0.5620 0.9885 0.2544 0.092 Uiso 1 1 calc R . . H22B H 0.5958 0.9951 0.3304 0.092 Uiso 1 1 calc R . . C315 C 0.5659(3) 0.9185(2) 0.3014(3) 0.0589(14) Uani 1 1 d D . . H21A H 0.5802 0.8926 0.2755 0.071 Uiso 1 1 calc R E . H21B H 0.5872 0.9069 0.3464 0.071 Uiso 1 1 calc R . . O316 O 0.48482(18) 0.92350(13) 0.27922(17) 0.0436(7) Uani 1 1 d . . . Cl1 Cl 0.36836(10) 0.66906(5) 0.12057(7) 0.0667(4) Uani 1 1 d . . . O1A O 0.3590(4) 0.6792(2) 0.0574(3) 0.102(2) Uani 1 1 d . . . O1B O 0.2885(3) 0.6687(2) 0.1194(3) 0.0920(16) Uani 1 1 d . . . O1C O 0.4023(3) 0.70917(18) 0.1628(2) 0.0879(16) Uani 1 1 d . . . O1D O 0.3936(3) 0.61843(17) 0.1408(3) 0.0908(17) Uani 1 1 d . . . Cl2 Cl 0.17927(7) 0.41767(5) 0.47105(7) 0.0500(3) Uani 1 1 d . . . O2A O 0.2222(2) 0.46479(15) 0.4784(2) 0.0581(9) Uani 1 1 d . . . O2B O 0.1858(3) 0.3861(2) 0.4222(3) 0.101(2) Uani 1 1 d . . . O2C O 0.2098(3) 0.3902(2) 0.5308(3) 0.0882(15) Uani 1 1 d . . . O2D O 0.1004(2) 0.42965(15) 0.45774(19) 0.0567(9) Uani 1 1 d . . . Cl3 Cl 0.07771(6) 0.90692(4) 0.82536(5) 0.0394(2) Uani 1 1 d D . . O3A O 0.0895(3) 0.95198(17) 0.7929(3) 0.0804(14) Uani 1 1 d D . . O3B O 0.0692(3) 0.92571(19) 0.88131(19) 0.0714(12) Uani 1 1 d D . . O3C O 0.0103(2) 0.88234(16) 0.7844(2) 0.0716(13) Uani 1 1 d D . . O3D O 0.14168(19) 0.87219(12) 0.84021(17) 0.0484(8) Uani 1 1 d D . . Cl4 Cl 0.06168(7) 0.93602(4) 0.61161(6) 0.0445(3) Uani 1 1 d . . . O4A O 0.1104(2) 0.89733(15) 0.6031(2) 0.0634(11) Uani 1 1 d . . . O4B O 0.0089(3) 0.91438(19) 0.6344(3) 0.0969(19) Uani 1 1 d . . . O4C O 0.0190(3) 0.9611(2) 0.5538(3) 0.101(2) Uani 1 1 d . . . O4D O 0.1041(4) 0.9781(3) 0.6475(5) 0.158(4) Uani 1 1 d . . . Cl5A Cl 0.28876(18) 0.14650(13) 0.4219(2) 0.0794(10) Uani 0.50 1 d PD C 1 O5A O 0.3166(3) 0.0964(2) 0.4525(3) 0.0972(17) Uani 0.50 1 d PD C 1 O5B O 0.2194(6) 0.1613(7) 0.4260(8) 0.109(5) Uani 0.50 1 d PD C 1 O5C O 0.3440(6) 0.1846(4) 0.4472(7) 0.123(6) Uani 0.50 1 d PD C 1 O5D O 0.2792(7) 0.1381(5) 0.3559(5) 0.104(4) Uani 0.50 1 d PD C 1 Cl5B Cl 0.28621(15) 0.12351(14) 0.4839(2) 0.0830(12) Uani 0.50 1 d PD D 2 O5E O 0.3166(3) 0.0964(2) 0.4525(3) 0.0972(17) Uani 0.50 1 d PD D 2 O5F O 0.2081(6) 0.1347(6) 0.4475(8) 0.099(5) Uani 0.50 1 d PD D 2 O5G O 0.3282(6) 0.1631(5) 0.5217(8) 0.126(5) Uani 0.50 1 d PD D 2 O5H O 0.2867(8) 0.0874(6) 0.5359(6) 0.132(5) Uani 0.50 1 d PD D 2 Cl6A Cl 0.54048(10) 1.15812(7) 0.07277(9) 0.0743(4) Uiso 0.50 1 d PD E 1 O6A O 0.5084(6) 1.1830(4) 0.1111(5) 0.080 Uiso 0.50 1 d PD E 1 O6B O 0.5428(6) 1.1030(3) 0.0743(5) 0.080 Uiso 0.50 1 d PD E 1 O6C O 0.6054(5) 1.1857(4) 0.0821(5) 0.080 Uiso 0.50 1 d PD E 1 O6D O 0.5083(6) 1.1753(4) 0.0063(4) 0.080 Uiso 0.50 1 d PD E 1 Cl6B Cl 0.54048(10) 1.15812(7) 0.07277(9) 0.0743(4) Uiso 0.50 1 d PD E 2 O6E O 0.5542(6) 1.1836(4) 0.1306(4) 0.080 Uiso 0.50 1 d PD E 2 O6F O 0.5837(6) 1.1103(4) 0.0878(5) 0.080 Uiso 0.50 1 d PD E 2 O6G O 0.5682(6) 1.1851(4) 0.0321(5) 0.080 Uiso 0.50 1 d PD E 2 O6H O 0.4607(5) 1.1526(4) 0.0393(5) 0.080 Uiso 0.50 1 d PD E 2 N400 N 0.5072(5) 1.0685(4) 0.1810(4) 0.115(3) Uani 1 1 d . E . C401 C 0.4795(5) 1.1009(5) 0.2008(5) 0.100(3) Uani 1 1 d . . . C402 C 0.4438(6) 1.1415(6) 0.2230(6) 0.142(5) Uani 1 1 d . E . H73A H 0.4210 1.1674 0.1892 0.213 Uiso 1 1 calc R . . H73B H 0.4820 1.1587 0.2601 0.213 Uiso 1 1 calc R . . H73C H 0.4038 1.1261 0.2351 0.213 Uiso 1 1 calc R . . N403 N -0.0993(4) 0.7305(3) 0.3784(3) 0.098(2) Uani 1 1 d . A . C404 C -0.0825(4) 0.6880(3) 0.3980(3) 0.0723(17) Uani 1 1 d . . . C405 C -0.0592(5) 0.6365(3) 0.4237(4) 0.079(2) Uani 1 1 d . A . H83A H -0.0629 0.6122 0.3893 0.119 Uiso 1 1 calc R . . H83B H -0.0926 0.6243 0.4449 0.119 Uiso 1 1 calc R . . H83C H -0.0063 0.6377 0.4546 0.119 Uiso 1 1 calc R . . N406 N 0.0823(3) 0.7200(2) 0.4893(3) 0.0741(15) Uani 1 1 d . . . C407 C 0.1100(3) 0.7592(2) 0.4915(3) 0.0553(13) Uani 1 1 d . . . C408 C 0.1457(4) 0.8107(2) 0.4937(3) 0.0658(16) Uani 1 1 d . . . H90A H 0.1225 0.8278 0.4520 0.099 Uiso 1 1 calc R . . H90B H 0.2006 0.8061 0.5044 0.099 Uiso 1 1 calc R . . H90C H 0.1378 0.8326 0.5260 0.099 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0287(3) 0.0288(3) 0.0291(3) 0.0011(2) 0.0114(2) 0.0026(2) Cu2 0.0445(4) 0.0288(3) 0.0317(4) 0.0018(2) 0.0104(3) 0.0000(2) Li1 0.116(11) 0.162(15) 0.092(10) 0.060(10) 0.057(9) 0.099(12) Li2 0.086(8) 0.105(10) 0.082(9) 0.013(7) 0.038(7) 0.003(7) N11 0.0295(17) 0.0385(18) 0.0331(19) -0.0029(14) 0.0129(14) -0.0021(14) C12 0.032(2) 0.047(2) 0.032(2) -0.0020(18) 0.0104(18) 0.0010(18) C13 0.033(2) 0.067(3) 0.038(3) 0.000(2) 0.0115(19) -0.005(2) C14 0.038(2) 0.067(3) 0.048(3) 0.000(2) 0.012(2) -0.016(2) C15 0.052(3) 0.048(3) 0.050(3) 0.000(2) 0.018(2) -0.015(2) C16 0.040(2) 0.042(2) 0.039(3) 0.0003(19) 0.0140(19) -0.0027(19) N21 0.0331(17) 0.0356(18) 0.0295(19) 0.0002(14) 0.0115(14) 0.0032(14) C22 0.039(2) 0.034(2) 0.027(2) 0.0019(15) 0.0096(17) 0.0071(17) S23 0.0438(6) 0.0440(6) 0.0479(7) 0.0098(5) 0.0058(5) 0.0139(5) C24 0.036(2) 0.057(3) 0.040(3) 0.002(2) 0.003(2) 0.006(2) C25 0.032(2) 0.047(2) 0.031(2) -0.0023(18) 0.0082(17) 0.0032(18) N31 0.0401(19) 0.0268(16) 0.0239(17) 0.0005(12) 0.0111(14) 0.0065(14) C32 0.041(2) 0.0260(19) 0.029(2) -0.0003(15) 0.0113(18) 0.0067(16) C33 0.041(2) 0.0269(19) 0.037(2) -0.0037(16) 0.0110(19) 0.0021(17) C34 0.050(3) 0.0251(19) 0.042(3) 0.0029(17) 0.019(2) 0.0024(17) C35 0.043(2) 0.032(2) 0.033(2) 0.0052(16) 0.0132(18) 0.0071(17) C36 0.042(2) 0.031(2) 0.025(2) 0.0029(15) 0.0124(17) 0.0073(17) N41 0.0365(18) 0.0248(16) 0.0311(19) -0.0015(13) 0.0045(15) 0.0012(13) C42 0.036(2) 0.0234(18) 0.038(2) -0.0031(16) 0.0078(18) 0.0024(16) C43 0.045(2) 0.032(2) 0.041(3) -0.0028(18) 0.015(2) 0.0026(18) C44 0.041(2) 0.032(2) 0.052(3) -0.0027(19) 0.013(2) 0.0057(18) C45 0.040(2) 0.030(2) 0.041(3) 0.0015(17) 0.0052(19) 0.0033(17) C46 0.036(2) 0.0261(19) 0.035(2) 0.0007(16) 0.0032(18) -0.0004(16) N51 0.043(2) 0.0337(18) 0.030(2) 0.0016(14) 0.0071(16) 0.0008(15) C52 0.038(2) 0.035(2) 0.033(2) 0.0023(17) 0.0017(18) -0.0040(17) S53 0.0426(6) 0.0364(5) 0.0378(6) 0.0091(4) 0.0017(5) 0.0021(4) C54 0.048(3) 0.044(2) 0.034(3) 0.0073(19) 0.004(2) -0.007(2) C55 0.043(2) 0.043(2) 0.028(2) 0.0022(18) 0.0032(18) -0.0106(19) N61 0.054(2) 0.0379(19) 0.029(2) -0.0018(15) 0.0135(17) -0.0050(17) C62 0.047(3) 0.039(2) 0.030(2) -0.0012(17) 0.0055(19) -0.0036(19) C63 0.060(3) 0.054(3) 0.027(2) 0.003(2) 0.010(2) -0.005(2) C64 0.072(4) 0.062(3) 0.038(3) -0.004(2) 0.024(3) -0.004(3) C65 0.072(4) 0.051(3) 0.042(3) -0.005(2) 0.023(3) 0.004(3) C66 0.062(3) 0.040(2) 0.037(3) -0.0044(19) 0.017(2) 0.005(2) N71 0.0323(17) 0.0301(16) 0.0280(18) -0.0029(13) 0.0125(14) -0.0011(13) C72 0.037(2) 0.0307(19) 0.034(2) -0.0043(16) 0.0176(18) -0.0019(16) C73 0.046(2) 0.037(2) 0.049(3) -0.0040(19) 0.028(2) 0.0049(19) C74 0.057(3) 0.048(3) 0.041(3) -0.004(2) 0.030(2) -0.002(2) C75 0.053(3) 0.045(2) 0.037(3) -0.0006(19) 0.024(2) -0.006(2) C76 0.038(2) 0.034(2) 0.032(2) -0.0016(17) 0.0122(18) -0.0021(17) N81 0.0293(16) 0.0287(16) 0.0303(18) -0.0025(13) 0.0125(14) -0.0006(13) C82 0.0304(19) 0.0249(18) 0.032(2) 0.0014(15) 0.0111(16) 0.0008(15) S83 0.0392(5) 0.0292(5) 0.0414(6) 0.0061(4) 0.0169(5) 0.0079(4) C84 0.039(2) 0.032(2) 0.047(3) -0.0009(18) 0.022(2) 0.0051(17) C85 0.033(2) 0.0288(19) 0.037(2) -0.0044(16) 0.0168(17) -0.0008(16) N91 0.0307(16) 0.0280(16) 0.0241(17) -0.0007(12) 0.0093(13) -0.0005(13) C92 0.0304(19) 0.0301(19) 0.028(2) -0.0016(15) 0.0103(16) -0.0003(15) C93 0.037(2) 0.044(2) 0.027(2) -0.0007(17) 0.0142(17) -0.0029(18) C94 0.039(2) 0.040(2) 0.032(2) 0.0076(17) 0.0130(18) -0.0029(18) C95 0.035(2) 0.036(2) 0.031(2) 0.0061(16) 0.0126(17) 0.0003(17) C96 0.0301(19) 0.0291(19) 0.030(2) 0.0015(15) 0.0119(16) -0.0015(15) N101 0.0400(19) 0.0300(16) 0.0257(18) 0.0002(13) 0.0148(15) 0.0047(14) C102 0.037(2) 0.035(2) 0.026(2) -0.0024(16) 0.0149(17) 0.0037(17) C103 0.039(2) 0.036(2) 0.038(2) 0.0008(17) 0.0178(19) 0.0052(17) C104 0.039(2) 0.043(2) 0.047(3) 0.003(2) 0.014(2) 0.0098(19) C105 0.049(3) 0.033(2) 0.043(3) 0.0029(18) 0.017(2) 0.0123(19) C106 0.045(2) 0.031(2) 0.031(2) 0.0000(16) 0.0177(18) 0.0059(17) N111 0.046(2) 0.0282(17) 0.0327(19) 0.0003(14) 0.0151(16) -0.0001(15) C112 0.051(3) 0.029(2) 0.034(2) -0.0014(16) 0.020(2) 0.0052(18) S113 0.0606(7) 0.0270(5) 0.0476(7) 0.0033(4) 0.0228(6) 0.0069(5) C114 0.064(3) 0.028(2) 0.050(3) -0.0032(18) 0.029(2) -0.001(2) C115 0.054(3) 0.029(2) 0.036(2) -0.0060(17) 0.019(2) -0.0042(18) N121 0.046(2) 0.0359(19) 0.038(2) -0.0049(15) 0.0113(17) -0.0050(16) C122 0.053(3) 0.033(2) 0.046(3) -0.0102(19) 0.020(2) -0.0041(19) C123 0.058(3) 0.037(2) 0.073(4) -0.015(2) 0.029(3) -0.010(2) C124 0.051(3) 0.055(3) 0.083(4) -0.020(3) 0.024(3) -0.017(3) C125 0.047(3) 0.058(3) 0.065(4) -0.014(3) 0.014(3) -0.004(2) C126 0.052(3) 0.044(3) 0.043(3) -0.007(2) 0.008(2) -0.001(2) O200 0.0411(17) 0.0294(15) 0.066(2) -0.0024(14) 0.0082(16) -0.0009(13) C201 0.048(3) 0.038(2) 0.061(3) -0.002(2) 0.019(2) -0.005(2) C202 0.054(3) 0.055(3) 0.074(4) -0.015(3) 0.021(3) -0.006(3) O203 0.060(3) 0.110(4) 0.070(3) 0.006(3) 0.020(2) 0.025(3) O214 0.094(4) 0.165(6) 0.111(5) 0.046(5) 0.045(4) 0.064(4) C215 0.118(8) 0.099(6) 0.110(8) 0.010(5) 0.050(6) 0.015(6) C216 0.113(7) 0.090(5) 0.105(7) -0.014(5) 0.072(6) -0.012(5) O217 0.128(4) 0.058(2) 0.091(4) -0.003(2) 0.071(3) -0.006(3) C218 0.101(5) 0.058(4) 0.067(4) -0.004(3) 0.035(4) 0.009(3) C219 0.073(4) 0.054(3) 0.065(4) 0.001(3) 0.039(3) 0.012(3) O220 0.062(2) 0.0376(17) 0.052(2) 0.0024(14) 0.0265(17) 0.0123(15) O300 0.0510(19) 0.056(2) 0.0365(18) 0.0028(14) 0.0259(15) 0.0103(15) C301 0.066(3) 0.093(4) 0.040(3) 0.011(3) 0.036(3) 0.014(3) C302 0.098(6) 0.121(7) 0.079(5) -0.028(5) 0.055(5) -0.030(5) O303 0.057(3) 0.170(6) 0.121(5) 0.021(5) 0.025(3) -0.033(4) C30A 0.23(3) 0.23(3) 0.09(2) -0.06(3) -0.04(3) -0.03(3) C30B 0.110(9) 0.194(14) 0.089(9) -0.072(10) 0.069(8) -0.087(10) C306 0.121(7) 0.080(5) 0.166(10) 0.012(6) 0.102(8) -0.004(5) O307 0.074(3) 0.082(3) 0.086(3) -0.006(2) 0.040(3) -0.014(2) C308 0.067(4) 0.100(5) 0.082(5) -0.002(4) 0.041(4) -0.012(4) C309 0.058(4) 0.139(7) 0.076(5) -0.002(5) 0.026(4) -0.014(4) O310 0.066(3) 0.097(3) 0.062(3) 0.004(2) 0.033(2) -0.007(2) C311 0.096(5) 0.083(5) 0.060(4) -0.015(3) 0.033(4) -0.041(4) C312 0.083(5) 0.120(6) 0.069(5) -0.011(4) 0.029(4) -0.054(5) O313 0.080(3) 0.082(3) 0.089(3) -0.009(3) 0.045(3) -0.026(2) C314 0.056(4) 0.061(4) 0.121(6) -0.013(4) 0.042(4) -0.014(3) C315 0.040(3) 0.055(3) 0.081(4) -0.004(3) 0.023(3) -0.001(2) O316 0.0359(16) 0.0424(17) 0.052(2) -0.0020(14) 0.0160(15) -0.0023(13) Cl1 0.0942(11) 0.0422(6) 0.0524(8) -0.0156(5) 0.0156(7) 0.0088(7) O1A 0.164(6) 0.089(3) 0.075(3) -0.031(3) 0.071(4) -0.060(4) O1B 0.077(3) 0.111(4) 0.085(4) -0.017(3) 0.028(3) 0.010(3) O1C 0.127(4) 0.058(3) 0.067(3) -0.021(2) 0.024(3) 0.007(3) O1D 0.125(4) 0.046(2) 0.137(5) -0.005(3) 0.091(4) 0.012(2) Cl2 0.0504(6) 0.0421(6) 0.0617(8) -0.0095(5) 0.0262(6) -0.0024(5) O2A 0.055(2) 0.057(2) 0.068(3) -0.0140(18) 0.0308(19) -0.0134(17) O2B 0.099(4) 0.099(4) 0.128(5) -0.068(4) 0.068(4) -0.029(3) O2C 0.078(3) 0.083(3) 0.100(4) 0.029(3) 0.031(3) 0.013(3) O2D 0.048(2) 0.053(2) 0.065(2) -0.0112(17) 0.0168(18) -0.0074(16) Cl3 0.0428(6) 0.0358(5) 0.0394(6) -0.0005(4) 0.0155(4) 0.0057(4) O3A 0.089(3) 0.053(2) 0.117(4) 0.036(2) 0.060(3) 0.023(2) O3B 0.085(3) 0.084(3) 0.045(2) 0.002(2) 0.025(2) 0.030(2) O3C 0.048(2) 0.057(2) 0.081(3) -0.016(2) -0.007(2) 0.0192(18) O3D 0.0459(18) 0.0336(16) 0.056(2) 0.0000(14) 0.0086(16) 0.0076(14) Cl4 0.0484(6) 0.0433(6) 0.0460(7) 0.0059(4) 0.0228(5) 0.0103(5) O4A 0.065(2) 0.054(2) 0.085(3) 0.015(2) 0.044(2) 0.0229(18) O4B 0.124(4) 0.069(3) 0.150(5) 0.032(3) 0.112(4) 0.034(3) O4C 0.107(4) 0.127(5) 0.095(4) 0.057(3) 0.066(3) 0.062(4) O4D 0.077(4) 0.106(5) 0.251(10) -0.095(6) 0.018(5) 0.006(3) Cl5A 0.0520(16) 0.0687(19) 0.099(3) -0.0083(17) 0.0079(16) 0.0082(14) O5A 0.071(3) 0.098(4) 0.112(4) 0.011(3) 0.023(3) 0.015(3) O5B 0.052(6) 0.155(16) 0.112(11) -0.013(10) 0.023(6) 0.035(8) O5C 0.072(7) 0.069(6) 0.161(12) -0.031(7) -0.030(7) 0.006(5) O5D 0.095(8) 0.125(10) 0.085(8) -0.005(7) 0.025(6) 0.021(7) Cl5B 0.0321(13) 0.0726(19) 0.130(3) -0.036(2) 0.0155(16) 0.0031(12) O5E 0.071(3) 0.098(4) 0.112(4) 0.011(3) 0.023(3) 0.015(3) O5F 0.051(6) 0.104(10) 0.134(14) -0.007(8) 0.025(7) 0.017(6) O5G 0.070(7) 0.117(10) 0.189(15) -0.041(10) 0.048(8) 0.019(7) O5H 0.099(9) 0.158(14) 0.106(10) -0.014(10) 0.002(8) 0.008(9) N400 0.098(5) 0.158(8) 0.105(6) 0.020(5) 0.057(5) 0.023(5) C401 0.072(5) 0.139(8) 0.090(6) 0.009(6) 0.034(5) 0.004(5) C402 0.084(6) 0.177(12) 0.151(11) -0.035(9) 0.029(7) 0.008(7) N403 0.084(4) 0.120(6) 0.085(5) 0.024(4) 0.026(4) 0.026(4) C404 0.062(4) 0.090(5) 0.067(4) 0.007(4) 0.027(3) 0.002(3) C405 0.115(6) 0.062(4) 0.071(4) -0.013(3) 0.048(4) -0.023(4) N406 0.072(3) 0.064(3) 0.078(4) 0.007(3) 0.018(3) -0.007(3) C407 0.060(3) 0.057(3) 0.045(3) -0.001(2) 0.016(2) -0.002(3) C408 0.078(4) 0.053(3) 0.064(4) -0.008(3) 0.025(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N21 1.938(3) . ? Cu1 N81 1.940(3) . ? Cu1 N11 2.144(3) . ? Cu1 N71 2.170(3) . ? Cu1 N31 2.468(3) . ? Cu2 N51 1.929(4) . ? Cu2 N111 1.933(3) . ? Cu2 N121 2.156(4) . ? Cu2 N61 2.157(4) . ? Li1 O217 2.00(2) . ? Li1 O22A 2.029(15) . ? Li1 O214 2.111(15) . ? Li1 N403 2.118(19) . ? Li1 O203 2.116(16) . ? Li1 O22B 2.18(2) . ? Li1 C216 2.67(2) . ? Li1 C23A 2.78(2) . ? Li2 O310 1.974(16) . ? Li2 N400 2.052(17) . ? Li2 O307 2.062(15) . ? Li2 O6B 2.075(17) . ? Li2 O6F 2.120(17) . ? Li2 O303 2.324(17) . ? N11 C16 1.338(6) . ? N11 C12 1.349(6) . ? C12 C13 1.388(6) . ? C12 C25 1.473(7) . ? C13 C14 1.378(8) . ? C14 C15 1.381(8) . ? C15 C16 1.389(7) . ? N21 C22 1.316(5) . ? N21 C25 1.363(6) . ? C22 C36 1.462(6) . ? C22 S23 1.715(4) . ? S23 C24 1.707(6) . ? C24 C25 1.354(7) . ? N31 C32 1.321(6) . ? N31 C36 1.355(5) . ? C32 C33 1.410(6) . ? C32 C42 1.490(6) . ? C33 O200 1.342(5) . ? C33 C34 1.396(6) . ? C34 C35 1.380(7) . ? C35 C36 1.382(6) . ? N41 C42 1.316(6) . ? N41 C46 1.361(5) . ? C42 C43 1.407(6) . ? C43 O220 1.347(6) . ? C43 C44 1.400(6) . ? C44 C45 1.374(7) . ? C45 C46 1.384(7) . ? C46 C52 1.440(7) . ? N51 C52 1.301(6) . ? N51 C55 1.382(6) . ? C52 S53 1.725(4) . ? S53 C54 1.709(6) . ? C54 C55 1.358(7) . ? C55 C62 1.464(7) . ? N61 C66 1.340(6) . ? N61 C62 1.359(6) . ? C62 C63 1.391(7) . ? C63 C64 1.365(8) . ? C64 C65 1.376(8) . ? C65 C66 1.385(8) . ? N71 C76 1.339(6) . ? N71 C72 1.348(5) . ? C72 C73 1.381(6) . ? C72 C85 1.478(6) . ? C73 C74 1.378(7) . ? C74 C75 1.378(7) . ? C75 C76 1.389(6) . ? N81 C82 1.309(5) . ? N81 C85 1.371(5) . ? C82 C96 1.462(6) . ? C82 S83 1.713(4) . ? S83 C84 1.717(5) . ? C84 C85 1.352(6) . ? N91 C92 1.326(5) . ? N91 C96 1.352(5) . ? C92 C93 1.415(6) . ? C92 C102 1.493(6) . ? C93 O300 1.361(5) . ? C93 C94 1.375(6) . ? C94 C95 1.382(6) . ? C95 C96 1.391(6) . ? N101 C102 1.322(6) . ? N101 C106 1.358(5) . ? C102 C103 1.400(6) . ? C103 O316 1.351(5) . ? C103 C104 1.400(6) . ? C104 C105 1.380(7) . ? C105 C106 1.385(7) . ? C106 C112 1.454(6) . ? N111 C112 1.309(6) . ? N111 C115 1.368(6) . ? C112 S113 1.721(4) . ? S113 C114 1.716(6) . ? C114 C115 1.353(7) . ? C115 C122 1.466(7) . ? N121 C126 1.339(7) . ? N121 C122 1.357(6) . ? C122 C123 1.380(7) . ? C123 C124 1.387(9) . ? C124 C125 1.357(9) . ? C125 C126 1.394(8) . ? O200 C201 1.442(6) . ? C201 C202 1.497(7) . ? C202 O203 1.400(7) . ? O203 C20A 1.396(12) . ? O203 C20B 1.475(12) . ? C20A C21A 1.526(15) . ? C21A O22A 1.551(13) . ? O22A C23A 1.488(12) . ? C23A C24A 1.545(14) . ? C24A O214 1.476(12) . ? C20B C21B 1.530(13) . ? C21B O22B 1.542(13) . ? O22B C23B 1.504(13) . ? C23B C24B 1.545(15) . ? C24B O214 1.479(13) . ? O214 C215 1.486(13) . ? C215 C216 1.432(13) . ? C216 O217 1.427(9) . ? O217 C218 1.450(8) . ? C218 C219 1.444(9) . ? C219 O220 1.446(6) . ? O300 C301 1.452(6) . ? C301 C302 1.479(10) . ? C302 O303 1.415(9) . ? O303 C30A 1.352(17) . ? O303 C30B 1.462(12) . ? C30A C306 1.430(14) . ? C30B C306 1.433(13) . ? C306 O307 1.418(9) . ? O307 C308 1.383(8) . ? C308 C309 1.494(11) . ? C309 O310 1.437(9) . ? O310 C311 1.429(8) . ? C311 C312 1.430(11) . ? C312 O313 1.432(8) . ? O313 C314 1.351(8) . ? C314 C315 1.503(8) . ? C315 O316 1.427(6) . ? Cl1 O1C 1.381(5) . ? Cl1 O1D 1.390(5) . ? Cl1 O1A 1.404(5) . ? Cl1 O1B 1.504(6) . ? Cl2 O2B 1.415(5) . ? Cl2 O2A 1.422(4) . ? Cl2 O2D 1.439(4) . ? Cl2 O2C 1.439(5) . ? Cl3 O3C 1.408(4) . ? Cl3 O3B 1.427(4) . ? Cl3 O3A 1.428(4) . ? Cl3 O3D 1.432(3) . ? Cl4 O4D 1.399(6) . ? Cl4 O4B 1.403(5) . ? Cl4 O4C 1.408(5) . ? Cl4 O4A 1.414(4) . ? Cl5A O5C 1.380(9) . ? Cl5A O5B 1.404(10) . ? Cl5A O5A 1.452(6) . ? Cl5A O5D 1.458(10) . ? Cl5B O5G 1.365(10) . ? Cl5B O5F 1.422(10) . ? Cl5B O5H 1.496(12) . ? Cl6A O6C 1.360(9) . ? Cl6A O6A 1.392(9) . ? Cl6A O6B 1.405(8) . ? Cl6A O6D 1.466(9) . ? N400 C401 1.157(12) . ? C401 C402 1.430(15) . ? N403 C404 1.167(10) . ? C404 C405 1.436(11) . ? N406 C407 1.120(8) . ? C407 C408 1.467(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 N21 Cu1 N81 177.34(15) . . ? N21 Cu1 N11 77.92(14) . . ? N81 Cu1 N11 99.44(14) . . ? N21 Cu1 N71 103.06(14) . . ? N81 Cu1 N71 77.60(13) . . ? N11 Cu1 N71 111.08(13) . . ? N21 Cu1 N31 71.41(13) . . ? N81 Cu1 N31 111.25(13) . . ? N11 Cu1 N31 148.59(12) . . ? N71 Cu1 N31 82.85(12) . . ? N51 Cu2 N111 177.13(16) . . ? N51 Cu2 N121 98.81(16) . . ? N111 Cu2 N121 78.36(15) . . ? N51 Cu2 N61 78.28(16) . . ? N111 Cu2 N61 102.46(15) . . ? N121 Cu2 N61 115.70(15) . . ? O217 Li1 O22A 108.7(10) . . ? O217 Li1 O214 81.9(7) . . ? O22A Li1 O214 80.4(5) . . ? O217 Li1 N403 107.0(7) . . ? O22A Li1 N403 142.8(12) . . ? O214 Li1 N403 94.7(7) . . ? O217 Li1 O203 122.5(9) . . ? O22A Li1 O203 79.0(6) . . ? O214 Li1 O203 152.2(10) . . ? N403 Li1 O203 90.5(7) . . ? O217 Li1 O22B 133.5(10) . . ? O22A Li1 O22B 26.3(5) . . ? O214 Li1 O22B 79.1(6) . . ? N403 Li1 O22B 116.5(12) . . ? O203 Li1 O22B 74.1(7) . . ? O217 Li1 C216 31.7(3) . . ? O22A Li1 C216 118.1(8) . . ? O214 Li1 C216 57.4(5) . . ? N403 Li1 C216 88.2(5) . . ? O203 Li1 C216 150.2(8) . . ? O22B Li1 C216 132.2(7) . . ? O217 Li1 C23A 116.2(8) . . ? O22A Li1 C23A 31.4(4) . . ? O214 Li1 C23A 54.7(4) . . ? N403 Li1 C23A 119.4(10) . . ? O203 Li1 C23A 99.3(6) . . ? O22B Li1 C23A 25.3(5) . . ? C216 Li1 C23A 107.3(6) . . ? O310 Li2 N400 99.7(7) . . ? O310 Li2 O307 81.3(6) . . ? N400 Li2 O307 173.2(9) . . ? O310 Li2 O6B 120.0(8) . . ? N400 Li2 O6B 89.1(7) . . ? O307 Li2 O6B 96.2(7) . . ? O310 Li2 O6F 100.7(7) . . ? N400 Li2 O6F 99.2(7) . . ? O307 Li2 O6F 87.1(6) . . ? O6B Li2 O6F 20.3(4) . . ? O310 Li2 O303 123.6(7) . . ? N400 Li2 O303 99.3(7) . . ? O307 Li2 O303 74.7(6) . . ? O6B Li2 O303 112.8(7) . . ? O6F Li2 O303 127.5(8) . . ? C16 N11 C12 118.8(4) . . ? C16 N11 Cu1 127.1(3) . . ? C12 N11 Cu1 114.1(3) . . ? N11 C12 C13 122.1(4) . . ? N11 C12 C25 113.5(4) . . ? C13 C12 C25 124.4(4) . . ? C14 C13 C12 118.5(5) . . ? C13 C14 C15 119.9(5) . . ? C14 C15 C16 118.6(5) . . ? N11 C16 C15 122.2(5) . . ? C22 N21 C25 112.9(4) . . ? C22 N21 Cu1 126.8(3) . . ? C25 N21 Cu1 120.2(3) . . ? N21 C22 C36 118.7(4) . . ? N21 C22 S23 112.5(3) . . ? C36 C22 S23 128.9(3) . . ? C24 S23 C22 90.2(2) . . ? C25 C24 S23 110.5(4) . . ? C24 C25 N21 113.9(4) . . ? C24 C25 C12 131.9(4) . . ? N21 C25 C12 114.2(4) . . ? C32 N31 C36 118.2(4) . . ? C32 N31 Cu1 130.7(3) . . ? C36 N31 Cu1 109.7(3) . . ? N31 C32 C33 122.8(4) . . ? N31 C32 C42 116.4(4) . . ? C33 C32 C42 120.7(4) . . ? O200 C33 C34 127.1(4) . . ? O200 C33 C32 114.3(4) . . ? C34 C33 C32 118.6(4) . . ? C35 C34 C33 118.2(4) . . ? C34 C35 C36 119.7(4) . . ? N31 C36 C35 122.6(4) . . ? N31 C36 C22 112.0(4) . . ? C35 C36 C22 125.4(4) . . ? C42 N41 C46 119.0(4) . . ? N41 C42 C43 122.5(4) . . ? N41 C42 C32 115.5(4) . . ? C43 C42 C32 122.0(4) . . ? O220 C43 C44 126.2(4) . . ? O220 C43 C42 115.7(4) . . ? C44 C43 C42 118.0(4) . . ? C45 C44 C43 119.3(4) . . ? C44 C45 C46 119.1(4) . . ? N41 C46 C45 122.0(4) . . ? N41 C46 C52 112.6(4) . . ? C45 C46 C52 125.4(4) . . ? C52 N51 C55 114.0(4) . . ? C52 N51 Cu2 126.4(3) . . ? C55 N51 Cu2 119.4(3) . . ? N51 C52 C46 119.9(4) . . ? N51 C52 S53 111.8(4) . . ? C46 C52 S53 128.3(4) . . ? C54 S53 C52 90.7(2) . . ? C55 C54 S53 110.5(4) . . ? C54 C55 N51 113.0(5) . . ? C54 C55 C62 132.1(5) . . ? N51 C55 C62 114.9(4) . . ? C66 N61 C62 117.7(4) . . ? C66 N61 Cu2 128.8(3) . . ? C62 N61 Cu2 113.4(3) . . ? N61 C62 C63 121.9(5) . . ? N61 C62 C55 113.4(4) . . ? C63 C62 C55 124.7(4) . . ? C64 C63 C62 119.2(5) . . ? C63 C64 C65 119.6(5) . . ? C64 C65 C66 118.8(5) . . ? N61 C66 C65 122.8(5) . . ? C76 N71 C72 117.9(4) . . ? C76 N71 Cu1 128.2(3) . . ? C72 N71 Cu1 113.9(3) . . ? N71 C72 C73 123.1(4) . . ? N71 C72 C85 113.5(3) . . ? C73 C72 C85 123.4(4) . . ? C74 C73 C72 118.4(4) . . ? C73 C74 C75 119.2(4) . . ? C74 C75 C76 119.2(4) . . ? N71 C76 C75 122.1(4) . . ? C82 N81 C85 112.8(3) . . ? C82 N81 Cu1 126.8(3) . . ? C85 N81 Cu1 120.4(3) . . ? N81 C82 C96 119.3(3) . . ? N81 C82 S83 112.9(3) . . ? C96 C82 S83 127.8(3) . . ? C82 S83 C84 90.2(2) . . ? C85 C84 S83 110.1(3) . . ? C84 C85 N81 114.0(4) . . ? C84 C85 C72 131.6(4) . . ? N81 C85 C72 114.4(3) . . ? C92 N91 C96 118.5(3) . . ? N91 C92 C93 121.9(4) . . ? N91 C92 C102 114.3(3) . . ? C93 C92 C102 123.7(4) . . ? O300 C93 C94 125.4(4) . . ? O300 C93 C92 115.5(4) . . ? C94 C93 C92 119.0(4) . . ? C93 C94 C95 119.2(4) . . ? C94 C95 C96 118.5(4) . . ? N91 C96 C95 122.8(4) . . ? N91 C96 C82 112.6(3) . . ? C95 C96 C82 124.6(4) . . ? C102 N101 C106 118.7(4) . . ? N101 C102 C103 122.7(4) . . ? N101 C102 C92 116.1(4) . . ? C103 C102 C92 121.1(4) . . ? O316 C103 C104 126.1(4) . . ? O316 C103 C102 115.2(4) . . ? C104 C103 C102 118.6(4) . . ? C105 C104 C103 118.3(4) . . ? C104 C105 C106 119.7(4) . . ? N101 C106 C105 121.9(4) . . ? N101 C106 C112 112.7(4) . . ? C105 C106 C112 125.4(4) . . ? C112 N111 C115 113.9(4) . . ? C112 N111 Cu2 126.4(3) . . ? C115 N111 Cu2 119.6(3) . . ? N111 C112 C106 119.5(4) . . ? N111 C112 S113 111.8(3) . . ? C106 C112 S113 128.7(3) . . ? C114 S113 C112 90.4(2) . . ? C115 C114 S113 110.3(4) . . ? C114 C115 N111 113.5(4) . . ? C114 C115 C122 131.5(4) . . ? N111 C115 C122 114.9(4) . . ? C126 N121 C122 119.1(4) . . ? C126 N121 Cu2 127.8(3) . . ? C122 N121 Cu2 113.0(3) . . ? N121 C122 C123 121.8(5) . . ? N121 C122 C115 113.8(4) . . ? C123 C122 C115 124.4(5) . . ? C122 C123 C124 118.1(5) . . ? C125 C124 C123 120.6(5) . . ? C124 C125 C126 118.8(5) . . ? N121 C126 C125 121.6(5) . . ? C33 O200 C201 118.2(4) . . ? O200 C201 C202 105.9(4) . . ? O203 C202 C201 112.3(5) . . ? C20A O203 C202 122.5(8) . . ? C20A O203 C20B 32.7(8) . . ? C202 O203 C20B 113.6(7) . . ? C20A O203 Li1 111.3(8) . . ? C202 O203 Li1 126.2(5) . . ? C20B O203 Li1 111.7(7) . . ? O203 C20A C21A 104.0(13) . . ? C20A C21A O22A 100.2(12) . . ? C23A O22A C21A 98.8(10) . . ? C23A O22A Li1 103.2(10) . . ? C21A O22A Li1 107.2(11) . . ? O22A C23A C24A 100.5(11) . . ? O22A C23A Li1 45.3(7) . . ? C24A C23A Li1 80.0(9) . . ? O214 C24A C23A 100.5(11) . . ? O203 C20B C21B 104.9(10) . . ? C20B C21B O22B 91.0(11) . . ? C23B O22B C21B 102.6(12) . . ? C23B O22B Li1 99.5(12) . . ? C21B O22B Li1 102.4(11) . . ? O22B C23B C24B 95.4(14) . . ? O214 C24B C23B 106.4(13) . . ? C24A O214 C24B 32.4(9) . . ? C24A O214 C215 103.9(9) . . ? C24B O214 C215 132.3(12) . . ? C24A O214 Li1 108.5(8) . . ? C24B O214 Li1 107.1(10) . . ? C215 O214 Li1 106.1(8) . . ? C216 C215 O214 107.1(8) . . ? O217 C216 C215 108.4(8) . . ? O217 C216 Li1 47.3(6) . . ? C215 C216 Li1 84.3(7) . . ? C216 O217 C218 110.1(5) . . ? C216 O217 Li1 101.0(7) . . ? C218 O217 Li1 135.7(6) . . ? C219 C218 O217 110.4(6) . . ? C218 C219 O220 109.2(5) . . ? C43 O220 C219 115.1(4) . . ? C93 O300 C301 115.9(4) . . ? O300 C301 C302 110.1(6) . . ? O303 C302 C301 109.8(7) . . ? C30A O303 C302 118.3(11) . . ? C30A O303 C30B 40.8(9) . . ? C302 O303 C30B 101.9(7) . . ? C30A O303 Li2 99.9(10) . . ? C302 O303 Li2 141.8(7) . . ? C30B O303 Li2 108.5(6) . . ? O303 C30A C306 112.3(12) . . ? C306 C30B O303 105.9(8) . . ? O307 C306 C30A 118.7(11) . . ? O307 C306 C30B 109.3(10) . . ? C30A C306 C30B 40.3(8) . . ? C308 O307 C306 111.1(7) . . ? C308 O307 Li2 106.4(6) . . ? C306 O307 Li2 107.9(6) . . ? O307 C308 C309 113.3(6) . . ? O310 C309 C308 106.2(6) . . ? C311 O310 C309 112.2(6) . . ? C311 O310 Li2 130.2(6) . . ? C309 O310 Li2 115.7(6) . . ? C312 C311 O310 115.8(7) . . ? O313 C312 C311 115.6(6) . . ? C314 O313 C312 114.6(6) . . ? O313 C314 C315 107.7(5) . . ? O316 C315 C314 105.9(5) . . ? C103 O316 C315 118.4(4) . . ? O1C Cl1 O1D 116.4(4) . . ? O1C Cl1 O1A 114.8(3) . . ? O1D Cl1 O1A 113.8(4) . . ? O1C Cl1 O1B 102.4(3) . . ? O1D Cl1 O1B 102.5(3) . . ? O1A Cl1 O1B 104.6(4) . . ? O2B Cl2 O2A 110.7(3) . . ? O2B Cl2 O2D 110.5(3) . . ? O2A Cl2 O2D 110.3(2) . . ? O2B Cl2 O2C 110.0(4) . . ? O2A Cl2 O2C 107.1(3) . . ? O2D Cl2 O2C 108.2(3) . . ? O3C Cl3 O3B 110.9(3) . . ? O3C Cl3 O3A 107.2(3) . . ? O3B Cl3 O3A 106.7(3) . . ? O3C Cl3 O3D 110.7(2) . . ? O3B Cl3 O3D 111.8(2) . . ? O3A Cl3 O3D 109.4(2) . . ? O4D Cl4 O4B 114.5(5) . . ? O4D Cl4 O4C 101.2(5) . . ? O4B Cl4 O4C 106.8(4) . . ? O4D Cl4 O4A 110.7(3) . . ? O4B Cl4 O4A 111.9(3) . . ? O4C Cl4 O4A 111.0(3) . . ? O5C Cl5A O5B 111.2(9) . . ? O5C Cl5A O5A 109.8(6) . . ? O5B Cl5A O5A 112.4(8) . . ? O5C Cl5A O5D 108.0(9) . . ? O5B Cl5A O5D 110.9(8) . . ? O5A Cl5A O5D 104.2(6) . . ? O5G Cl5B O5F 116.4(8) . . ? O5G Cl5B O5H 97.5(9) . . ? O5F Cl5B O5H 105.9(8) . . ? O6C Cl6A O6A 104.6(6) . . ? O6C Cl6A O6B 119.6(6) . . ? O6A Cl6A O6B 117.1(6) . . ? O6C Cl6A O6D 90.1(6) . . ? O6A Cl6A O6D 113.8(6) . . ? O6B Cl6A O6D 108.7(6) . . ? Cl6A O6B Li2 139.8(8) . . ? C401 N400 Li2 153.6(10) . . ? N400 C401 C402 178.0(12) . . ? C404 N403 Li1 170.9(8) . . ? N403 C404 C405 177.9(9) . . ? N406 C407 C408 179.4(8) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 70.25 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.693 _refine_diff_density_min -1.679 _refine_diff_density_rms 0.108