# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Kai Chen' _publ_contact_author_email kaichen85@gmail.com _publ_author_name 'Kai Chen' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 882714' #TrackingRef '- compound 1 -3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 Ca2 Cl4 N20 O11' _chemical_formula_weight 1068.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.7209(15) _cell_length_b 19.4444(9) _cell_length_c 32.739(2) _cell_angle_alpha 90.00 _cell_angle_beta 115.904(2) _cell_angle_gamma 90.00 _cell_volume 18737.2(18) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5075 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 21.56 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12448 _exptl_absorpt_coefficient_mu 0.547 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8976 _exptl_absorpt_correction_T_max 0.9469 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 205392 _diffrn_reflns_av_R_equivalents 0.1702 _diffrn_reflns_av_sigmaI/netI 0.0802 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16481 _reflns_number_gt 5932 _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 SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1250P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16481 _refine_ls_number_parameters 1208 _refine_ls_number_restraints 154 _refine_ls_R_factor_all 0.1753 _refine_ls_R_factor_gt 0.1015 _refine_ls_wR_factor_ref 0.2911 _refine_ls_wR_factor_gt 0.2591 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.087 _refine_ls_shift/su_mean 0.014 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 Cl3 Cl 0.68107(10) 0.00004(12) 0.06872(10) 0.0738(11) Uani 0.997(7) 1 d P . . Cl4 Cl 0.31898(9) 0.49985(12) 0.93118(10) 0.0718(8) Uani 1 1 d . . . Cl5 Cl 0.15285(14) 0.10390(18) 0.82696(16) 0.1329(15) Uani 1 1 d . . . Cl6 Cl 0.1521(2) 0.3965(2) 0.82678(19) 0.168(2) Uani 1 1 d . . . Cl7 Cl 0.57653(17) 0.1038(2) 0.90189(16) 0.1427(16) Uani 1 1 d . . . Cl8 Cl 0.57632(16) 0.39660(17) 0.90166(18) 0.1510(18) Uani 1 1 d . . . O1W O 0.62501(19) 0.2508(5) 1.26260(17) 0.0804(18) Uani 1 1 d . . . O2W O 0.51248(17) 0.2500(5) 0.87481(19) 0.0756(17) Uani 1 1 d . . . Cl1 Cl 0.52303(6) 0.25017(13) 1.09446(6) 0.0494(4) Uani 1 1 d . . . Cl2 Cl 0.34430(5) 0.25020(13) 0.77283(6) 0.0491(4) Uani 1 1 d . . . Ca1 Ca 0.57292(4) 0.24999(10) 1.18575(4) 0.0390(3) Uani 1 1 d . . . Ca2 Ca 0.46467(5) 0.25032(10) 0.98666(5) 0.0458(4) Uani 1 1 d . . . Ca3 Ca 0.43571(4) 0.24991(10) 0.82283(4) 0.0389(3) Uani 1 1 d . . . Ca4 Ca 0.23657(5) 0.25008(10) 0.71457(5) 0.0451(3) Uani 1 1 d . . . C1 C 0.5788(3) 0.0926(3) 1.1432(3) 0.038(2) Uani 1 1 d U . . C2 C 0.5338(3) 0.0257(4) 1.0826(3) 0.036(2) Uani 1 1 d . . . H2 H 0.5329 -0.0257 1.0836 0.043 Uiso 1 1 calc R . . C3 C 0.5752(3) 0.0506(3) 1.0769(3) 0.0368(19) Uani 1 1 d . . . H3 H 0.5924 0.0107 1.0729 0.044 Uiso 1 1 calc R . . C4 C 0.5098(3) 0.0903(4) 1.0174(3) 0.0374(19) Uani 1 1 d U . . C5 C 0.6447(2) 0.1235(3) 1.1283(2) 0.0268(16) Uani 1 1 d . . . H5A H 0.6626 0.0966 1.1161 0.032 Uiso 1 1 calc R . . H5B H 0.6625 0.1262 1.1616 0.032 Uiso 1 1 calc R . . C6 C 0.5818(3) 0.1233(3) 1.0137(3) 0.042(2) Uani 1 1 d . . . H6A H 0.6088 0.0947 1.0196 0.050 Uiso 1 1 calc R . . H6B H 0.5622 0.1226 0.9805 0.050 Uiso 1 1 calc R . . C7 C 0.63829(18) 0.2484(5) 1.1338(2) 0.0354(14) Uani 1 1 d U . . C8 C 0.6385(3) 0.2105(4) 1.0662(3) 0.039(2) Uani 1 1 d . . . H8 H 0.6657 0.1918 1.0636 0.046 Uiso 1 1 calc R . . C9 C 0.6377(2) 0.2909(4) 1.0663(3) 0.0328(18) Uani 1 1 d U . . H9 H 0.6648 0.3106 1.0638 0.039 Uiso 1 1 calc R . . C10 C 0.5734(2) 0.2508(4) 1.0054(2) 0.0322(12) Uani 1 1 d . . . C11 C 0.6449(3) 0.3754(4) 1.1293(3) 0.044(2) Uani 1 1 d U . . H11A H 0.6631 0.4027 1.1177 0.053 Uiso 1 1 calc R . . H11B H 0.6623 0.3725 1.1628 0.053 Uiso 1 1 calc R . . C12 C 0.5814(2) 0.3762(4) 1.0129(3) 0.0366(19) Uani 1 1 d U . . H12A H 0.5620 0.3759 0.9797 0.044 Uiso 1 1 calc R . . H12B H 0.6082 0.4052 1.0187 0.044 Uiso 1 1 calc R . . C13 C 0.5811(2) 0.4030(4) 1.1475(3) 0.0362(19) Uani 1 1 d . . . C14 C 0.5759(2) 0.4481(4) 1.0767(3) 0.0379(19) Uani 1 1 d U . . H14 H 0.5935 0.4878 1.0731 0.045 Uiso 1 1 calc R . . C15 C 0.5342(2) 0.4734(4) 1.0841(3) 0.0350(19) Uani 1 1 d U . . H15 H 0.5334 0.5248 1.0854 0.042 Uiso 1 1 calc R . . C16 C 0.5089(2) 0.4096(4) 1.0143(3) 0.038(2) Uani 1 1 d . . . C17 C 0.5130(2) 0.4542(4) 1.1486(2) 0.0306(17) Uani 1 1 d U . . H17A H 0.5314 0.4533 1.1819 0.037 Uiso 1 1 calc R . . H17B H 0.4994 0.5007 1.1404 0.037 Uiso 1 1 calc R . . C18 C 0.4488(3) 0.4562(4) 1.0342(3) 0.040(2) Uani 1 1 d . . . H18A H 0.4305 0.4557 1.0008 0.048 Uiso 1 1 calc R . . H18B H 0.4451 0.5021 1.0452 0.048 Uiso 1 1 calc R . . C19 C 0.4802(3) 0.3466(5) 1.1589(3) 0.046(2) Uani 1 1 d . . . C20 C 0.4326(3) 0.4111(4) 1.0993(3) 0.041(2) Uani 1 1 d U . . H20 H 0.4171 0.4542 1.1017 0.049 Uiso 1 1 calc R . . C21 C 0.4061(3) 0.3460(4) 1.1028(3) 0.040(2) Uani 1 1 d . . . H21 H 0.3782 0.3582 1.1066 0.048 Uiso 1 1 calc R . . C22 C 0.4066(2) 0.3474(4) 1.0295(3) 0.0285(16) Uani 1 1 d U . . C23 C 0.4324(2) 0.2495(4) 1.1624(2) 0.0425(15) Uani 1 1 d . . . H23A H 0.4531 0.2491 1.1953 0.051 Uiso 1 1 calc R . . H23B H 0.4008 0.2493 1.1591 0.051 Uiso 1 1 calc R . . C24 C 0.3670(2) 0.2510(4) 1.0449(2) 0.0390(14) Uani 1 1 d . . . H24A H 0.3442 0.2522 1.0572 0.047 Uiso 1 1 calc R . . H24B H 0.3504 0.2507 1.0113 0.047 Uiso 1 1 calc R . . C25 C 0.4806(3) 0.1560(4) 1.1600(3) 0.0365(19) Uani 1 1 d U . . C26 C 0.4071(3) 0.1529(4) 1.1033(3) 0.040(2) Uani 1 1 d . . . H26 H 0.3799 0.1406 1.1082 0.048 Uiso 1 1 calc R . . C27 C 0.4318(3) 0.0878(3) 1.0989(3) 0.0337(19) Uani 1 1 d . . . H27 H 0.4167 0.0446 1.1018 0.040 Uiso 1 1 calc R . . C28 C 0.4085(3) 0.1512(4) 1.0346(3) 0.0361(19) Uani 1 1 d U . . C29 C 0.5126(3) 0.0470(4) 1.1495(3) 0.043(2) Uani 1 1 d U . . H29A H 0.5319 0.0515 1.1825 0.052 Uiso 1 1 calc R . . H29B H 0.4995 0.0001 1.1437 0.052 Uiso 1 1 calc R . . C30 C 0.4483(3) 0.0444(4) 1.0336(3) 0.040(2) Uani 1 1 d . . . H30A H 0.4299 0.0476 1.0003 0.047 Uiso 1 1 calc R . . H30B H 0.4436 -0.0022 1.0431 0.047 Uiso 1 1 calc R . . C31 C 0.3843(2) 0.2509(4) 0.88862(19) 0.0320(13) Uani 1 1 d . . . C32 C 0.3174(2) 0.2915(4) 0.8884(3) 0.0327(18) Uani 1 1 d U . . H32 H 0.3152 0.3112 0.9156 0.039 Uiso 1 1 calc R . . C33 C 0.3157(2) 0.2103(4) 0.8879(3) 0.0344(18) Uani 1 1 d U . . H33 H 0.3130 0.1915 0.9151 0.041 Uiso 1 1 calc R . . C34 C 0.25569(19) 0.2509(4) 0.8239(2) 0.0328(13) Uani 1 1 d U . . C35 C 0.3778(2) 0.1249(4) 0.8937(3) 0.0359(18) Uani 1 1 d U . . H35A H 0.3655 0.0978 0.9115 0.043 Uiso 1 1 calc R . . H35B H 0.4112 0.1275 0.9119 0.043 Uiso 1 1 calc R . . C36 C 0.2625(3) 0.1221(4) 0.8312(3) 0.049(2) Uani 1 1 d . . . H36A H 0.2684 0.0928 0.8579 0.059 Uiso 1 1 calc R . . H36B H 0.2293 0.1221 0.8117 0.059 Uiso 1 1 calc R . . C37 C 0.3960(2) 0.0956(3) 0.8313(2) 0.0261(16) Uani 1 1 d U . . C38 C 0.3260(2) 0.0507(4) 0.8260(2) 0.0312(17) Uani 1 1 d U . . H38 H 0.3223 0.0107 0.8433 0.037 Uiso 1 1 calc R . . C39 C 0.3337(3) 0.0275(4) 0.7844(3) 0.048(2) Uani 1 1 d . . . H39 H 0.3349 -0.0238 0.7832 0.058 Uiso 1 1 calc R . . C40 C 0.2650(3) 0.0929(4) 0.7584(3) 0.038(2) Uani 1 1 d . . . C41 C 0.3992(2) 0.0470(4) 0.7630(3) 0.0370(19) Uani 1 1 d U . . H41A H 0.3924 0.0002 0.7499 0.044 Uiso 1 1 calc R . . H41B H 0.4325 0.0501 0.7817 0.044 Uiso 1 1 calc R . . C42 C 0.2838(2) 0.0438(4) 0.6984(2) 0.0293(16) Uani 1 1 d U . . H42A H 0.2946 -0.0021 0.6944 0.035 Uiso 1 1 calc R . . H42B H 0.2504 0.0449 0.6803 0.035 Uiso 1 1 calc R . . C43 C 0.4099(2) 0.1544(4) 0.7308(3) 0.0335(18) Uani 1 1 d U . . C44 C 0.3487(2) 0.0882(3) 0.6820(2) 0.0277(16) Uani 1 1 d . . . H44 H 0.3514 0.0449 0.6669 0.033 Uiso 1 1 calc R . . C45 C 0.3535(3) 0.1547(4) 0.6563(3) 0.043(2) Uani 1 1 d U . . H45 H 0.3580 0.1429 0.6288 0.051 Uiso 1 1 calc R . . C46 C 0.2820(2) 0.1530(4) 0.6567(2) 0.0314(18) Uani 1 1 d . . . C47 C 0.4115(2) 0.2489(5) 0.6816(2) 0.0416(14) Uani 1 1 d U . . H47A H 0.4078 0.2477 0.6499 0.050 Uiso 1 1 calc R . . H47B H 0.4445 0.2493 0.7019 0.050 Uiso 1 1 calc R . . C48 C 0.2952(2) 0.2495(4) 0.6174(2) 0.0396(15) Uani 1 1 d . . . H48A H 0.3076 0.2496 0.5947 0.047 Uiso 1 1 calc R . . H48B H 0.2616 0.2484 0.6006 0.047 Uiso 1 1 calc R . . C49 C 0.4093(3) 0.3438(5) 0.7296(4) 0.049(2) Uani 1 1 d . . . C50 C 0.3513(2) 0.3479(4) 0.6556(2) 0.0296(17) Uani 1 1 d . . . H50 H 0.3552 0.3605 0.6279 0.036 Uiso 1 1 calc R . . C51 C 0.3496(3) 0.4122(4) 0.6821(3) 0.045(2) Uani 1 1 d . . . H51 H 0.3524 0.4553 0.6668 0.054 Uiso 1 1 calc R . . C52 C 0.2815(3) 0.3485(3) 0.6586(3) 0.036(2) Uani 1 1 d . . . C53 C 0.3981(3) 0.4543(4) 0.7622(3) 0.0387(19) Uani 1 1 d U . . H53A H 0.3908 0.5009 0.7487 0.046 Uiso 1 1 calc R . . H53B H 0.4314 0.4522 0.7811 0.046 Uiso 1 1 calc R . . C54 C 0.2836(3) 0.4556(4) 0.6980(3) 0.056(3) Uani 1 1 d . . . H54A H 0.2502 0.4526 0.6800 0.067 Uiso 1 1 calc R . . H54B H 0.2931 0.5020 0.6932 0.067 Uiso 1 1 calc R . . C55 C 0.3929(3) 0.4071(4) 0.8279(3) 0.046(2) Uani 1 1 d U . . C56 C 0.3328(2) 0.4754(3) 0.7837(2) 0.0259(16) Uani 1 1 d U . . H56 H 0.3338 0.5268 0.7827 0.031 Uiso 1 1 calc R . . C57 C 0.3273(3) 0.4496(4) 0.8250(3) 0.040(2) Uani 1 1 d . . . H57 H 0.3234 0.4890 0.8427 0.048 Uiso 1 1 calc R . . C58 C 0.2672(3) 0.4115(3) 0.7598(2) 0.0323(18) Uani 1 1 d U . . C59 C 0.3785(3) 0.3753(3) 0.8951(3) 0.0356(19) Uani 1 1 d . . . H59A H 0.4119 0.3720 0.9132 0.043 Uiso 1 1 calc R . . H59B H 0.3663 0.4026 0.9128 0.043 Uiso 1 1 calc R . . C60 C 0.2641(2) 0.3753(3) 0.8322(2) 0.0292(17) Uani 1 1 d . . . H60A H 0.2705 0.4042 0.8593 0.035 Uiso 1 1 calc R . . H60B H 0.2309 0.3757 0.8133 0.035 Uiso 1 1 calc R . . N1 N 0.5407(2) 0.0553(3) 1.1259(2) 0.0327(15) Uani 1 1 d . . . N2 N 0.60283(19) 0.0881(3) 1.1181(2) 0.0322(14) Uani 1 1 d U . . N3 N 0.4960(2) 0.0520(3) 1.0438(2) 0.0382(16) Uani 1 1 d . . . N4 N 0.5567(2) 0.0919(3) 1.0366(2) 0.0394(17) Uani 1 1 d U . . N5 N 0.6380(2) 0.1920(3) 1.1097(2) 0.0328(15) Uani 1 1 d U . . N6 N 0.6387(2) 0.3059(3) 1.1102(2) 0.0394(17) Uani 1 1 d . . . N7 N 0.5966(2) 0.1936(3) 1.0273(2) 0.0413(18) Uani 1 1 d . . . N8 N 0.59668(19) 0.3066(3) 1.0274(2) 0.0310(15) Uani 1 1 d U . . N9 N 0.6017(2) 0.4115(3) 1.1184(2) 0.0394(17) Uani 1 1 d . . . N10 N 0.5426(2) 0.4437(3) 1.1273(2) 0.0379(16) Uani 1 1 d . . . N11 N 0.5555(2) 0.4078(3) 1.0353(2) 0.0370(16) Uani 1 1 d . . . N12 N 0.4961(2) 0.4475(3) 1.0440(2) 0.0374(16) Uani 1 1 d . . . N13 N 0.4771(2) 0.4054(3) 1.1369(2) 0.0387(16) Uani 1 1 d . . . N14 N 0.4399(2) 0.3124(3) 1.1423(2) 0.0407(17) Uani 1 1 d . . . N15 N 0.4305(2) 0.4045(3) 1.0540(2) 0.0411(17) Uani 1 1 d . . . N16 N 0.3952(2) 0.3134(3) 1.0594(2) 0.0394(17) Uani 1 1 d . . . N17 N 0.4399(2) 0.1879(3) 1.1415(2) 0.0356(16) Uani 1 1 d . . . N18 N 0.4763(2) 0.0965(3) 1.1358(2) 0.0371(16) Uani 1 1 d U . . N19 N 0.3937(2) 0.1875(3) 1.0600(2) 0.0381(17) Uani 1 1 d . . . N20 N 0.4315(2) 0.0941(3) 1.0551(2) 0.0371(16) Uani 1 1 d . . . N21 N 0.3592(2) 0.3073(3) 0.8879(2) 0.0343(16) Uani 1 1 d . . . N22 N 0.3597(2) 0.1931(3) 0.8883(2) 0.0380(16) Uani 1 1 d . . . N23 N 0.2780(2) 0.3057(3) 0.8472(2) 0.0376(16) Uani 1 1 d U . . N24 N 0.2774(2) 0.1928(3) 0.8466(2) 0.0352(16) Uani 1 1 d . . . N25 N 0.36833(19) 0.0877(3) 0.8519(2) 0.0319(15) Uani 1 1 d . . . N26 N 0.3768(2) 0.0565(3) 0.7921(2) 0.0374(16) Uani 1 1 d . . . N27 N 0.2852(2) 0.0927(3) 0.8060(2) 0.0414(17) Uani 1 1 d . . . N28 N 0.2943(2) 0.0529(3) 0.7468(2) 0.0435(18) Uani 1 1 d . . . N29 N 0.3862(2) 0.0963(3) 0.7264(2) 0.0381(16) Uani 1 1 d U . . N30 N 0.3920(2) 0.1881(3) 0.6902(2) 0.0351(16) Uani 1 1 d . . . N31 N 0.3039(2) 0.0954(3) 0.6806(2) 0.0404(16) Uani 1 1 d U . . N32 N 0.3104(2) 0.1874(3) 0.6449(2) 0.0386(16) Uani 1 1 d . . . N33 N 0.3910(2) 0.3133(3) 0.6886(2) 0.0423(18) Uani 1 1 d . . . N34 N 0.3861(2) 0.4052(3) 0.7264(2) 0.0371(16) Uani 1 1 d . . . N35 N 0.3086(2) 0.3125(3) 0.6436(2) 0.0366(16) Uani 1 1 d . . . N36 N 0.3044(2) 0.4057(3) 0.6807(2) 0.0352(16) Uani 1 1 d . . . N37 N 0.3756(2) 0.4446(3) 0.7909(2) 0.0411(17) Uani 1 1 d U . . N38 N 0.3686(2) 0.4108(3) 0.8526(2) 0.0374(16) Uani 1 1 d . . . N39 N 0.29430(18) 0.4481(3) 0.7462(2) 0.0349(16) Uani 1 1 d U . . N40 N 0.2864(2) 0.4076(3) 0.8058(2) 0.0335(15) Uani 1 1 d . . . O1 O 0.59377(16) 0.1260(3) 1.18036(17) 0.0359(13) Uani 1 1 d . . . O2 O 0.64002(13) 0.2495(3) 1.17187(14) 0.0369(9) Uani 1 1 d . . . O3 O 0.59431(19) 0.3726(3) 1.18139(18) 0.0448(14) Uani 1 1 d . . . O4 O 0.51510(18) 0.3260(3) 1.19212(19) 0.0410(14) Uani 1 1 d . . . O5 O 0.51509(19) 0.1754(3) 1.19278(19) 0.0460(15) Uani 1 1 d . . . O6 O 0.48511(18) 0.1144(3) 0.9806(2) 0.0463(15) Uani 1 1 d . . . O7 O 0.53804(14) 0.2507(3) 0.96978(15) 0.0403(10) Uani 1 1 d . . . O8 O 0.48320(17) 0.3844(3) 0.97933(18) 0.0379(13) Uani 1 1 d . . . O9 O 0.40029(18) 0.3317(3) 0.99199(18) 0.0422(14) Uani 1 1 d . . . O10 O 0.39954(18) 0.1679(2) 0.99369(19) 0.0423(14) Uani 1 1 d . . . O11 O 0.42188(13) 0.2508(3) 0.89017(13) 0.0365(9) Uani 1 1 d . . . O12 O 0.43100(15) 0.1265(2) 0.84391(17) 0.0356(13) Uani 1 1 d . . . O13 O 0.44268(16) 0.1751(3) 0.76534(18) 0.0389(13) Uani 1 1 d . . . O14 O 0.4419(2) 0.3253(3) 0.7643(2) 0.0461(15) Uani 1 1 d . . . O15 O 0.43027(19) 0.3743(3) 0.84402(18) 0.0466(15) Uani 1 1 d . . . O16 O 0.21985(14) 0.2496(3) 0.78788(15) 0.0417(10) Uani 1 1 d . . . O17 O 0.22926(16) 0.1153(2) 0.73414(18) 0.0371(13) Uani 1 1 d . . . O18 O 0.24315(16) 0.1671(2) 0.65019(18) 0.0368(13) Uani 1 1 d . . . O19 O 0.24292(19) 0.3312(3) 0.6500(2) 0.0465(15) Uani 1 1 d . . . O20 O 0.23073(19) 0.3851(3) 0.73419(19) 0.0456(14) 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 Cl3 0.106(2) 0.0504(16) 0.103(2) 0.0214(15) 0.081(2) 0.0230(14) Cl4 0.095(2) 0.0555(16) 0.095(2) -0.0166(15) 0.0696(18) -0.0143(14) Cl5 0.168(3) 0.083(2) 0.223(5) -0.008(3) 0.156(4) 0.006(2) Cl6 0.285(6) 0.077(3) 0.242(5) -0.001(3) 0.207(5) -0.021(3) Cl7 0.221(4) 0.099(3) 0.189(4) 0.006(3) 0.164(4) -0.004(3) Cl8 0.225(4) 0.0575(19) 0.261(5) -0.020(3) 0.190(4) 0.003(2) O1W 0.070(3) 0.134(6) 0.043(3) -0.008(5) 0.030(3) 0.001(5) O2W 0.049(3) 0.120(5) 0.063(3) 0.000(5) 0.029(3) -0.001(5) Cl1 0.0570(9) 0.0490(9) 0.0460(10) -0.0014(13) 0.0259(8) -0.0028(13) Cl2 0.0493(9) 0.0473(9) 0.0542(10) -0.0046(14) 0.0258(8) -0.0019(12) Ca1 0.0464(7) 0.0349(7) 0.0427(7) 0.0017(10) 0.0260(6) 0.0034(9) Ca2 0.0595(8) 0.0323(7) 0.0536(9) -0.0011(11) 0.0322(7) 0.0007(10) Ca3 0.0437(7) 0.0358(7) 0.0449(8) -0.0017(10) 0.0264(6) 0.0019(9) Ca4 0.0544(8) 0.0329(7) 0.0571(9) -0.0012(11) 0.0328(7) 0.0013(10) C1 0.063(5) 0.007(3) 0.036(5) 0.000(3) 0.015(4) 0.009(3) C2 0.057(5) 0.021(4) 0.053(6) -0.010(4) 0.045(5) -0.009(4) C3 0.058(5) 0.010(3) 0.051(5) 0.001(3) 0.032(4) 0.002(3) C4 0.073(6) 0.020(4) 0.026(5) -0.002(3) 0.028(4) 0.004(4) C5 0.035(4) 0.015(3) 0.035(4) 0.004(3) 0.020(3) 0.005(2) C6 0.069(5) 0.011(3) 0.078(6) -0.014(3) 0.063(5) -0.010(3) C7 0.028(3) 0.035(3) 0.044(4) 0.022(5) 0.016(3) -0.001(4) C8 0.051(5) 0.017(4) 0.067(6) -0.001(3) 0.044(4) 0.002(3) C9 0.033(2) 0.033(2) 0.033(2) 0.0008(10) 0.0145(12) 0.0001(10) C10 0.044(3) 0.029(3) 0.031(3) 0.005(4) 0.023(3) -0.001(4) C11 0.044(2) 0.044(2) 0.044(2) -0.0001(10) 0.0192(13) -0.0001(10) C12 0.037(2) 0.037(2) 0.037(2) 0.0006(10) 0.0163(12) -0.0002(10) C13 0.037(4) 0.039(5) 0.050(5) -0.011(4) 0.034(4) -0.001(4) C14 0.038(2) 0.038(2) 0.038(2) 0.0000(10) 0.0169(12) 0.0001(10) C15 0.044(5) 0.016(4) 0.035(5) -0.007(3) 0.008(4) -0.009(3) C16 0.031(4) 0.014(4) 0.073(6) 0.006(4) 0.026(4) 0.002(3) C17 0.0318(19) 0.0290(19) 0.0314(19) -0.0011(10) 0.0142(11) 0.0003(10) C18 0.049(5) 0.035(5) 0.056(6) 0.003(4) 0.041(5) -0.005(4) C19 0.043(5) 0.052(6) 0.060(6) -0.032(5) 0.038(5) -0.009(4) C20 0.041(2) 0.041(2) 0.041(2) 0.0001(10) 0.0181(12) 0.0000(10) C21 0.036(4) 0.035(5) 0.060(6) 0.000(4) 0.030(4) 0.000(4) C22 0.0289(18) 0.0277(19) 0.0290(19) 0.0000(10) 0.0128(11) 0.0007(10) C23 0.064(4) 0.034(3) 0.059(4) 0.008(5) 0.054(4) 0.012(5) C24 0.050(3) 0.027(3) 0.050(4) -0.001(5) 0.031(3) 0.015(4) C25 0.047(5) 0.034(4) 0.038(5) -0.015(4) 0.026(4) -0.010(4) C26 0.062(5) 0.032(4) 0.041(5) 0.002(4) 0.037(4) -0.012(4) C27 0.060(5) 0.014(3) 0.055(5) 0.008(3) 0.051(4) 0.002(3) C28 0.037(2) 0.036(2) 0.037(2) 0.0009(10) 0.0167(12) -0.0011(10) C29 0.044(2) 0.042(2) 0.044(2) 0.0010(10) 0.0197(13) -0.0007(10) C30 0.050(5) 0.031(4) 0.037(5) -0.016(4) 0.019(4) -0.019(4) C31 0.048(3) 0.023(3) 0.029(3) -0.013(4) 0.021(3) -0.014(4) C32 0.034(2) 0.032(2) 0.033(2) -0.0002(10) 0.0152(12) 0.0007(10) C33 0.036(2) 0.034(2) 0.034(2) 0.0005(10) 0.0161(12) -0.0008(10) C34 0.036(3) 0.028(3) 0.042(4) 0.014(4) 0.024(3) 0.012(4) C35 0.036(2) 0.036(2) 0.036(2) 0.0004(10) 0.0157(12) -0.0002(10) C36 0.066(6) 0.019(4) 0.082(7) -0.018(4) 0.050(5) -0.022(4) C37 0.0267(18) 0.0253(18) 0.0268(18) 0.0001(10) 0.0121(11) 0.0007(10) C38 0.0317(19) 0.031(2) 0.031(2) -0.0004(10) 0.0139(12) 0.0004(10) C39 0.067(6) 0.020(4) 0.058(6) 0.016(4) 0.028(5) 0.010(4) C40 0.039(5) 0.017(4) 0.066(6) -0.007(4) 0.031(5) 0.000(3) C41 0.038(2) 0.036(2) 0.038(2) -0.0011(10) 0.0176(12) 0.0014(10) C42 0.0291(18) 0.0289(19) 0.0297(19) 0.0000(10) 0.0127(11) -0.0010(10) C43 0.034(2) 0.034(2) 0.033(2) 0.0006(10) 0.0153(12) -0.0003(10) C44 0.034(4) 0.023(4) 0.027(4) -0.006(3) 0.013(3) 0.005(3) C45 0.043(2) 0.043(2) 0.043(2) -0.0002(10) 0.0195(13) 0.0002(10) C46 0.035(4) 0.035(4) 0.024(4) -0.008(3) 0.012(3) 0.001(3) C47 0.0428(16) 0.0429(17) 0.0420(17) -0.0001(10) 0.0213(11) 0.0003(10) C48 0.055(4) 0.029(3) 0.049(4) -0.018(5) 0.037(3) -0.005(5) C49 0.050(5) 0.044(5) 0.067(6) 0.007(4) 0.040(5) -0.012(4) C50 0.039(4) 0.034(4) 0.031(4) 0.008(3) 0.029(3) -0.001(3) C51 0.070(6) 0.029(4) 0.069(7) -0.003(4) 0.061(5) -0.001(4) C52 0.067(6) 0.015(4) 0.043(5) 0.003(3) 0.040(5) 0.009(4) C53 0.040(2) 0.038(2) 0.039(2) 0.0008(10) 0.0181(12) -0.0014(10) C54 0.095(7) 0.021(4) 0.080(7) 0.016(4) 0.065(6) 0.014(4) C55 0.047(2) 0.045(2) 0.047(2) -0.0006(10) 0.0205(13) -0.0002(10) C56 0.033(4) 0.015(3) 0.043(5) 0.009(3) 0.029(4) 0.008(3) C57 0.057(5) 0.013(3) 0.063(5) -0.006(3) 0.039(4) -0.006(3) C58 0.051(5) 0.014(4) 0.028(4) -0.010(3) 0.014(4) 0.007(3) C59 0.066(5) 0.012(3) 0.042(4) 0.000(3) 0.036(4) -0.004(3) C60 0.036(4) 0.029(4) 0.028(4) -0.004(3) 0.019(3) -0.005(3) N1 0.050(4) 0.013(3) 0.046(4) -0.006(3) 0.030(3) -0.010(3) N2 0.0325(16) 0.0328(17) 0.0324(17) 0.0000(10) 0.0151(11) 0.0000(10) N3 0.039(4) 0.038(4) 0.036(4) 0.017(3) 0.015(3) 0.007(3) N4 0.044(4) 0.019(3) 0.060(5) -0.004(3) 0.026(4) -0.002(3) N5 0.043(4) 0.027(4) 0.037(4) -0.003(3) 0.026(3) -0.004(3) N6 0.055(4) 0.024(3) 0.054(5) -0.008(3) 0.037(4) -0.010(3) N7 0.070(4) 0.019(3) 0.053(4) 0.004(3) 0.043(4) 0.003(3) N8 0.0316(17) 0.0308(17) 0.0310(17) 0.0001(10) 0.0140(11) -0.0009(10) N9 0.054(4) 0.021(3) 0.057(4) -0.002(3) 0.037(3) 0.003(3) N10 0.041(4) 0.030(4) 0.048(4) -0.004(3) 0.025(3) -0.005(3) N11 0.055(4) 0.026(3) 0.050(4) -0.014(3) 0.042(4) -0.011(3) N12 0.047(4) 0.024(3) 0.053(5) 0.009(3) 0.033(4) 0.002(3) N13 0.058(4) 0.022(3) 0.043(4) 0.000(3) 0.029(4) 0.005(3) N14 0.049(4) 0.040(4) 0.053(5) -0.008(3) 0.041(4) 0.004(3) N15 0.057(4) 0.039(4) 0.035(4) 0.005(3) 0.026(3) -0.003(3) N16 0.059(4) 0.026(3) 0.030(4) -0.006(3) 0.016(3) -0.005(3) N17 0.040(4) 0.027(3) 0.042(4) -0.012(3) 0.021(3) 0.000(3) N18 0.042(4) 0.026(3) 0.043(4) -0.002(3) 0.019(3) 0.008(3) N19 0.051(4) 0.023(3) 0.063(5) -0.002(3) 0.047(4) 0.006(3) N20 0.059(4) 0.013(3) 0.053(4) 0.011(3) 0.038(4) 0.001(3) N21 0.047(4) 0.013(3) 0.063(5) -0.009(3) 0.042(4) -0.005(3) N22 0.054(4) 0.030(4) 0.031(4) 0.001(3) 0.020(3) -0.002(3) N23 0.051(4) 0.019(3) 0.055(5) -0.009(3) 0.034(4) -0.009(3) N24 0.044(4) 0.030(4) 0.043(4) -0.003(3) 0.028(3) 0.001(3) N25 0.037(3) 0.031(3) 0.034(4) -0.010(3) 0.021(3) 0.002(3) N26 0.035(3) 0.037(4) 0.047(4) 0.010(3) 0.025(3) -0.003(3) N27 0.040(4) 0.036(4) 0.054(5) 0.017(3) 0.025(3) 0.013(3) N28 0.066(5) 0.020(3) 0.038(4) 0.006(3) 0.017(4) -0.015(3) N29 0.044(4) 0.033(4) 0.048(4) 0.011(3) 0.031(3) 0.002(3) N30 0.044(4) 0.032(4) 0.035(4) -0.011(3) 0.023(3) -0.017(3) N31 0.0403(18) 0.0405(19) 0.0407(18) 0.0002(10) 0.0182(11) 0.0003(10) N32 0.045(4) 0.034(4) 0.049(5) 0.006(3) 0.032(4) 0.001(3) N33 0.061(5) 0.037(4) 0.046(5) -0.013(3) 0.039(4) -0.020(3) N34 0.052(4) 0.017(3) 0.047(4) 0.001(3) 0.026(4) -0.003(3) N35 0.043(4) 0.022(3) 0.049(4) -0.004(3) 0.023(3) -0.005(3) N36 0.052(4) 0.011(3) 0.062(4) -0.010(3) 0.044(3) -0.005(2) N37 0.069(5) 0.018(3) 0.050(5) 0.012(3) 0.038(4) 0.004(3) N38 0.053(4) 0.028(3) 0.044(4) -0.005(3) 0.033(3) 0.008(3) N39 0.025(3) 0.044(4) 0.043(4) 0.011(3) 0.022(3) -0.010(3) N40 0.054(4) 0.014(3) 0.044(4) 0.008(3) 0.032(3) 0.003(3) O1 0.041(3) 0.032(3) 0.042(3) 0.012(3) 0.024(3) 0.002(2) O2 0.043(2) 0.032(2) 0.044(3) 0.011(3) 0.027(2) 0.003(3) O3 0.062(4) 0.035(3) 0.035(3) 0.012(3) 0.019(3) -0.005(3) O4 0.047(3) 0.034(3) 0.050(4) -0.004(3) 0.028(3) -0.005(3) O5 0.050(4) 0.050(4) 0.043(4) 0.001(3) 0.025(3) -0.007(3) O6 0.052(3) 0.036(3) 0.061(4) -0.010(3) 0.034(3) -0.002(3) O7 0.052(2) 0.031(2) 0.043(3) 0.000(3) 0.025(2) 0.005(3) O8 0.045(3) 0.029(3) 0.039(3) -0.008(3) 0.017(3) -0.007(2) O9 0.060(4) 0.038(3) 0.040(3) 0.001(3) 0.033(3) 0.010(3) O10 0.057(3) 0.020(3) 0.056(4) -0.002(3) 0.030(3) 0.012(2) O11 0.043(2) 0.034(2) 0.040(2) 0.000(3) 0.025(2) -0.005(3) O12 0.032(3) 0.027(3) 0.046(3) 0.004(2) 0.016(2) 0.000(2) O13 0.037(3) 0.039(3) 0.046(4) -0.004(3) 0.024(3) -0.004(2) O14 0.063(4) 0.039(3) 0.045(4) -0.008(3) 0.032(3) -0.011(3) O15 0.057(4) 0.043(3) 0.046(4) -0.003(3) 0.028(3) -0.005(3) O16 0.044(2) 0.034(2) 0.055(3) -0.002(4) 0.029(2) 0.002(3) O17 0.038(3) 0.027(3) 0.053(4) 0.010(3) 0.026(3) 0.012(2) O18 0.039(3) 0.030(3) 0.052(4) -0.011(3) 0.030(3) -0.001(2) O19 0.055(4) 0.027(3) 0.065(4) -0.013(3) 0.033(3) -0.001(3) O20 0.056(4) 0.038(3) 0.048(4) 0.003(3) 0.028(3) 0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1W Ca1 2.343(5) . ? O2W Ca3 2.339(5) . ? Cl1 Ca1 2.708(2) . ? Cl1 Ca2 3.196(2) . ? Cl2 Ca3 2.711(2) . ? Cl2 Ca4 3.192(2) . ? Ca1 O2 2.429(4) . ? Ca1 O5 2.474(6) . ? Ca1 O4 2.480(5) . ? Ca1 O3 2.507(6) . ? Ca1 O1 2.533(5) . ? Ca2 O7 2.689(4) . ? Ca2 O9 2.701(5) . ? Ca2 O8 2.712(5) . ? Ca2 O10 2.756(6) . ? Ca2 O6 2.755(6) . ? Ca2 O11 2.842(4) . ? Ca2 C31 3.137(6) . ? Ca3 O11 2.437(4) . ? Ca3 O13 2.466(5) . ? Ca3 O14 2.489(6) . ? Ca3 O12 2.519(5) . ? Ca3 O15 2.543(6) . ? Ca4 O16 2.685(4) . ? Ca4 O19 2.716(6) . ? Ca4 O20 2.729(6) . ? Ca4 O17 2.733(5) . ? Ca4 O18 2.737(5) . ? Ca4 O2 2.842(4) 8_455 ? Ca4 C7 3.148(6) 8_455 ? C1 O1 1.273(8) . ? C1 N1 1.338(9) . ? C1 N2 1.366(10) . ? C2 N3 1.427(10) . ? C2 N1 1.452(9) . ? C2 C3 1.524(10) . ? C2 H2 1.0000 . ? C3 N4 1.432(9) . ? C3 N2 1.450(9) . ? C3 H3 1.0000 . ? C4 O6 1.212(9) . ? C4 N3 1.358(9) . ? C4 N4 1.380(10) . ? C5 N2 1.436(8) . ? C5 N5 1.441(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N7 1.452(9) . ? C6 N4 1.467(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O2 1.223(7) . ? C7 N5 1.349(10) . ? C7 N6 1.361(9) . ? C7 Ca4 3.148(6) 8_556 ? C8 N7 1.444(10) . ? C8 N5 1.476(10) . ? C8 C9 1.564(8) . ? C8 H8 1.0000 . ? C9 N8 1.423(9) . ? C9 N6 1.453(9) . ? C9 H9 1.0000 . ? C10 O7 1.233(7) . ? C10 N8 1.340(9) . ? C10 N7 1.360(9) . ? C11 N6 1.467(10) . ? C11 N9 1.474(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N8 1.450(9) . ? C12 N11 1.475(9) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O3 1.162(9) . ? C13 N10 1.386(9) . ? C13 N9 1.398(9) . ? C14 N9 1.441(9) . ? C14 N11 1.450(9) . ? C14 C15 1.568(10) . ? C14 H14 1.0000 . ? C15 N10 1.439(9) . ? C15 N12 1.450(9) . ? C15 H15 1.0000 . ? C16 O8 1.189(9) . ? C16 N11 1.372(9) . ? C16 N12 1.422(10) . ? C17 N13 1.427(9) . ? C17 N10 1.433(9) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N12 1.446(9) . ? C18 N15 1.462(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 O4 1.250(10) . ? C19 N13 1.331(11) . ? C19 N14 1.360(10) . ? C20 N13 1.442(9) . ? C20 N15 1.458(9) . ? C20 C21 1.568(10) . ? C20 H20 1.0000 . ? C21 N14 1.439(10) . ? C21 N16 1.450(9) . ? C21 H21 1.0000 . ? C22 O9 1.194(8) . ? C22 N16 1.359(9) . ? C22 N15 1.393(9) . ? C23 N17 1.453(9) . ? C23 N14 1.460(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N19 1.468(9) . ? C24 N16 1.474(10) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O5 1.229(9) . ? C25 N17 1.349(9) . ? C25 N18 1.373(9) . ? C26 N17 1.417(9) . ? C26 N19 1.452(9) . ? C26 C27 1.544(10) . ? C26 H26 1.0000 . ? C27 N20 1.433(9) . ? C27 N18 1.437(9) . ? C27 H27 1.0000 . ? C28 O10 1.281(9) . ? C28 N19 1.334(9) . ? C28 N20 1.345(9) . ? C29 N1 1.443(9) . ? C29 N18 1.443(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 N20 1.439(9) . ? C30 N3 1.456(9) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 O11 1.208(7) . ? C31 N21 1.364(9) . ? C31 N22 1.379(9) . ? C32 N21 1.409(9) . ? C32 N23 1.429(9) . ? C32 C33 1.579(8) . ? C32 H32 1.0000 . ? C33 N24 1.426(9) . ? C33 N22 1.475(9) . ? C33 H33 1.0000 . ? C34 O16 1.249(7) . ? C34 N23 1.328(10) . ? C34 N24 1.367(9) . ? C35 N22 1.432(9) . ? C35 N25 1.458(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 N27 1.445(10) . ? C36 N24 1.474(9) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 O12 1.197(7) . ? C37 N25 1.352(8) . ? C37 N26 1.384(9) . ? C38 N27 1.456(8) . ? C38 N25 1.458(8) . ? C38 C39 1.557(11) . ? C38 H38 1.0000 . ? C39 N28 1.427(10) . ? C39 N26 1.436(10) . ? C39 H39 1.0000 . ? C40 O17 1.174(8) . ? C40 N27 1.401(10) . ? C40 N28 1.409(10) . ? C41 N26 1.444(9) . ? C41 N29 1.446(9) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 N31 1.453(9) . ? C42 N28 1.478(9) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 O13 1.238(8) . ? C43 N29 1.343(9) . ? C43 N30 1.363(9) . ? C44 N29 1.443(9) . ? C44 N31 1.453(9) . ? C44 C45 1.587(10) . ? C44 H44 1.0000 . ? C45 N30 1.420(9) . ? C45 N32 1.440(10) . ? C45 H45 1.0000 . ? C46 O18 1.224(8) . ? C46 N32 1.333(9) . ? C46 N31 1.375(9) . ? C47 N30 1.428(9) . ? C47 N33 1.484(10) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 N35 1.451(9) . ? C48 N32 1.457(10) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 O14 1.226(10) . ? C49 N33 1.345(11) . ? C49 N34 1.395(10) . ? C50 N33 1.443(10) . ? C50 N35 1.448(9) . ? C50 C51 1.536(10) . ? C50 H50 1.0000 . ? C51 N34 1.427(10) . ? C51 N36 1.463(9) . ? C51 H51 1.0000 . ? C52 O19 1.214(9) . ? C52 N36 1.360(9) . ? C52 N35 1.378(9) . ? C53 N34 1.428(9) . ? C53 N37 1.438(9) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 N36 1.437(9) . ? C54 N39 1.468(10) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 O15 1.273(9) . ? C55 N37 1.310(10) . ? C55 N38 1.361(10) . ? C56 N39 1.422(9) . ? C56 N37 1.447(8) . ? C56 C57 1.526(10) . ? C56 H56 1.0000 . ? C57 N40 1.456(9) . ? C57 N38 1.466(9) . ? C57 H57 1.0000 . ? C58 O20 1.231(8) . ? C58 N39 1.354(9) . ? C58 N40 1.357(9) . ? C59 N21 1.441(8) . ? C59 N38 1.457(9) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 N23 1.443(9) . ? C60 N40 1.493(8) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? O2 Ca4 2.842(4) 8_556 ? 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 Ca1 Cl1 Ca2 179.69(8) . . ? Ca3 Cl2 Ca4 179.57(9) . . ? O1W Ca1 O2 84.72(17) . . ? O1W Ca1 O5 97.5(2) . . ? O2 Ca1 O5 143.7(2) . . ? O1W Ca1 O4 97.4(2) . . ? O2 Ca1 O4 143.5(2) . . ? O5 Ca1 O4 72.47(15) . . ? O1W Ca1 O3 88.0(3) . . ? O2 Ca1 O3 72.3(2) . . ? O5 Ca1 O3 143.8(2) . . ? O4 Ca1 O3 71.35(18) . . ? O1W Ca1 O1 89.4(2) . . ? O2 Ca1 O1 71.93(18) . . ? O5 Ca1 O1 71.85(18) . . ? O4 Ca1 O1 144.25(17) . . ? O3 Ca1 O1 144.21(15) . . ? O1W Ca1 Cl1 171.94(15) . . ? O2 Ca1 Cl1 87.24(11) . . ? O5 Ca1 Cl1 89.24(14) . . ? O4 Ca1 Cl1 88.74(14) . . ? O3 Ca1 Cl1 89.12(14) . . ? O1 Ca1 Cl1 88.57(14) . . ? O7 Ca2 O9 143.46(19) . . ? O7 Ca2 O8 74.04(17) . . ? O9 Ca2 O8 69.69(16) . . ? O7 Ca2 O10 144.21(17) . . ? O9 Ca2 O10 71.47(13) . . ? O8 Ca2 O10 141.08(16) . . ? O7 Ca2 O6 73.81(17) . . ? O9 Ca2 O6 141.97(17) . . ? O8 Ca2 O6 147.75(14) . . ? O10 Ca2 O6 70.64(15) . . ? O7 Ca2 O11 79.75(13) . . ? O9 Ca2 O11 92.90(15) . . ? O8 Ca2 O11 85.37(17) . . ? O10 Ca2 O11 94.08(16) . . ? O6 Ca2 O11 86.58(18) . . ? O7 Ca2 C31 102.37(15) . . ? O9 Ca2 C31 74.65(17) . . ? O8 Ca2 C31 91.49(19) . . ? O10 Ca2 C31 75.78(17) . . ? O6 Ca2 C31 92.9(2) . . ? O11 Ca2 C31 22.62(12) . . ? O7 Ca2 Cl1 94.04(11) . . ? O9 Ca2 Cl1 92.06(13) . . ? O8 Ca2 Cl1 92.85(13) . . ? O10 Ca2 Cl1 91.04(13) . . ? O6 Ca2 Cl1 91.81(14) . . ? O11 Ca2 Cl1 173.79(10) . . ? C31 Ca2 Cl1 163.59(12) . . ? O2W Ca3 O11 84.64(17) . . ? O2W Ca3 O13 97.3(2) . . ? O11 Ca3 O13 144.1(2) . . ? O2W Ca3 O14 97.8(2) . . ? O11 Ca3 O14 143.3(2) . . ? O13 Ca3 O14 72.18(14) . . ? O2W Ca3 O12 88.7(2) . . ? O11 Ca3 O12 72.60(19) . . ? O13 Ca3 O12 71.64(17) . . ? O14 Ca3 O12 143.76(18) . . ? O2W Ca3 O15 88.9(3) . . ? O11 Ca3 O15 71.58(19) . . ? O13 Ca3 O15 144.03(18) . . ? O14 Ca3 O15 71.89(18) . . ? O12 Ca3 O15 144.16(15) . . ? O2W Ca3 Cl2 172.03(15) . . ? O11 Ca3 Cl2 87.39(11) . . ? O13 Ca3 Cl2 89.19(13) . . ? O14 Ca3 Cl2 88.48(15) . . ? O12 Ca3 Cl2 89.08(13) . . ? O15 Ca3 Cl2 88.43(14) . . ? O16 Ca4 O19 144.32(18) . . ? O16 Ca4 O20 74.38(17) . . ? O19 Ca4 O20 70.21(16) . . ? O16 Ca4 O17 73.37(17) . . ? O19 Ca4 O17 141.58(16) . . ? O20 Ca4 O17 147.66(14) . . ? O16 Ca4 O18 143.28(18) . . ? O19 Ca4 O18 71.64(12) . . ? O20 Ca4 O18 141.79(17) . . ? O17 Ca4 O18 70.09(16) . . ? O16 Ca4 O2 79.79(13) . 8_455 ? O19 Ca4 O2 93.54(16) . 8_455 ? O20 Ca4 O2 86.30(17) . 8_455 ? O17 Ca4 O2 85.76(16) . 8_455 ? O18 Ca4 O2 93.88(14) . 8_455 ? O16 Ca4 C7 102.63(15) . 8_455 ? O19 Ca4 C7 74.8(2) . 8_455 ? O20 Ca4 C7 92.2(2) . 8_455 ? O17 Ca4 C7 92.5(2) . 8_455 ? O18 Ca4 C7 75.73(16) . 8_455 ? O2 Ca4 C7 22.84(13) 8_455 8_455 ? O16 Ca4 Cl2 93.96(11) . . ? O19 Ca4 Cl2 91.41(13) . . ? O20 Ca4 Cl2 91.80(13) . . ? O17 Ca4 Cl2 92.73(12) . . ? O18 Ca4 Cl2 91.30(12) . . ? O2 Ca4 Cl2 173.75(10) 8_455 . ? C7 Ca4 Cl2 163.40(13) 8_455 . ? O1 C1 N1 125.4(8) . . ? O1 C1 N2 121.9(7) . . ? N1 C1 N2 112.7(7) . . ? N3 C2 N1 115.6(6) . . ? N3 C2 C3 104.2(6) . . ? N1 C2 C3 103.2(6) . . ? N3 C2 H2 111.1 . . ? N1 C2 H2 111.1 . . ? C3 C2 H2 111.1 . . ? N4 C3 N2 114.5(5) . . ? N4 C3 C2 104.6(6) . . ? N2 C3 C2 105.8(6) . . ? N4 C3 H3 110.6 . . ? N2 C3 H3 110.6 . . ? C2 C3 H3 110.6 . . ? O6 C4 N3 125.4(8) . . ? O6 C4 N4 124.8(8) . . ? N3 C4 N4 109.5(7) . . ? N2 C5 N5 113.1(5) . . ? N2 C5 H5A 109.0 . . ? N5 C5 H5A 109.0 . . ? N2 C5 H5B 109.0 . . ? N5 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N7 C6 N4 114.9(6) . . ? N7 C6 H6A 108.5 . . ? N4 C6 H6A 108.5 . . ? N7 C6 H6B 108.5 . . ? N4 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? O2 C7 N5 126.5(8) . . ? O2 C7 N6 123.9(9) . . ? N5 C7 N6 109.6(5) . . ? O2 C7 Ca4 64.4(3) . 8_556 ? N5 C7 Ca4 104.0(4) . 8_556 ? N6 C7 Ca4 102.1(4) . 8_556 ? N7 C8 N5 113.0(6) . . ? N7 C8 C9 102.7(7) . . ? N5 C8 C9 103.5(7) . . ? N7 C8 H8 112.3 . . ? N5 C8 H8 112.3 . . ? C9 C8 H8 112.3 . . ? N8 C9 N6 116.5(6) . . ? N8 C9 C8 102.8(7) . . ? N6 C9 C8 102.1(7) . . ? N8 C9 H9 111.5 . . ? N6 C9 H9 111.5 . . ? C8 C9 H9 111.5 . . ? O7 C10 N8 126.0(8) . . ? O7 C10 N7 125.0(8) . . ? N8 C10 N7 109.0(5) . . ? N6 C11 N9 113.3(6) . . ? N6 C11 H11A 108.9 . . ? N9 C11 H11A 108.9 . . ? N6 C11 H11B 108.9 . . ? N9 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N8 C12 N11 114.7(6) . . ? N8 C12 H12A 108.6 . . ? N11 C12 H12A 108.6 . . ? N8 C12 H12B 108.6 . . ? N11 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? O3 C13 N10 128.9(7) . . ? O3 C13 N9 128.4(7) . . ? N10 C13 N9 102.6(7) . . ? N9 C14 N11 117.2(6) . . ? N9 C14 C15 101.4(6) . . ? N11 C14 C15 103.8(6) . . ? N9 C14 H14 111.2 . . ? N11 C14 H14 111.2 . . ? C15 C14 H14 111.2 . . ? N10 C15 N12 118.1(6) . . ? N10 C15 C14 102.8(6) . . ? N12 C15 C14 102.2(6) . . ? N10 C15 H15 111.0 . . ? N12 C15 H15 111.0 . . ? C14 C15 H15 111.0 . . ? O8 C16 N11 129.6(8) . . ? O8 C16 N12 125.1(7) . . ? N11 C16 N12 105.3(7) . . ? N13 C17 N10 115.3(6) . . ? N13 C17 H17A 108.4 . . ? N10 C17 H17A 108.4 . . ? N13 C17 H17B 108.4 . . ? N10 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? N12 C18 N15 115.4(6) . . ? N12 C18 H18A 108.4 . . ? N15 C18 H18A 108.4 . . ? N12 C18 H18B 108.4 . . ? N15 C18 H18B 108.4 . . ? H18A C18 H18B 107.5 . . ? O4 C19 N13 124.9(8) . . ? O4 C19 N14 123.3(9) . . ? N13 C19 N14 111.7(8) . . ? N13 C20 N15 116.3(6) . . ? N13 C20 C21 105.0(6) . . ? N15 C20 C21 102.8(6) . . ? N13 C20 H20 110.7 . . ? N15 C20 H20 110.7 . . ? C21 C20 H20 110.7 . . ? N14 C21 N16 116.4(6) . . ? N14 C21 C20 101.5(6) . . ? N16 C21 C20 100.7(6) . . ? N14 C21 H21 112.3 . . ? N16 C21 H21 112.3 . . ? C20 C21 H21 112.3 . . ? O9 C22 N16 129.7(7) . . ? O9 C22 N15 126.7(7) . . ? N16 C22 N15 103.5(6) . . ? N17 C23 N14 112.5(5) . . ? N17 C23 H23A 109.1 . . ? N14 C23 H23A 109.1 . . ? N17 C23 H23B 109.1 . . ? N14 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? N19 C24 N16 112.8(5) . . ? N19 C24 H24A 109.0 . . ? N16 C24 H24A 109.0 . . ? N19 C24 H24B 109.0 . . ? N16 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? O5 C25 N17 126.8(7) . . ? O5 C25 N18 125.9(8) . . ? N17 C25 N18 107.2(6) . . ? N17 C26 N19 115.4(6) . . ? N17 C26 C27 104.5(7) . . ? N19 C26 C27 103.6(6) . . ? N17 C26 H26 110.9 . . ? N19 C26 H26 110.9 . . ? C27 C26 H26 110.9 . . ? N20 C27 N18 113.2(6) . . ? N20 C27 C26 104.4(6) . . ? N18 C27 C26 101.7(6) . . ? N20 C27 H27 112.3 . . ? N18 C27 H27 112.3 . . ? C26 C27 H27 112.3 . . ? O10 C28 N19 122.7(7) . . ? O10 C28 N20 123.6(7) . . ? N19 C28 N20 113.6(7) . . ? N1 C29 N18 112.9(6) . . ? N1 C29 H29A 109.0 . . ? N18 C29 H29A 109.0 . . ? N1 C29 H29B 109.0 . . ? N18 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? N20 C30 N3 114.9(6) . . ? N20 C30 H30A 108.5 . . ? N3 C30 H30A 108.5 . . ? N20 C30 H30B 108.5 . . ? N3 C30 H30B 108.6 . . ? H30A C30 H30B 107.5 . . ? O11 C31 N21 126.6(7) . . ? O11 C31 N22 125.3(8) . . ? N21 C31 N22 108.1(5) . . ? O11 C31 Ca2 64.8(3) . . ? N21 C31 Ca2 104.5(4) . . ? N22 C31 Ca2 103.3(4) . . ? N21 C32 N23 115.3(7) . . ? N21 C32 C33 104.3(6) . . ? N23 C32 C33 99.8(6) . . ? N21 C32 H32 112.2 . . ? N23 C32 H32 112.2 . . ? C33 C32 H32 112.2 . . ? N24 C33 N22 113.9(6) . . ? N24 C33 C32 105.2(7) . . ? N22 C33 C32 101.4(6) . . ? N24 C33 H33 111.9 . . ? N22 C33 H33 111.9 . . ? C32 C33 H33 111.9 . . ? O16 C34 N23 127.8(8) . . ? O16 C34 N24 123.1(8) . . ? N23 C34 N24 109.0(5) . . ? N22 C35 N25 115.8(6) . . ? N22 C35 H35A 108.3 . . ? N25 C35 H35A 108.3 . . ? N22 C35 H35B 108.3 . . ? N25 C35 H35B 108.3 . . ? H35A C35 H35B 107.4 . . ? N27 C36 N24 112.9(6) . . ? N27 C36 H36A 109.0 . . ? N24 C36 H36A 109.0 . . ? N27 C36 H36B 109.0 . . ? N24 C36 H36B 109.0 . . ? H36A C36 H36B 107.8 . . ? O12 C37 N25 129.3(7) . . ? O12 C37 N26 125.0(6) . . ? N25 C37 N26 105.7(6) . . ? N27 C38 N25 115.9(6) . . ? N27 C38 C39 103.6(6) . . ? N25 C38 C39 100.1(6) . . ? N27 C38 H38 112.1 . . ? N25 C38 H38 112.1 . . ? C39 C38 H38 112.1 . . ? N28 C39 N26 117.6(7) . . ? N28 C39 C38 103.0(6) . . ? N26 C39 C38 104.8(7) . . ? N28 C39 H39 110.3 . . ? N26 C39 H39 110.3 . . ? C38 C39 H39 110.3 . . ? O17 C40 N27 126.9(7) . . ? O17 C40 N28 128.0(8) . . ? N27 C40 N28 104.7(7) . . ? N26 C41 N29 114.3(6) . . ? N26 C41 H41A 108.7 . . ? N29 C41 H41A 108.7 . . ? N26 C41 H41B 108.7 . . ? N29 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? N31 C42 N28 114.4(6) . . ? N31 C42 H42A 108.7 . . ? N28 C42 H42A 108.7 . . ? N31 C42 H42B 108.7 . . ? N28 C42 H42B 108.7 . . ? H42A C42 H42B 107.6 . . ? O13 C43 N29 126.9(7) . . ? O13 C43 N30 124.5(7) . . ? N29 C43 N30 108.6(7) . . ? N29 C44 N31 115.1(6) . . ? N29 C44 C45 102.0(6) . . ? N31 C44 C45 103.7(6) . . ? N29 C44 H44 111.8 . . ? N31 C44 H44 111.8 . . ? C45 C44 H44 111.8 . . ? N30 C45 N32 115.7(7) . . ? N30 C45 C44 102.7(6) . . ? N32 C45 C44 100.7(6) . . ? N30 C45 H45 112.3 . . ? N32 C45 H45 112.3 . . ? C44 C45 H45 112.2 . . ? O18 C46 N32 129.8(7) . . ? O18 C46 N31 121.6(7) . . ? N32 C46 N31 108.6(7) . . ? N30 C47 N33 113.3(5) . . ? N30 C47 H47A 108.9 . . ? N33 C47 H47A 108.9 . . ? N30 C47 H47B 108.9 . . ? N33 C47 H47B 108.9 . . ? H47A C47 H47B 107.7 . . ? N35 C48 N32 113.6(5) . . ? N35 C48 H48A 108.9 . . ? N32 C48 H48A 108.9 . . ? N35 C48 H48B 108.9 . . ? N32 C48 H48B 108.9 . . ? H48A C48 H48B 107.7 . . ? O14 C49 N33 128.7(9) . . ? O14 C49 N34 123.1(9) . . ? N33 C49 N34 108.2(8) . . ? N33 C50 N35 115.3(6) . . ? N33 C50 C51 101.6(6) . . ? N35 C50 C51 105.7(6) . . ? N33 C50 H50 111.2 . . ? N35 C50 H50 111.2 . . ? C51 C50 H50 111.2 . . ? N34 C51 N36 114.1(7) . . ? N34 C51 C50 106.0(6) . . ? N36 C51 C50 101.4(6) . . ? N34 C51 H51 111.6 . . ? N36 C51 H51 111.6 . . ? C50 C51 H51 111.6 . . ? O19 C52 N36 128.8(7) . . ? O19 C52 N35 122.9(7) . . ? N36 C52 N35 108.1(7) . . ? N34 C53 N37 114.4(6) . . ? N34 C53 H53A 108.6 . . ? N37 C53 H53A 108.6 . . ? N34 C53 H53B 108.7 . . ? N37 C53 H53B 108.7 . . ? H53A C53 H53B 107.6 . . ? N36 C54 N39 115.1(7) . . ? N36 C54 H54A 108.5 . . ? N39 C54 H54A 108.5 . . ? N36 C54 H54B 108.5 . . ? N39 C54 H54B 108.5 . . ? H54A C54 H54B 107.5 . . ? O15 C55 N37 127.7(8) . . ? O15 C55 N38 118.9(8) . . ? N37 C55 N38 113.1(8) . . ? N39 C56 N37 114.6(6) . . ? N39 C56 C57 103.8(5) . . ? N37 C56 C57 101.6(5) . . ? N39 C56 H56 112.0 . . ? N37 C56 H56 112.0 . . ? C57 C56 H56 112.0 . . ? N40 C57 N38 113.8(6) . . ? N40 C57 C56 104.0(6) . . ? N38 C57 C56 106.3(6) . . ? N40 C57 H57 110.8 . . ? N38 C57 H57 110.8 . . ? C56 C57 H57 110.8 . . ? O20 C58 N39 125.1(7) . . ? O20 C58 N40 125.0(8) . . ? N39 C58 N40 109.9(7) . . ? N21 C59 N38 112.3(6) . . ? N21 C59 H59A 109.1 . . ? N38 C59 H59A 109.1 . . ? N21 C59 H59B 109.1 . . ? N38 C59 H59B 109.2 . . ? H59A C59 H59B 107.9 . . ? N23 C60 N40 115.6(6) . . ? N23 C60 H60A 108.4 . . ? N40 C60 H60A 108.4 . . ? N23 C60 H60B 108.4 . . ? N40 C60 H60B 108.4 . . ? H60A C60 H60B 107.4 . . ? C1 N1 C29 121.9(7) . . ? C1 N1 C2 110.2(6) . . ? C29 N1 C2 127.9(6) . . ? C1 N2 C5 124.7(6) . . ? C1 N2 C3 107.7(6) . . ? C5 N2 C3 127.0(6) . . ? C4 N3 C2 111.4(6) . . ? C4 N3 C30 122.2(7) . . ? C2 N3 C30 126.3(6) . . ? C4 N4 C3 110.2(6) . . ? C4 N4 C6 122.3(7) . . ? C3 N4 C6 126.8(7) . . ? C7 N5 C5 122.9(6) . . ? C7 N5 C8 111.5(6) . . ? C5 N5 C8 124.7(6) . . ? C7 N6 C9 113.3(6) . . ? C7 N6 C11 123.2(7) . . ? C9 N6 C11 123.2(7) . . ? C10 N7 C8 111.9(6) . . ? C10 N7 C6 125.0(7) . . ? C8 N7 C6 123.1(7) . . ? C10 N8 C9 113.6(6) . . ? C10 N8 C12 123.1(6) . . ? C9 N8 C12 123.3(6) . . ? C13 N9 C14 116.4(6) . . ? C13 N9 C11 118.4(7) . . ? C14 N9 C11 124.7(6) . . ? C13 N10 C17 121.1(7) . . ? C13 N10 C15 116.2(6) . . ? C17 N10 C15 122.7(6) . . ? C16 N11 C14 114.4(6) . . ? C16 N11 C12 120.8(6) . . ? C14 N11 C12 124.1(6) . . ? C16 N12 C18 121.0(7) . . ? C16 N12 C15 114.1(6) . . ? C18 N12 C15 124.9(7) . . ? C19 N13 C17 124.5(7) . . ? C19 N13 C20 109.8(7) . . ? C17 N13 C20 125.6(6) . . ? C19 N14 C21 111.6(7) . . ? C19 N14 C23 123.6(7) . . ? C21 N14 C23 124.7(6) . . ? C22 N15 C20 114.9(6) . . ? C22 N15 C18 121.9(7) . . ? C20 N15 C18 123.1(7) . . ? C22 N16 C21 117.8(6) . . ? C22 N16 C24 119.9(6) . . ? C21 N16 C24 121.7(6) . . ? C25 N17 C26 113.2(6) . . ? C25 N17 C23 120.4(6) . . ? C26 N17 C23 126.3(6) . . ? C25 N18 C27 113.3(6) . . ? C25 N18 C29 121.3(7) . . ? C27 N18 C29 125.2(6) . . ? C28 N19 C26 109.1(6) . . ? C28 N19 C24 124.0(7) . . ? C26 N19 C24 126.9(6) . . ? C28 N20 C27 109.2(6) . . ? C28 N20 C30 124.1(7) . . ? C27 N20 C30 126.4(6) . . ? C31 N21 C32 113.9(5) . . ? C31 N21 C59 121.2(6) . . ? C32 N21 C59 123.8(6) . . ? C31 N22 C35 123.1(7) . . ? C31 N22 C33 112.3(6) . . ? C35 N22 C33 124.1(6) . . ? C34 N23 C32 115.5(6) . . ? C34 N23 C60 123.0(7) . . ? C32 N23 C60 121.5(6) . . ? C34 N24 C33 110.5(6) . . ? C34 N24 C36 124.7(7) . . ? C33 N24 C36 124.8(7) . . ? C37 N25 C38 116.1(6) . . ? C37 N25 C35 119.9(6) . . ? C38 N25 C35 123.2(6) . . ? C37 N26 C39 112.9(6) . . ? C37 N26 C41 121.8(6) . . ? C39 N26 C41 125.3(7) . . ? C40 N27 C36 121.5(7) . . ? C40 N27 C38 113.3(6) . . ? C36 N27 C38 124.3(7) . . ? C40 N28 C39 115.0(7) . . ? C40 N28 C42 119.2(7) . . ? C39 N28 C42 125.7(7) . . ? C43 N29 C44 113.4(6) . . ? C43 N29 C41 121.5(7) . . ? C44 N29 C41 125.1(6) . . ? C43 N30 C45 113.4(6) . . ? C43 N30 C47 123.4(6) . . ? C45 N30 C47 123.1(6) . . ? C46 N31 C42 125.2(6) . . ? C46 N31 C44 111.4(6) . . ? C42 N31 C44 123.2(6) . . ? C46 N32 C45 115.5(7) . . ? C46 N32 C48 120.1(6) . . ? C45 N32 C48 124.0(6) . . ? C49 N33 C50 113.8(7) . . ? C49 N33 C47 119.4(7) . . ? C50 N33 C47 126.8(6) . . ? C49 N34 C53 124.5(7) . . ? C49 N34 C51 110.2(7) . . ? C53 N34 C51 125.4(6) . . ? C52 N35 C50 111.0(6) . . ? C52 N35 C48 124.3(6) . . ? C50 N35 C48 124.7(6) . . ? C52 N36 C54 120.9(7) . . ? C52 N36 C51 113.8(6) . . ? C54 N36 C51 125.2(6) . . ? C55 N37 C53 122.7(7) . . ? C55 N37 C56 112.2(7) . . ? C53 N37 C56 125.1(6) . . ? C55 N38 C59 126.9(7) . . ? C55 N38 C57 106.3(7) . . ? C59 N38 C57 126.3(6) . . ? C58 N39 C56 111.9(6) . . ? C58 N39 C54 121.5(7) . . ? C56 N39 C54 126.6(6) . . ? C58 N40 C57 110.0(6) . . ? C58 N40 C60 124.1(6) . . ? C57 N40 C60 125.0(6) . . ? C1 O1 Ca1 123.3(4) . . ? C7 O2 Ca1 123.2(4) . . ? C7 O2 Ca4 92.8(3) . 8_556 ? Ca1 O2 Ca4 144.05(18) . 8_556 ? C13 O3 Ca1 122.8(5) . . ? C19 O4 Ca1 123.9(5) . . ? C25 O5 Ca1 123.1(5) . . ? C4 O6 Ca2 112.2(5) . . ? C10 O7 Ca2 111.1(3) . . ? C16 O8 Ca2 113.7(5) . . ? C22 O9 Ca2 115.3(5) . . ? C28 O10 Ca2 113.7(5) . . ? C31 O11 Ca3 123.3(4) . . ? C31 O11 Ca2 92.6(3) . . ? Ca3 O11 Ca2 144.07(17) . . ? C37 O12 Ca3 123.3(4) . . ? C43 O13 Ca3 123.9(5) . . ? C49 O14 Ca3 123.8(5) . . ? C55 O15 Ca3 122.2(5) . . ? C34 O16 Ca4 111.8(3) . . ? C40 O17 Ca4 110.6(5) . . ? C46 O18 Ca4 115.0(4) . . ? C52 O19 Ca4 114.0(5) . . ? C58 O20 Ca4 114.5(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.813 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.162 data_compound2 _database_code_depnum_ccdc_archive 'CCDC 882715' #TrackingRef '- compound 1 -3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H30 N20 O10, 2(C7 H6 O3), 13(H2 O)' _chemical_formula_sum 'C44 H68 N20 O29' _chemical_formula_weight 1341.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2' _symmetry_space_group_name_Hall 'P 2 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 15.8841(18) _cell_length_b 12.4803(14) _cell_length_c 14.1747(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2810.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9571 _exptl_absorpt_correction_T_max 0.9622 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18314 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.10 _reflns_number_total 4965 _reflns_number_gt 4628 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+1.8497P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.4(13) _chemical_absolute_configuration unk _refine_ls_number_reflns 4965 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1303 _refine_ls_wR_factor_gt 0.1282 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.10015(17) 0.8209(2) 0.6731(2) 0.0276(6) Uani 1 1 d . . . C2 C 0.11822(19) 0.9745(2) 0.5840(2) 0.0322(6) Uani 1 1 d . . . H2 H 0.1327 0.9739 0.5161 0.039 Uiso 1 1 calc R . . C3 C 0.19626(19) 0.9582(2) 0.6458(2) 0.0308(6) Uani 1 1 d . . . H3 H 0.2477 0.9487 0.6072 0.037 Uiso 1 1 calc R . . C4 C 0.13471(19) 1.1243(2) 0.6791(2) 0.0312(7) Uani 1 1 d . . . C5 C 0.23296(17) 0.8120(2) 0.7642(2) 0.0296(6) Uani 1 1 d . . . H5A H 0.2910 0.8228 0.7428 0.035 Uiso 1 1 calc R . . H5B H 0.2217 0.7348 0.7633 0.035 Uiso 1 1 calc R . . C6 C 0.2654(2) 1.0817(2) 0.7678(2) 0.0354(7) Uani 1 1 d . . . H6A H 0.3182 1.0496 0.7459 0.043 Uiso 1 1 calc R . . H6B H 0.2733 1.1596 0.7696 0.043 Uiso 1 1 calc R . . C7 C 0.17032(18) 0.8054(2) 0.9242(2) 0.0283(6) Uani 1 1 d . . . C8 C 0.27069(18) 0.9401(2) 0.8999(2) 0.0309(6) Uani 1 1 d . . . H8 H 0.3323 0.9287 0.8978 0.037 Uiso 1 1 calc R . . C9 C 0.23850(17) 0.9457(2) 1.0029(2) 0.0277(6) Uani 1 1 d . . . H9 H 0.2837 0.9293 1.0488 0.033 Uiso 1 1 calc R . . C10 C 0.21557(16) 1.1112(2) 0.9308(2) 0.0270(6) Uani 1 1 d . . . C11 C 0.13120(18) 0.8290(2) 1.0895(2) 0.0301(6) Uani 1 1 d . . . H11A H 0.1694 0.8387 1.1430 0.036 Uiso 1 1 calc R . . H11B H 0.1188 0.7523 1.0840 0.036 Uiso 1 1 calc R . . C12 C 0.17129(18) 1.0985(2) 1.0967(2) 0.0306(6) Uani 1 1 d . . . H12A H 0.1999 1.0688 1.1521 0.037 Uiso 1 1 calc R . . H12B H 0.1802 1.1762 1.0971 0.037 Uiso 1 1 calc R . . C13 C -0.02374(17) 0.8457(2) 1.08364(19) 0.0274(6) Uani 1 1 d . . . C14 C 0.04728(18) 0.9882(2) 1.15568(19) 0.0259(6) Uani 1 1 d . . . H14 H 0.0697 0.9837 1.2207 0.031 Uiso 1 1 calc R . . C15 C -0.0169(2) 0.8652(2) 0.5678(2) 0.0354(7) Uani 1 1 d . . . H15A H -0.0285 0.7881 0.5706 0.042 Uiso 1 1 calc R . . H15B H -0.0153 0.8859 0.5011 0.042 Uiso 1 1 calc R . . N1 N 0.06420(17) 0.88505(19) 0.60881(17) 0.0324(6) Uani 1 1 d . . . N2 N 0.17714(15) 0.86363(19) 0.69912(18) 0.0322(6) Uani 1 1 d . . . N3 N 0.08504(17) 1.07839(19) 0.61319(18) 0.0341(6) Uani 1 1 d . . . N4 N 0.19963(16) 1.05674(19) 0.70116(18) 0.0331(6) Uani 1 1 d . . . N5 N 0.22600(15) 0.84965(19) 0.86003(18) 0.0310(5) Uani 1 1 d . . . N6 N 0.17271(15) 0.86484(19) 1.00417(17) 0.0304(5) Uani 1 1 d . . . N7 N 0.24818(16) 1.04413(19) 0.86211(19) 0.0354(6) Uani 1 1 d . . . N8 N 0.20979(16) 1.05375(18) 1.01167(18) 0.0313(6) Uani 1 1 d . . . N9 N 0.05348(15) 0.8866(2) 1.10787(17) 0.0311(6) Uani 1 1 d . . . N10 N 0.08324(15) 1.07775(18) 1.10490(17) 0.0301(5) Uani 1 1 d . . . O1 O 0.07008(13) 0.73580(15) 0.70391(15) 0.0348(5) Uani 1 1 d . . . O2 O 0.12861(13) 0.72542(16) 0.90998(15) 0.0343(5) Uani 1 1 d . . . O3 O -0.03737(14) 0.75921(16) 1.04862(16) 0.0378(5) Uani 1 1 d . . . O4 O 0.12682(15) 1.21594(17) 0.71131(16) 0.0424(5) Uani 1 1 d . . . O5 O 0.19682(13) 1.20539(15) 0.92045(15) 0.0345(5) Uani 1 1 d . . . C16 C 0.3022(2) 0.7335(3) 0.5327(2) 0.0366(7) Uani 1 1 d . . . H16 H 0.3545 0.7541 0.5580 0.044 Uiso 1 1 calc R . . C17 C 0.2665(2) 0.7935(2) 0.4622(2) 0.0334(7) Uani 1 1 d . . . H17 H 0.2939 0.8557 0.4408 0.040 Uiso 1 1 calc R . . C18 C 0.1903(2) 0.7631(2) 0.4219(2) 0.0364(7) Uani 1 1 d . . . C19 C 0.14894(19) 0.6727(2) 0.4568(2) 0.0362(7) Uani 1 1 d . . . H19 H 0.0966 0.6522 0.4316 0.043 Uiso 1 1 calc R . . C20 C 0.18555(19) 0.6129(2) 0.5292(2) 0.0347(7) Uani 1 1 d . . . H20 H 0.1578 0.5518 0.5523 0.042 Uiso 1 1 calc R . . C21 C 0.26214(19) 0.6426(2) 0.5674(2) 0.0319(6) Uani 1 1 d . . . C22 C 0.3052(2) 0.5715(3) 0.6385(2) 0.0375(7) Uani 1 1 d . . . O6 O 0.15483(16) 0.81747(19) 0.34983(18) 0.0481(6) Uani 1 1 d . . . H6 H 0.1864 0.8672 0.3336 0.072 Uiso 1 1 calc R . . O7 O 0.26483(16) 0.49684(18) 0.67699(16) 0.0443(6) Uani 1 1 d . . . O8 O 0.38180(18) 0.5864(3) 0.6527(2) 0.0722(9) Uani 1 1 d . . . H8A H 0.3880 0.6246 0.7001 0.108 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 C1 0.0284(14) 0.0297(15) 0.0245(15) -0.0081(11) 0.0033(11) 0.0007(12) C2 0.0408(17) 0.0330(16) 0.0227(14) 0.0011(12) 0.0087(13) 0.0022(13) C3 0.0343(15) 0.0304(14) 0.0278(15) 0.0016(12) 0.0086(13) 0.0011(12) C4 0.0356(15) 0.0269(15) 0.0311(16) 0.0008(12) 0.0160(12) -0.0021(12) C5 0.0255(14) 0.0272(14) 0.0360(16) -0.0005(12) 0.0031(12) 0.0048(11) C6 0.0376(16) 0.0298(15) 0.0389(17) 0.0001(13) 0.0116(13) -0.0063(13) C7 0.0279(14) 0.0212(13) 0.0359(16) 0.0014(12) -0.0049(12) 0.0101(11) C8 0.0214(13) 0.0282(14) 0.0432(17) -0.0019(13) -0.0020(12) 0.0032(11) C9 0.0243(14) 0.0268(14) 0.0321(15) -0.0013(12) -0.0065(12) 0.0022(11) C10 0.0155(12) 0.0310(15) 0.0346(16) -0.0054(12) -0.0011(11) -0.0065(11) C11 0.0297(14) 0.0266(14) 0.0340(16) 0.0048(12) -0.0023(13) 0.0091(12) C12 0.0326(15) 0.0360(16) 0.0231(14) -0.0074(12) -0.0007(12) -0.0002(12) C13 0.0341(15) 0.0254(14) 0.0226(13) 0.0066(11) 0.0019(11) -0.0008(12) C14 0.0349(15) 0.0223(13) 0.0205(13) 0.0014(10) 0.0003(11) -0.0032(11) C15 0.0474(18) 0.0278(15) 0.0311(16) -0.0093(13) -0.0062(13) 0.0039(13) N1 0.0414(14) 0.0252(12) 0.0307(13) -0.0025(10) -0.0001(11) 0.0000(11) N2 0.0345(13) 0.0283(12) 0.0339(13) 0.0015(10) 0.0063(11) -0.0006(10) N3 0.0395(14) 0.0285(13) 0.0343(14) 0.0003(10) 0.0067(11) 0.0041(11) N4 0.0358(13) 0.0280(12) 0.0354(14) -0.0024(11) 0.0039(11) -0.0010(10) N5 0.0335(13) 0.0279(12) 0.0316(13) 0.0000(10) 0.0077(11) -0.0038(10) N6 0.0291(12) 0.0333(13) 0.0287(13) -0.0006(10) -0.0040(10) -0.0041(10) N7 0.0400(14) 0.0277(12) 0.0387(14) -0.0026(11) 0.0018(12) -0.0014(11) N8 0.0346(13) 0.0216(11) 0.0377(14) -0.0027(10) 0.0023(11) -0.0018(10) N9 0.0312(13) 0.0326(13) 0.0296(13) -0.0035(10) -0.0019(10) 0.0012(10) N10 0.0350(13) 0.0215(11) 0.0338(13) -0.0002(10) -0.0034(10) -0.0029(10) O1 0.0389(11) 0.0280(10) 0.0375(11) 0.0041(9) 0.0003(9) -0.0005(9) O2 0.0367(11) 0.0240(10) 0.0423(12) -0.0034(9) 0.0006(9) -0.0065(9) O3 0.0442(12) 0.0255(11) 0.0437(12) -0.0060(9) -0.0021(10) -0.0044(9) O4 0.0540(14) 0.0343(12) 0.0390(13) -0.0029(10) 0.0117(11) 0.0036(10) O5 0.0361(11) 0.0234(10) 0.0440(12) 0.0008(9) -0.0043(10) -0.0027(8) C16 0.0379(16) 0.0377(16) 0.0341(16) -0.0071(14) 0.0024(13) 0.0020(14) C17 0.0455(17) 0.0231(13) 0.0317(15) 0.0007(12) 0.0067(14) 0.0069(13) C18 0.0462(18) 0.0270(14) 0.0358(17) -0.0055(13) 0.0018(14) 0.0081(13) C19 0.0333(16) 0.0333(15) 0.0418(18) 0.0024(14) -0.0016(13) 0.0020(13) C20 0.0331(16) 0.0304(15) 0.0405(18) -0.0024(13) 0.0081(13) 0.0027(12) C21 0.0397(16) 0.0272(14) 0.0289(15) -0.0009(12) 0.0065(12) 0.0016(12) C22 0.0494(19) 0.0355(16) 0.0277(15) -0.0012(13) -0.0011(14) -0.0011(14) O6 0.0549(14) 0.0378(13) 0.0518(15) 0.0100(11) -0.0149(12) 0.0020(11) O7 0.0596(15) 0.0311(11) 0.0422(13) 0.0058(10) 0.0034(11) -0.0020(11) O8 0.0613(18) 0.082(2) 0.073(2) 0.0326(17) -0.0319(16) -0.0141(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.244(3) . ? C1 N1 1.341(4) . ? C1 N2 1.384(4) . ? C2 N1 1.451(4) . ? C2 N3 1.459(4) . ? C2 C3 1.531(4) . ? C2 H2 0.9900 . ? C3 N2 1.434(4) . ? C3 N4 1.460(4) . ? C3 H3 0.9900 . ? C4 O4 1.238(4) . ? C4 N3 1.351(4) . ? C4 N4 1.368(4) . ? C5 N2 1.433(4) . ? C5 N5 1.441(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.443(4) . ? C6 N4 1.443(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.214(3) . ? C7 N6 1.356(4) . ? C7 N5 1.383(4) . ? C8 N5 1.448(4) . ? C8 N7 1.449(4) . ? C8 C9 1.548(4) . ? C8 H8 0.9900 . ? C9 N8 1.429(3) . ? C9 N6 1.453(4) . ? C9 H9 0.9900 . ? C10 O5 1.222(3) . ? C10 N8 1.354(4) . ? C10 N7 1.384(4) . ? C11 N6 1.448(4) . ? C11 N9 1.452(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N10 1.427(4) . ? C12 N8 1.463(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.207(4) . ? C13 N9 1.372(4) . ? C13 N10 1.377(4) 2_575 ? C14 N9 1.440(4) . ? C14 N10 1.447(4) . ? C14 C14 1.531(6) 2_575 ? C14 H14 0.9900 . ? C15 N1 1.436(4) . ? C15 N3 1.442(4) 2_575 ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? N3 C15 1.442(4) 2_575 ? N10 C13 1.377(4) 2_575 ? C16 C17 1.372(4) . ? C16 C21 1.391(4) . ? C16 H16 0.9400 . ? C17 C18 1.391(5) . ? C17 H17 0.9400 . ? C18 O6 1.349(4) . ? C18 C19 1.396(4) . ? C19 C20 1.396(5) . ? C19 H19 0.9400 . ? C20 C21 1.382(4) . ? C20 H20 0.9400 . ? C21 C22 1.508(4) . ? C22 O8 1.247(4) . ? C22 O7 1.256(4) . ? O6 H6 0.8300 . ? O8 H8A 0.8300 . ? 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 O1 C1 N1 125.8(3) . . ? O1 C1 N2 125.1(3) . . ? N1 C1 N2 109.1(2) . . ? N1 C2 N3 113.7(2) . . ? N1 C2 C3 103.8(2) . . ? N3 C2 C3 104.4(2) . . ? N1 C2 H2 111.5 . . ? N3 C2 H2 111.5 . . ? C3 C2 H2 111.5 . . ? N2 C3 N4 114.7(2) . . ? N2 C3 C2 103.9(2) . . ? N4 C3 C2 103.0(2) . . ? N2 C3 H3 111.6 . . ? N4 C3 H3 111.6 . . ? C2 C3 H3 111.6 . . ? O4 C4 N3 126.0(3) . . ? O4 C4 N4 124.2(3) . . ? N3 C4 N4 109.7(2) . . ? N2 C5 N5 114.4(2) . . ? N2 C5 H5A 108.7 . . ? N5 C5 H5A 108.7 . . ? N2 C5 H5B 108.7 . . ? N5 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N7 C6 N4 113.5(2) . . ? N7 C6 H6A 108.9 . . ? N4 C6 H6A 108.9 . . ? N7 C6 H6B 108.9 . . ? N4 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 127.1(3) . . ? O2 C7 N5 124.6(3) . . ? N6 C7 N5 108.2(2) . . ? N5 C8 N7 115.6(2) . . ? N5 C8 C9 104.0(2) . . ? N7 C8 C9 103.1(2) . . ? N5 C8 H8 111.2 . . ? N7 C8 H8 111.2 . . ? C9 C8 H8 111.2 . . ? N8 C9 N6 115.1(2) . . ? N8 C9 C8 103.3(2) . . ? N6 C9 C8 102.6(2) . . ? N8 C9 H9 111.7 . . ? N6 C9 H9 111.7 . . ? C8 C9 H9 111.7 . . ? O5 C10 N8 126.5(3) . . ? O5 C10 N7 126.0(3) . . ? N8 C10 N7 107.5(2) . . ? N6 C11 N9 112.6(2) . . ? N6 C11 H11A 109.1 . . ? N9 C11 H11A 109.1 . . ? N6 C11 H11B 109.1 . . ? N9 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? N10 C12 N8 114.0(2) . . ? N10 C12 H12A 108.7 . . ? N8 C12 H12A 108.7 . . ? N10 C12 H12B 108.7 . . ? N8 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? O3 C13 N9 126.6(3) . . ? O3 C13 N10 125.9(3) . 2_575 ? N9 C13 N10 107.5(2) . 2_575 ? N9 C14 N10 114.7(2) . . ? N9 C14 C14 103.7(2) . 2_575 ? N10 C14 C14 103.8(2) . 2_575 ? N9 C14 H14 111.4 . . ? N10 C14 H14 111.4 . . ? C14 C14 H14 111.4 2_575 . ? N1 C15 N3 114.1(2) . 2_575 ? N1 C15 H15A 108.7 . . ? N3 C15 H15A 108.7 2_575 . ? N1 C15 H15B 108.7 . . ? N3 C15 H15B 108.7 2_575 . ? H15A C15 H15B 107.6 . . ? C1 N1 C15 123.7(2) . . ? C1 N1 C2 111.9(2) . . ? C15 N1 C2 124.5(2) . . ? C1 N2 C5 123.0(2) . . ? C1 N2 C3 111.3(3) . . ? C5 N2 C3 125.3(2) . . ? C4 N3 C15 122.7(2) . 2_575 ? C4 N3 C2 111.2(3) . . ? C15 N3 C2 125.3(3) 2_575 . ? C4 N4 C6 124.2(3) . . ? C4 N4 C3 111.7(2) . . ? C6 N4 C3 124.1(2) . . ? C7 N5 C5 122.5(2) . . ? C7 N5 C8 111.6(2) . . ? C5 N5 C8 125.8(2) . . ? C7 N6 C11 121.1(2) . . ? C7 N6 C9 113.0(2) . . ? C11 N6 C9 123.5(2) . . ? C10 N7 C6 121.8(2) . . ? C10 N7 C8 111.9(2) . . ? C6 N7 C8 125.9(3) . . ? C10 N8 C9 113.8(2) . . ? C10 N8 C12 121.6(2) . . ? C9 N8 C12 124.4(2) . . ? C13 N9 C14 112.6(2) . . ? C13 N9 C11 122.0(2) . . ? C14 N9 C11 125.3(2) . . ? C13 N10 C12 121.9(2) 2_575 . ? C13 N10 C14 112.0(2) 2_575 . ? C12 N10 C14 124.6(2) . . ? C17 C16 C21 120.9(3) . . ? C17 C16 H16 119.6 . . ? C21 C16 H16 119.6 . . ? C16 C17 C18 120.7(3) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? O6 C18 C17 122.5(3) . . ? O6 C18 C19 118.6(3) . . ? C17 C18 C19 118.9(3) . . ? C18 C19 C20 119.8(3) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C21 C20 C19 120.7(3) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C16 118.9(3) . . ? C20 C21 C22 120.3(3) . . ? C16 C21 C22 120.6(3) . . ? O8 C22 O7 122.6(3) . . ? O8 C22 C21 117.6(3) . . ? O7 C22 C21 119.7(3) . . ? C18 O6 H6 109.5 . . ? C22 O8 H8A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.274 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.052 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 -0.008 301 121 ' ' 2 0.000 0.000 0.860 58 12 ' ' 3 0.000 0.500 0.234 298 119 ' ' 4 0.500 0.500 0.140 55 10 ' ' _platon_squeeze_details ; ; data_compound3 _database_code_depnum_ccdc_archive 'CCDC 882716' #TrackingRef '- compound 1 -3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H38 Ca N20 O14, C7 H6 O3, 2Cl, 12(H2 O)' _chemical_formula_sum 'C37 H68 Ca Cl2 N20 O29' _chemical_formula_weight 1368.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 65' _symmetry_space_group_name_Hall 'P 65' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'x-y, x, z+5/6' 'y, -x+y, z+1/6' _cell_length_a 14.7327(18) _cell_length_b 14.7327(18) _cell_length_c 46.389(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8720(3) _cell_formula_units_Z 6 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4296 _exptl_absorpt_coefficient_mu 0.306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9274 _exptl_absorpt_correction_T_max 0.9441 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59169 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.09 _reflns_number_total 10098 _reflns_number_gt 8730 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1760P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.1(2) _refine_ls_number_reflns 10098 _refine_ls_number_parameters 655 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.2189 _refine_ls_wR_factor_gt 0.2124 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 5.223 _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 O1W O 0.5504(14) 0.0297(14) 0.5168(6) 0.051(5) Uani 1 1 d . . . O2W O 0.8425(13) 0.3477(14) 0.5066(5) 0.046(4) Uani 1 1 d . . . O3W O 0.4802(15) 0.1763(17) 0.5233(6) 0.056(5) Uani 1 1 d . . . O4W O 0.6762(19) 0.3881(16) 0.4937(6) 0.063(6) Uani 1 1 d . . . Ca1 Ca 0.6627(4) 0.2170(4) 0.5109(3) 0.0331(12) Uani 1 1 d . . . Cl1 Cl 0.0484(17) 0.024(3) 0.4326(6) 0.173(9) Uani 1 1 d . . . Cl3 Cl 0.091(9) -0.560(11) 0.364(6) 1.0(3) Uani 0.50 1 d P . . Cl4 Cl 0.578(6) 0.020(4) 0.2576(13) 0.19(2) Uani 0.50 1 d P . . C1 C 0.7747(18) 0.1414(19) 0.4551(6) 0.036(5) Uani 1 1 d . . . C2 C 0.8521(19) 0.100(2) 0.4178(6) 0.038(5) Uani 1 1 d . . . H2 H 0.9277 0.1224 0.4182 0.046 Uiso 1 1 calc R . . C3 C 0.8332(19) 0.188(2) 0.4075(6) 0.039(5) Uani 1 1 d . . . H3 H 0.8995 0.2507 0.4017 0.046 Uiso 1 1 calc R . . C4 C 0.7487(18) 0.0460(18) 0.3763(6) 0.035(5) Uani 1 1 d . . . C5 C 0.7564(18) 0.2856(18) 0.4330(6) 0.033(5) Uani 1 1 d . . . H5A H 0.8045 0.3451 0.4210 0.040 Uiso 1 1 calc R . . H5B H 0.7622 0.3112 0.4528 0.040 Uiso 1 1 calc R . . C6 C 0.7325(18) 0.2005(18) 0.3636(6) 0.033(5) Uani 1 1 d . . . H6A H 0.7883 0.2740 0.3631 0.040 Uiso 1 1 calc R . . H6B H 0.7246 0.1719 0.3441 0.040 Uiso 1 1 calc R . . C7 C 0.5663(18) 0.2034(16) 0.4413(6) 0.031(5) Uani 1 1 d . . . C8 C 0.6230(18) 0.2603(17) 0.3934(6) 0.030(5) Uani 1 1 d . . . H8 H 0.6591 0.3349 0.3875 0.036 Uiso 1 1 calc R . . C9 C 0.5034(17) 0.2137(17) 0.3955(6) 0.032(5) Uani 1 1 d . . . H9 H 0.4831 0.2663 0.3904 0.038 Uiso 1 1 calc R . . C10 C 0.5415(18) 0.1200(17) 0.3612(5) 0.030(5) Uani 1 1 d . . . C11 C 0.3791(19) 0.1473(18) 0.4397(6) 0.034(5) Uani 1 1 d . . . H11A H 0.3924 0.1743 0.4595 0.041 Uiso 1 1 calc R . . H11B H 0.3419 0.1776 0.4296 0.041 Uiso 1 1 calc R . . C12 C 0.3514(17) 0.0544(18) 0.3701(6) 0.033(5) Uani 1 1 d . . . H12A H 0.3128 0.0926 0.3704 0.039 Uiso 1 1 calc R . . H12B H 0.3429 0.0235 0.3509 0.039 Uiso 1 1 calc R . . C13 C 0.3105(16) -0.0271(18) 0.4630(6) 0.031(5) Uani 1 1 d . . . C14 C 0.2490(17) -0.0261(18) 0.4164(6) 0.031(5) Uani 1 1 d . . . H14 H 0.1958 -0.0065 0.4113 0.037 Uiso 1 1 calc R . . C15 C 0.1966(16) -0.1410(16) 0.4282(5) 0.027(4) Uani 1 1 d . . . H15 H 0.1201 -0.1717 0.4310 0.033 Uiso 1 1 calc R . . C16 C 0.2836(17) -0.1284(17) 0.3847(6) 0.030(5) Uani 1 1 d . . . C17 C 0.2147(18) -0.2143(18) 0.4763(6) 0.035(5) Uani 1 1 d . . . H17A H 0.2250 -0.1842 0.4956 0.042 Uiso 1 1 calc R . . H17B H 0.1394 -0.2625 0.4737 0.042 Uiso 1 1 calc R . . C18 C 0.1897(18) -0.3046(17) 0.4066(6) 0.034(5) Uani 1 1 d . . . H18A H 0.1181 -0.3440 0.4141 0.041 Uiso 1 1 calc R . . H18B H 0.1888 -0.3295 0.3869 0.041 Uiso 1 1 calc R . . C19 C 0.3564(18) -0.2488(18) 0.4908(6) 0.033(5) Uani 1 1 d . . . C20 C 0.2428(17) -0.3569(17) 0.4544(6) 0.033(5) Uani 1 1 d . . . H20 H 0.1718 -0.4169 0.4580 0.039 Uiso 1 1 calc R . . C21 C 0.329(2) -0.3875(19) 0.4600(6) 0.038(6) Uani 1 1 d . . . H21 H 0.2987 -0.4608 0.4668 0.046 Uiso 1 1 calc R . . C22 C 0.335(2) -0.3395(17) 0.4115(6) 0.035(5) Uani 1 1 d . . . C23 C 0.488(2) -0.304(2) 0.4942(7) 0.048(6) Uani 1 1 d . . . H23A H 0.4793 -0.3744 0.4959 0.057 Uiso 1 1 calc R . . H23B H 0.4984 -0.2741 0.5135 0.057 Uiso 1 1 calc R . . C24 C 0.456(2) -0.3978(19) 0.4250(7) 0.042(6) Uani 1 1 d . . . H24A H 0.4453 -0.4238 0.4051 0.050 Uiso 1 1 calc R . . H24B H 0.4482 -0.4544 0.4377 0.050 Uiso 1 1 calc R . . C25 C 0.652(2) -0.136(2) 0.4847(6) 0.038(6) Uani 1 1 d . . . C26 C 0.625(2) -0.276(2) 0.4537(7) 0.044(6) Uani 1 1 d . . . H26 H 0.6378 -0.3313 0.4610 0.053 Uiso 1 1 calc R . . C27 C 0.726(2) -0.179(2) 0.4457(6) 0.037(5) Uani 1 1 d . . . H27 H 0.7860 -0.1906 0.4470 0.044 Uiso 1 1 calc R . . C28 C 0.6162(19) -0.2396(19) 0.4048(6) 0.037(5) Uani 1 1 d . . . C29 C 0.819(2) 0.009(2) 0.4671(7) 0.045(6) Uani 1 1 d . . . H29A H 0.8221 0.0361 0.4865 0.054 Uiso 1 1 calc R . . H29B H 0.8859 0.0116 0.4634 0.054 Uiso 1 1 calc R . . C30 C 0.7876(19) -0.086(2) 0.3966(6) 0.036(5) Uani 1 1 d . . . H30A H 0.7730 -0.1143 0.3770 0.044 Uiso 1 1 calc R . . H30B H 0.8553 -0.0771 0.4026 0.044 Uiso 1 1 calc R . . N1 N 0.8062(15) 0.0750(17) 0.4465(6) 0.038(5) Uani 1 1 d . . . N2 N 0.7884(16) 0.2085(16) 0.4325(5) 0.037(5) Uani 1 1 d . . . N3 N 0.7954(15) 0.0172(16) 0.3963(5) 0.038(5) Uani 1 1 d . . . N4 N 0.7636(16) 0.1421(17) 0.3833(5) 0.037(5) Uani 1 1 d . . . N5 N 0.6514(15) 0.2475(15) 0.4230(5) 0.032(4) Uani 1 1 d . . . N6 N 0.4794(14) 0.1816(14) 0.4253(5) 0.029(4) Uani 1 1 d . . . N7 N 0.6340(15) 0.1953(15) 0.3722(5) 0.033(4) Uani 1 1 d . . . N8 N 0.4631(15) 0.1293(16) 0.3748(5) 0.034(4) Uani 1 1 d . . . N9 N 0.3131(14) 0.0355(15) 0.4405(5) 0.033(4) Uani 1 1 d . . . N10 N 0.2496(15) -0.1299(15) 0.4551(5) 0.032(4) Uani 1 1 d . . . N11 N 0.3057(14) -0.0291(14) 0.3912(5) 0.030(4) Uani 1 1 d . . . N12 N 0.2206(15) -0.1949(15) 0.4053(5) 0.033(4) Uani 1 1 d . . . N13 N 0.2683(15) -0.2728(14) 0.4744(5) 0.033(4) Uani 1 1 d . . . N14 N 0.3938(17) -0.3127(17) 0.4818(6) 0.043(5) Uani 1 1 d . . . N15 N 0.2565(15) -0.3270(15) 0.4240(5) 0.033(4) Uani 1 1 d . . . N16 N 0.3784(17) -0.3718(15) 0.4319(5) 0.036(4) Uani 1 1 d . . . N17 N 0.5802(17) -0.2387(17) 0.4765(6) 0.042(5) Uani 1 1 d . . . N18 N 0.7345(17) -0.1016(18) 0.4661(5) 0.040(5) Uani 1 1 d . . . N19 N 0.5654(17) -0.3067(17) 0.4279(6) 0.041(5) Uani 1 1 d . . . N20 N 0.7063(17) -0.1603(18) 0.4159(5) 0.039(5) Uani 1 1 d . . . O1 O 0.7429(13) 0.1459(13) 0.4791(4) 0.038(4) Uani 1 1 d . . . O2 O 0.5677(13) 0.1874(13) 0.4666(5) 0.037(4) Uani 1 1 d . . . O3 O 0.3537(13) 0.0063(13) 0.4865(4) 0.036(4) Uani 1 1 d . . . O4 O 0.3918(14) -0.1831(14) 0.5098(5) 0.041(4) Uani 1 1 d . . . O5 O 0.6427(16) -0.0918(15) 0.5050(5) 0.049(4) Uani 1 1 d . . . O6 O 0.7001(14) -0.0060(14) 0.3549(5) 0.042(4) Uani 1 1 d . . . O7 O 0.5281(13) 0.0572(13) 0.3420(4) 0.037(4) Uani 1 1 d . . . O8 O 0.3135(12) -0.1537(12) 0.3627(4) 0.033(3) Uani 1 1 d . . . O9 O 0.3594(15) -0.3236(15) 0.3861(5) 0.043(4) Uani 1 1 d . . . O10 O 0.5851(15) -0.2486(14) 0.3800(5) 0.044(4) Uani 1 1 d . . . C31 C -0.043(3) -0.210(4) 0.3805(8) 0.142(11) Uani 1 1 d D . . H31 H -0.0808 -0.1917 0.3932 0.171 Uiso 1 1 calc R . . C32 C 0.025(4) -0.136(3) 0.3610(9) 0.142(11) Uani 1 1 d D . . H32 H 0.0345 -0.0677 0.3605 0.171 Uiso 1 1 calc R . . C33 C 0.079(3) -0.165(3) 0.3422(8) 0.142(11) Uani 1 1 d D . . C34 C 0.067(3) -0.265(3) 0.3424(8) 0.142(11) Uani 1 1 d D . . H34 H 0.1051 -0.2818 0.3291 0.171 Uiso 1 1 calc R . . C35 C -0.001(3) -0.342(3) 0.3625(8) 0.142(11) Uani 1 1 d D . . H35 H -0.0098 -0.4099 0.3628 0.171 Uiso 1 1 calc R . . C36 C -0.057(3) -0.313(3) 0.3820(7) 0.142(11) Uani 1 1 d D . . C37 C -0.127(3) -0.388(6) 0.4013(9) 0.142(11) Uani 1 1 d D . . O11 O 0.149(5) -0.090(4) 0.3222(14) 0.33(4) Uani 1 1 d D . . H11 H 0.1489 -0.0342 0.3247 0.494 Uiso 1 1 calc R . . O12 O -0.149(7) -0.485(7) 0.4049(18) 0.33(4) Uani 1 1 d D . . H12 H -0.1137 -0.4980 0.3935 0.494 Uiso 1 1 calc R . . O13 O -0.175(5) -0.357(7) 0.4184(15) 0.33(4) Uani 1 1 d 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 O1W 0.043(10) 0.048(10) 0.054(12) -0.015(9) -0.005(9) 0.018(8) O2W 0.038(9) 0.045(10) 0.048(12) -0.009(8) -0.001(8) 0.017(8) O3W 0.045(10) 0.074(13) 0.051(13) -0.023(11) -0.007(9) 0.031(10) O4W 0.080(15) 0.052(12) 0.045(13) -0.013(10) -0.030(11) 0.024(11) Ca1 0.036(2) 0.039(2) 0.022(2) -0.0078(18) -0.0069(18) 0.017(2) Cl1 0.144(14) 0.26(3) 0.178(19) -0.010(18) 0.009(13) 0.148(18) Cl3 0.26(9) 0.45(17) 1.7(6) -0.7(3) 0.5(2) -0.19(11) Cl4 0.27(6) 0.19(4) 0.20(5) 0.01(4) -0.02(4) 0.17(5) C1 0.028(11) 0.042(13) 0.031(14) -0.009(10) -0.006(9) 0.013(10) C2 0.035(12) 0.054(15) 0.027(13) -0.002(11) -0.001(10) 0.023(11) C3 0.035(12) 0.045(13) 0.034(14) -0.005(10) -0.001(10) 0.018(11) C4 0.032(11) 0.038(12) 0.034(14) -0.001(10) 0.002(10) 0.017(10) C5 0.034(12) 0.031(11) 0.025(12) -0.004(9) -0.001(9) 0.009(9) C6 0.033(11) 0.033(11) 0.026(12) 0.004(9) 0.005(9) 0.011(9) C7 0.038(12) 0.026(10) 0.025(13) -0.009(8) -0.005(9) 0.012(9) C8 0.039(12) 0.028(10) 0.019(11) 0.000(8) -0.002(9) 0.013(9) C9 0.036(12) 0.024(10) 0.036(14) 0.002(9) 0.000(10) 0.016(9) C10 0.039(12) 0.033(11) 0.018(12) 0.006(9) -0.004(9) 0.019(10) C11 0.039(12) 0.034(12) 0.031(13) 0.000(10) 0.005(10) 0.021(10) C12 0.035(11) 0.034(11) 0.024(12) 0.008(9) -0.006(9) 0.013(9) C13 0.025(10) 0.037(12) 0.025(13) 0.007(9) 0.003(9) 0.013(9) C14 0.033(11) 0.039(12) 0.021(11) -0.003(9) -0.001(9) 0.018(10) C15 0.023(9) 0.030(10) 0.022(11) -0.008(8) -0.004(8) 0.009(8) C16 0.026(10) 0.030(11) 0.028(13) -0.003(9) -0.007(9) 0.010(9) C17 0.029(11) 0.038(12) 0.028(13) 0.005(10) 0.007(9) 0.009(10) C18 0.036(12) 0.025(11) 0.027(13) -0.007(9) -0.008(9) 0.004(9) C19 0.034(11) 0.032(11) 0.027(13) 0.007(9) 0.008(9) 0.011(10) C20 0.032(11) 0.029(11) 0.030(13) 0.001(9) 0.010(9) 0.010(9) C21 0.051(14) 0.033(12) 0.034(14) 0.008(10) 0.009(11) 0.023(11) C22 0.047(13) 0.027(11) 0.029(14) -0.003(9) 0.004(10) 0.016(10) C23 0.060(16) 0.063(17) 0.027(14) 0.011(12) 0.007(12) 0.036(14) C24 0.053(14) 0.034(12) 0.038(15) 0.001(10) 0.006(11) 0.022(11) C25 0.055(15) 0.054(15) 0.019(13) 0.004(10) -0.005(10) 0.037(13) C26 0.067(17) 0.061(16) 0.035(15) 0.000(12) -0.003(12) 0.054(15) C27 0.046(13) 0.056(14) 0.029(13) 0.002(10) -0.006(10) 0.040(12) C28 0.044(13) 0.043(13) 0.033(15) -0.008(10) -0.005(10) 0.028(11) C29 0.035(13) 0.066(17) 0.038(16) 0.000(12) -0.004(10) 0.028(12) C30 0.039(12) 0.055(14) 0.025(13) -0.002(10) 0.002(10) 0.031(12) N1 0.033(10) 0.052(12) 0.033(12) -0.003(9) -0.002(8) 0.024(9) N2 0.041(11) 0.040(11) 0.028(11) 0.000(8) 0.001(8) 0.017(9) N3 0.032(10) 0.044(11) 0.033(12) -0.007(9) -0.005(8) 0.015(9) N4 0.038(10) 0.047(11) 0.023(11) -0.006(8) -0.004(8) 0.019(9) N5 0.033(10) 0.032(9) 0.026(11) -0.001(8) -0.005(8) 0.012(8) N6 0.031(9) 0.033(9) 0.024(10) 0.001(7) 0.002(8) 0.016(8) N7 0.038(10) 0.034(10) 0.026(11) -0.004(8) -0.003(8) 0.018(8) N8 0.034(10) 0.043(11) 0.025(10) 0.001(8) 0.000(8) 0.019(9) N9 0.030(9) 0.031(9) 0.035(11) -0.001(8) -0.006(8) 0.013(8) N10 0.042(11) 0.038(10) 0.018(10) 0.002(8) 0.002(8) 0.021(9) N11 0.029(9) 0.032(9) 0.029(11) 0.001(8) 0.002(8) 0.016(8) N12 0.035(10) 0.033(10) 0.027(11) -0.003(8) 0.005(8) 0.014(8) N13 0.042(11) 0.033(10) 0.019(10) -0.001(7) 0.004(8) 0.016(9) N14 0.047(12) 0.047(12) 0.034(12) -0.002(9) -0.005(9) 0.024(10) N15 0.038(10) 0.034(10) 0.026(11) -0.002(8) 0.001(8) 0.017(8) N16 0.049(11) 0.030(9) 0.027(11) 0.002(8) 0.006(9) 0.019(9) N17 0.052(12) 0.045(12) 0.035(12) 0.006(9) 0.010(10) 0.029(11) N18 0.043(11) 0.055(13) 0.033(12) -0.006(9) -0.006(9) 0.033(10) N19 0.054(12) 0.042(11) 0.032(12) 0.004(9) 0.000(10) 0.028(10) N20 0.050(12) 0.055(12) 0.023(11) -0.001(9) -0.003(9) 0.034(11) O1 0.043(9) 0.049(9) 0.022(9) -0.007(7) 0.001(7) 0.023(8) O2 0.035(9) 0.044(9) 0.022(9) -0.006(7) -0.008(7) 0.013(7) O3 0.043(9) 0.039(9) 0.022(9) 0.000(7) -0.003(7) 0.015(7) O4 0.050(10) 0.049(10) 0.025(9) -0.007(8) -0.004(8) 0.026(8) O5 0.066(12) 0.053(11) 0.030(11) -0.003(8) -0.002(9) 0.033(10) O6 0.052(10) 0.046(10) 0.026(9) -0.004(8) -0.001(8) 0.023(8) O7 0.046(9) 0.039(9) 0.026(9) -0.004(7) 0.000(7) 0.020(8) O8 0.035(8) 0.035(8) 0.025(9) 0.002(6) 0.006(6) 0.014(7) O9 0.059(11) 0.049(10) 0.025(10) -0.008(7) 0.005(8) 0.030(9) O10 0.058(11) 0.050(10) 0.026(10) -0.004(7) 0.004(8) 0.029(9) C31 0.14(2) 0.117(18) 0.16(3) -0.032(17) -0.08(2) 0.055(16) C32 0.14(2) 0.117(18) 0.16(3) -0.032(17) -0.08(2) 0.055(16) C33 0.14(2) 0.117(18) 0.16(3) -0.032(17) -0.08(2) 0.055(16) C34 0.14(2) 0.117(18) 0.16(3) -0.032(17) -0.08(2) 0.055(16) C35 0.14(2) 0.117(18) 0.16(3) -0.032(17) -0.08(2) 0.055(16) C36 0.14(2) 0.117(18) 0.16(3) -0.032(17) -0.08(2) 0.055(16) C37 0.14(2) 0.117(18) 0.16(3) -0.032(17) -0.08(2) 0.055(16) O11 0.36(8) 0.21(5) 0.28(7) -0.10(5) 0.10(6) 0.05(5) O12 0.36(8) 0.21(5) 0.28(7) -0.10(5) 0.10(6) 0.05(5) O13 0.36(8) 0.21(5) 0.28(7) -0.10(5) 0.10(6) 0.05(5) _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 O1W Ca1 2.421(19) . ? O2W Ca1 2.381(18) . ? O3W Ca1 2.51(2) . ? O4W Ca1 2.55(2) . ? Ca1 O9 2.385(18) 6_665 ? Ca1 O2 2.398(16) . ? Ca1 O1 2.432(17) . ? Ca1 O10 2.450(19) 6_665 ? C1 O1 1.22(3) . ? C1 N1 1.34(3) . ? C1 N2 1.39(3) . ? C2 N1 1.45(3) . ? C2 N3 1.47(3) . ? C2 C3 1.53(4) . ? C2 H2 0.9900 . ? C3 N2 1.44(3) . ? C3 N4 1.44(3) . ? C3 H3 0.9900 . ? C4 O6 1.24(3) . ? C4 N3 1.34(3) . ? C4 N4 1.36(3) . ? C5 N2 1.43(3) . ? C5 N5 1.43(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.47(3) . ? C6 N4 1.48(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.20(3) . ? C7 N6 1.37(3) . ? C7 N5 1.38(3) . ? C8 N7 1.44(3) . ? C8 N5 1.47(3) . ? C8 C9 1.54(3) . ? C8 H8 0.9900 . ? C9 N8 1.44(3) . ? C9 N6 1.45(3) . ? C9 H9 0.9900 . ? C10 O7 1.23(3) . ? C10 N7 1.35(3) . ? C10 N8 1.38(3) . ? C11 N9 1.44(3) . ? C11 N6 1.46(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.45(3) . ? C12 N8 1.47(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.24(3) . ? C13 N10 1.37(3) . ? C13 N9 1.38(3) . ? C14 N9 1.45(3) . ? C14 N11 1.45(3) . ? C14 C15 1.57(3) . ? C14 H14 0.9900 . ? C15 N10 1.44(3) . ? C15 N12 1.47(3) . ? C15 H15 0.9900 . ? C16 O8 1.24(3) . ? C16 N12 1.35(3) . ? C16 N11 1.37(3) . ? C17 N13 1.43(3) . ? C17 N10 1.46(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.44(3) . ? C18 N12 1.44(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.22(3) . ? C19 N14 1.37(3) . ? C19 N13 1.39(3) . ? C20 N13 1.44(3) . ? C20 N15 1.46(3) . ? C20 C21 1.57(4) . ? C20 H20 0.9900 . ? C21 N14 1.45(4) . ? C21 N16 1.45(3) . ? C21 H21 0.9900 . ? C22 O9 1.22(3) . ? C22 N16 1.35(3) . ? C22 N15 1.39(3) . ? C23 N14 1.45(4) . ? C23 N17 1.46(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.41(3) . ? C24 N19 1.50(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.20(3) . ? C25 N18 1.36(3) . ? C25 N17 1.40(4) . ? C26 N19 1.42(4) . ? C26 N17 1.48(3) . ? C26 C27 1.50(4) . ? C26 H26 0.9900 . ? C27 N18 1.44(3) . ? C27 N20 1.46(3) . ? C27 H27 0.9900 . ? C28 O10 1.22(3) . ? C28 N20 1.36(3) . ? C28 N19 1.40(3) . ? C29 N1 1.44(4) . ? C29 N18 1.47(4) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.46(3) . ? C30 N3 1.46(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? O9 Ca1 2.385(18) 5_544 ? O10 Ca1 2.450(19) 5_544 ? C31 C32 1.388(10) . ? C31 C36 1.424(10) . ? C31 H31 0.9400 . ? C32 C33 1.390(10) . ? C32 H32 0.9400 . ? C33 C34 1.390(10) . ? C33 O11 1.41(7) . ? C34 C35 1.427(10) . ? C34 H34 0.9400 . ? C35 C36 1.426(10) . ? C35 H35 0.9400 . ? C36 C37 1.39(5) . ? C37 O13 1.296(10) . ? C37 O12 1.31(9) . ? O11 H11 0.8300 . ? O12 H12 0.8300 . ? 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 O2W Ca1 O9 81.5(7) . 6_665 ? O2W Ca1 O2 112.8(7) . . ? O9 Ca1 O2 132.2(6) 6_665 . ? O2W Ca1 O1W 141.4(7) . . ? O9 Ca1 O1W 114.2(7) 6_665 . ? O2 Ca1 O1W 83.4(7) . . ? O2W Ca1 O1 73.4(6) . . ? O9 Ca1 O1 148.4(6) 6_665 . ? O2 Ca1 O1 76.5(6) . . ? O1W Ca1 O1 77.3(6) . . ? O2W Ca1 O10 75.8(7) . 6_665 ? O9 Ca1 O10 75.1(6) 6_665 6_665 ? O2 Ca1 O10 151.2(6) . 6_665 ? O1W Ca1 O10 74.9(7) . 6_665 ? O1 Ca1 O10 80.3(6) . 6_665 ? O2W Ca1 O3W 146.9(7) . . ? O9 Ca1 O3W 73.2(7) 6_665 . ? O2 Ca1 O3W 72.3(7) . . ? O1W Ca1 O3W 70.2(7) . . ? O1 Ca1 O3W 136.8(6) . . ? O10 Ca1 O3W 116.2(7) 6_665 . ? O2W Ca1 O4W 70.7(7) . . ? O9 Ca1 O4W 72.8(7) 6_665 . ? O2 Ca1 O4W 70.3(6) . . ? O1W Ca1 O4W 146.3(7) . . ? O1 Ca1 O4W 114.9(7) . . ? O10 Ca1 O4W 136.2(6) 6_665 . ? O3W Ca1 O4W 81.6(8) . . ? O1 C1 N1 127(2) . . ? O1 C1 N2 125(2) . . ? N1 C1 N2 108(2) . . ? N1 C2 N3 114(2) . . ? N1 C2 C3 104(2) . . ? N3 C2 C3 103(2) . . ? N1 C2 H2 111.7 . . ? N3 C2 H2 111.7 . . ? C3 C2 H2 111.7 . . ? N2 C3 N4 116(2) . . ? N2 C3 C2 103(2) . . ? N4 C3 C2 104(2) . . ? N2 C3 H3 111.3 . . ? N4 C3 H3 111.3 . . ? C2 C3 H3 111.3 . . ? O6 C4 N3 126(2) . . ? O6 C4 N4 125(2) . . ? N3 C4 N4 109(2) . . ? N2 C5 N5 113.8(19) . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? N5 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N7 C6 N4 112.8(18) . . ? N7 C6 H6A 109.0 . . ? N4 C6 H6A 109.0 . . ? N7 C6 H6B 109.0 . . ? N4 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? O2 C7 N6 126(2) . . ? O2 C7 N5 126(2) . . ? N6 C7 N5 108(2) . . ? N7 C8 N5 114.7(19) . . ? N7 C8 C9 103.2(17) . . ? N5 C8 C9 102.7(18) . . ? N7 C8 H8 111.8 . . ? N5 C8 H8 111.8 . . ? C9 C8 H8 111.8 . . ? N8 C9 N6 115.2(18) . . ? N8 C9 C8 103.3(18) . . ? N6 C9 C8 104.0(17) . . ? N8 C9 H9 111.3 . . ? N6 C9 H9 111.3 . . ? C8 C9 H9 111.3 . . ? O7 C10 N7 127(2) . . ? O7 C10 N8 125(2) . . ? N7 C10 N8 107.1(19) . . ? N9 C11 N6 113.4(19) . . ? N9 C11 H11A 108.9 . . ? N6 C11 H11A 108.9 . . ? N9 C11 H11B 108.9 . . ? N6 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N11 C12 N8 114.1(18) . . ? N11 C12 H12A 108.7 . . ? N8 C12 H12A 108.7 . . ? N11 C12 H12B 108.7 . . ? N8 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? O3 C13 N10 127(2) . . ? O3 C13 N9 124(2) . . ? N10 C13 N9 109(2) . . ? N9 C14 N11 115.9(18) . . ? N9 C14 C15 102.8(17) . . ? N11 C14 C15 103.3(17) . . ? N9 C14 H14 111.4 . . ? N11 C14 H14 111.4 . . ? C15 C14 H14 111.4 . . ? N10 C15 N12 115.1(18) . . ? N10 C15 C14 103.6(16) . . ? N12 C15 C14 102.1(17) . . ? N10 C15 H15 111.8 . . ? N12 C15 H15 111.8 . . ? C14 C15 H15 111.8 . . ? O8 C16 N12 126(2) . . ? O8 C16 N11 125(2) . . ? N12 C16 N11 109(2) . . ? N13 C17 N10 113.9(19) . . ? N13 C17 H17A 108.8 . . ? N10 C17 H17A 108.8 . . ? N13 C17 H17B 108.8 . . ? N10 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? N15 C18 N12 114.3(18) . . ? N15 C18 H18A 108.7 . . ? N12 C18 H18A 108.7 . . ? N15 C18 H18B 108.7 . . ? N12 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? O4 C19 N14 127(2) . . ? O4 C19 N13 125(2) . . ? N14 C19 N13 108(2) . . ? N13 C20 N15 115.2(18) . . ? N13 C20 C21 103.8(19) . . ? N15 C20 C21 103.9(18) . . ? N13 C20 H20 111.2 . . ? N15 C20 H20 111.2 . . ? C21 C20 H20 111.2 . . ? N14 C21 N16 115(2) . . ? N14 C21 C20 102.6(19) . . ? N16 C21 C20 102.4(19) . . ? N14 C21 H21 112.1 . . ? N16 C21 H21 112.1 . . ? C20 C21 H21 112.1 . . ? O9 C22 N16 127(2) . . ? O9 C22 N15 124(2) . . ? N16 C22 N15 109(2) . . ? N14 C23 N17 112(2) . . ? N14 C23 H23A 109.3 . . ? N17 C23 H23A 109.3 . . ? N14 C23 H23B 109.3 . . ? N17 C23 H23B 109.3 . . ? H23A C23 H23B 107.9 . . ? N16 C24 N19 113(2) . . ? N16 C24 H24A 109.0 . . ? N19 C24 H24A 109.0 . . ? N16 C24 H24B 109.0 . . ? N19 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? O5 C25 N18 128(3) . . ? O5 C25 N17 125(2) . . ? N18 C25 N17 107(2) . . ? N19 C26 N17 114(2) . . ? N19 C26 C27 105(2) . . ? N17 C26 C27 104(2) . . ? N19 C26 H26 111.4 . . ? N17 C26 H26 111.4 . . ? C27 C26 H26 111.4 . . ? N18 C27 N20 115(2) . . ? N18 C27 C26 104(2) . . ? N20 C27 C26 103(2) . . ? N18 C27 H27 111.4 . . ? N20 C27 H27 111.4 . . ? C26 C27 H27 111.4 . . ? O10 C28 N20 127(2) . . ? O10 C28 N19 127(2) . . ? N20 C28 N19 105(2) . . ? N1 C29 N18 114(2) . . ? N1 C29 H29A 108.8 . . ? N18 C29 H29A 108.8 . . ? N1 C29 H29B 108.8 . . ? N18 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? N20 C30 N3 113.5(19) . . ? N20 C30 H30A 108.9 . . ? N3 C30 H30A 108.9 . . ? N20 C30 H30B 108.9 . . ? N3 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C1 N1 C29 120(2) . . ? C1 N1 C2 112(2) . . ? C29 N1 C2 125(2) . . ? C1 N2 C5 124(2) . . ? C1 N2 C3 112(2) . . ? C5 N2 C3 123(2) . . ? C4 N3 C30 123(2) . . ? C4 N3 C2 112(2) . . ? C30 N3 C2 125(2) . . ? C4 N4 C3 112(2) . . ? C4 N4 C6 122(2) . . ? C3 N4 C6 124(2) . . ? C7 N5 C5 122(2) . . ? C7 N5 C8 112.5(18) . . ? C5 N5 C8 124.8(19) . . ? C7 N6 C9 113.1(18) . . ? C7 N6 C11 120(2) . . ? C9 N6 C11 126.0(18) . . ? C10 N7 C8 113.6(19) . . ? C10 N7 C6 120.2(19) . . ? C8 N7 C6 126.0(19) . . ? C10 N8 C9 112.7(18) . . ? C10 N8 C12 122(2) . . ? C9 N8 C12 124.8(19) . . ? C13 N9 C11 124(2) . . ? C13 N9 C14 111.8(18) . . ? C11 N9 C14 123.5(19) . . ? C13 N10 C15 112.1(18) . . ? C13 N10 C17 121(2) . . ? C15 N10 C17 123.1(19) . . ? C16 N11 C12 122(2) . . ? C16 N11 C14 112.2(18) . . ? C12 N11 C14 123.4(19) . . ? C16 N12 C18 123.8(19) . . ? C16 N12 C15 112.6(18) . . ? C18 N12 C15 123.3(19) . . ? C19 N13 C17 123(2) . . ? C19 N13 C20 112.3(19) . . ? C17 N13 C20 125(2) . . ? C19 N14 C23 121(2) . . ? C19 N14 C21 113(2) . . ? C23 N14 C21 125(2) . . ? C22 N15 C18 120(2) . . ? C22 N15 C20 111(2) . . ? C18 N15 C20 127(2) . . ? C22 N16 C24 122(2) . . ? C22 N16 C21 114(2) . . ? C24 N16 C21 125(2) . . ? C25 N17 C23 121(2) . . ? C25 N17 C26 111(2) . . ? C23 N17 C26 126(2) . . ? C25 N18 C27 114(2) . . ? C25 N18 C29 120(2) . . ? C27 N18 C29 126(2) . . ? C28 N19 C26 113(2) . . ? C28 N19 C24 121(2) . . ? C26 N19 C24 125(2) . . ? C28 N20 C30 120(2) . . ? C28 N20 C27 113(2) . . ? C30 N20 C27 124(2) . . ? C1 O1 Ca1 149.2(17) . . ? C7 O2 Ca1 150.2(16) . . ? C22 O9 Ca1 152.7(18) . 5_544 ? C28 O10 Ca1 150.0(18) . 5_544 ? C32 C31 C36 122.3(19) . . ? C32 C31 H31 118.8 . . ? C36 C31 H31 118.8 . . ? C31 C32 C33 118(3) . . ? C31 C32 H32 121.2 . . ? C33 C32 H32 121.2 . . ? C34 C33 C32 123(3) . . ? C34 C33 O11 120(5) . . ? C32 C33 O11 118(4) . . ? C33 C34 C35 120.7(19) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C36 C35 C34 117(2) . . ? C36 C35 H35 121.4 . . ? C34 C35 H35 121.4 . . ? C37 C36 C31 122(4) . . ? C37 C36 C35 118(4) . . ? C31 C36 C35 119.5(18) . . ? O13 C37 O12 115(6) . . ? O13 C37 C36 116(8) . . ? O12 C37 C36 129(5) . . ? C33 O11 H11 109.5 . . ? C37 O12 H12 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.991 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.098 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 1.000 0.002 1610 626 ' ' 2 0.062 0.580 0.094 49 10 ' ' 3 -0.062 0.420 0.594 49 10 ' ' 4 0.087 0.440 0.965 24 8 ' ' 5 0.352 0.913 0.299 24 8 ' ' 6 0.420 0.481 0.761 49 10 ' ' 7 0.440 0.352 0.132 24 8 ' ' 8 0.481 0.062 0.928 49 10 ' ' 9 0.518 0.938 0.428 49 10 ' ' 10 0.580 0.518 0.261 49 10 ' ' 11 0.560 0.647 0.632 24 8 ' ' 12 0.647 0.087 0.799 24 8 ' ' 13 0.913 0.560 0.465 24 8 ' ' _platon_squeeze_details ; ; data_compound2_no_squeeze _database_code_depnum_ccdc_archive 'CCDC 895165' #TrackingRef '- compound 1 -3.cif' no squeeze _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H40 N25 O20' _chemical_formula_weight 1190.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 15.8841(18) _cell_length_b 12.4803(14) _cell_length_c 14.1747(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2810.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1230 _exptl_absorpt_coefficient_mu 0.116 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18741 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.99 _reflns_number_total 5287 _reflns_number_gt 4847 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1396P)^2^+0.8217P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.8(14) _refine_ls_number_reflns 5287 _refine_ls_number_parameters 438 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1874 _refine_ls_wR_factor_gt 0.1823 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.165 _refine_ls_shift/su_mean 0.017 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.17062(19) -0.1949(2) -0.0759(2) 0.0259(7) Uani 1 1 d . . . C2 C 0.1309(2) -0.1699(3) 0.0901(2) 0.0274(7) Uani 1 1 d . . . H2A H 0.1192 -0.2461 0.0857 0.033 Uiso 1 1 calc R . . H2B H 0.1685 -0.1590 0.1431 0.033 Uiso 1 1 calc R . . C3 C -0.02338(19) -0.1540(3) 0.0835(2) 0.0258(7) Uani 1 1 d . . . C4 C -0.1718(2) -0.0995(3) 0.0960(2) 0.0290(7) Uani 1 1 d . . . H4A H -0.1806 -0.1764 0.0953 0.035 Uiso 1 1 calc R . . H4B H -0.2005 -0.0711 0.1510 0.035 Uiso 1 1 calc R . . C5 C -0.21564(19) -0.1113(3) -0.0696(2) 0.0273(7) Uani 1 1 d . . . C6 C -0.2650(2) -0.0821(3) -0.2326(2) 0.0301(7) Uani 1 1 d . . . H6A H -0.2727 -0.1592 -0.2309 0.036 Uiso 1 1 calc R . . H6B H -0.3174 -0.0505 -0.2542 0.036 Uiso 1 1 calc R . . C7 C -0.1361(2) -0.1262(3) -0.3209(2) 0.0302(7) Uani 1 1 d . . . C8 C -0.0181(2) -0.1358(3) -0.4325(2) 0.0335(8) Uani 1 1 d . . . H8A H -0.0171 -0.1163 -0.4987 0.040 Uiso 1 1 calc R . . H8B H -0.0297 -0.2120 -0.4287 0.040 Uiso 1 1 calc R . . C9 C -0.1167(2) 0.0250(3) -0.4163(2) 0.0296(7) Uani 1 1 d . . . H9 H -0.1313 0.0253 -0.4835 0.035 Uiso 1 1 calc R . . C10 C -0.1959(2) 0.0415(3) -0.3539(2) 0.0291(7) Uani 1 1 d . . . H10 H -0.2466 0.0509 -0.3924 0.035 Uiso 1 1 calc R . . C11 C -0.1004(2) 0.1808(3) -0.3263(2) 0.0266(7) Uani 1 1 d . . . C12 C -0.2329(2) 0.1888(3) -0.2355(2) 0.0278(7) Uani 1 1 d . . . H12A H -0.2220 0.2653 -0.2359 0.033 Uiso 1 1 calc R . . H12B H -0.2903 0.1780 -0.2568 0.033 Uiso 1 1 calc R . . C13 C -0.0474(2) 0.0121(3) 0.1563(2) 0.0248(6) Uani 1 1 d . . . H13 H -0.0699 0.0167 0.2206 0.030 Uiso 1 1 calc R . . C14 C 0.23856(19) -0.0547(3) 0.0027(2) 0.0275(7) Uani 1 1 d . . . H14 H 0.2834 -0.0712 0.0479 0.033 Uiso 1 1 calc R . . C15 C 0.2710(2) -0.0602(3) -0.1012(2) 0.0278(7) Uani 1 1 d . . . H15 H 0.3320 -0.0717 -0.1039 0.033 Uiso 1 1 calc R . . C16 C -0.1943(3) -0.0720(3) -0.6381(2) 0.0361(8) Uani 1 1 d . . . C17 C -0.2374(2) -0.1414(3) -0.5667(2) 0.0306(7) Uani 1 1 d . . . C18 C -0.1982(2) -0.2329(3) -0.5328(2) 0.0316(7) Uani 1 1 d . . . H18 H -0.1468 -0.2537 -0.5583 0.038 Uiso 1 1 calc R . . C19 C -0.2337(2) -0.2941(3) -0.4619(3) 0.0334(7) Uani 1 1 d . . . H19 H -0.2067 -0.3557 -0.4408 0.040 Uiso 1 1 calc R . . C20 C -0.3102(2) -0.2630(3) -0.4222(3) 0.0338(7) Uani 1 1 d . . . C21 C -0.3514(2) -0.1730(3) -0.4572(3) 0.0383(8) Uani 1 1 d . . . H21 H -0.4033 -0.1529 -0.4324 0.046 Uiso 1 1 calc R . . C22 C -0.3152(2) -0.1133(3) -0.5289(3) 0.0343(8) Uani 1 1 d . . . H22 H -0.3433 -0.0536 -0.5521 0.041 Uiso 1 1 calc R . . N1 N -0.19953(19) -0.0570(2) -0.2994(2) 0.0316(6) Uani 1 1 d . . . N2 N -0.08561(19) -0.0785(2) -0.3870(2) 0.0304(6) Uani 1 1 d . . . N3 N -0.06443(19) 0.1154(2) -0.39225(19) 0.0301(6) Uani 1 1 d . . . N4 N -0.17609(17) 0.1373(2) -0.3016(2) 0.0297(6) Uani 1 1 d . . . N5 N -0.24769(19) -0.0444(2) -0.1378(2) 0.0329(6) Uani 1 1 d . . . N6 N -0.20957(17) -0.0540(2) 0.0126(2) 0.0288(6) Uani 1 1 d . . . N7 N -0.08261(17) -0.0786(2) 0.10536(19) 0.0270(6) Uani 1 1 d . . . N8 N 0.05293(17) -0.1136(2) 0.1079(2) 0.0282(6) Uani 1 1 d . . . N9 N 0.17269(16) -0.1354(2) 0.0045(2) 0.0275(6) Uani 1 1 d . . . N10 N 0.22544(17) -0.1498(2) -0.1396(2) 0.0285(6) Uani 1 1 d . . . O1 O -0.12582(16) -0.21470(19) -0.28781(18) 0.0368(6) Uani 1 1 d . . . O2 O -0.19752(14) -0.20471(18) -0.08012(19) 0.0322(5) Uani 1 1 d . . . O1W O -0.04901(19) -0.3240(2) -0.1403(2) 0.0509(7) Uani 1 1 d . . . O3 O -0.03705(15) -0.24127(18) 0.04838(18) 0.0339(6) Uani 1 1 d . . . O2W O 0.0000 0.0000 -0.1418(14) 0.251(8) Uani 1 2 d S . . O4 O 0.12894(15) -0.27520(19) -0.08959(18) 0.0334(5) Uani 1 1 d . . . O3W O -0.0122(2) -0.2431(3) -0.7047(3) 0.0687(9) Uani 1 1 d . . . O5 O -0.07075(15) 0.26366(18) -0.29608(17) 0.0330(5) Uani 1 1 d . . . O4W O -0.4362(6) 0.0576(7) -0.3947(8) 0.168(3) Uani 1 1 d . . . O6 O -0.2360(2) 0.0031(2) -0.67614(19) 0.0449(7) Uani 1 1 d . . . O5W O 0.1258(3) -0.4840(3) -0.2083(6) 0.139(3) Uani 1 1 d . . . O7 O -0.1192(2) -0.0868(3) -0.6551(3) 0.0679(11) Uani 1 1 d . . . H7 H -0.1017 -0.1366 -0.6229 0.102 Uiso 1 1 calc R . . O6W O 0.0184(13) -0.4433(9) 0.1327(10) 0.287(9) Uani 1 1 d . . . O8 O -0.34613(19) -0.3171(2) -0.3500(2) 0.0458(7) Uani 1 1 d . . . H8 H -0.3164 -0.3683 -0.3357 0.069 Uiso 1 1 calc R . . O7W O 0.0667(5) -0.4730(5) -0.0246(6) 0.139(2) Uani 1 1 d . . . O8W O -0.4403(6) 0.0586(8) -0.2922(6) 0.159(3) Uani 1 1 d . . . O9W O -0.4704(6) 0.0768(7) -0.5980(7) 0.170(4) 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 C1 0.0239(15) 0.0229(15) 0.0309(17) 0.0016(13) -0.0023(13) 0.0045(12) C2 0.0286(15) 0.0237(15) 0.0301(17) 0.0028(13) -0.0015(13) 0.0059(12) C3 0.0299(16) 0.0269(16) 0.0206(14) 0.0025(12) -0.0005(12) -0.0005(12) C4 0.0279(16) 0.0290(16) 0.0302(17) 0.0047(13) 0.0063(13) -0.0038(13) C5 0.0224(14) 0.0244(15) 0.0352(18) 0.0036(13) 0.0021(12) -0.0052(12) C6 0.0300(16) 0.0265(16) 0.0339(18) -0.0024(13) -0.0075(13) -0.0064(13) C7 0.0358(17) 0.0246(16) 0.0302(17) -0.0015(13) -0.0127(13) -0.0023(13) C8 0.046(2) 0.0241(15) 0.0302(18) -0.0097(13) -0.0053(14) 0.0050(14) C9 0.0391(17) 0.0277(17) 0.0219(15) 0.0002(13) -0.0100(14) 0.0035(14) C10 0.0287(15) 0.0307(16) 0.0278(16) -0.0011(13) -0.0120(13) 0.0000(13) C11 0.0322(16) 0.0248(16) 0.0228(15) 0.0042(12) -0.0053(12) 0.0028(13) C12 0.0266(15) 0.0253(15) 0.0314(17) 0.0002(13) -0.0015(13) 0.0082(12) C13 0.0296(16) 0.0279(15) 0.0169(13) -0.0010(11) 0.0034(12) -0.0010(12) C14 0.0227(14) 0.0278(16) 0.0322(17) 0.0012(13) -0.0060(13) 0.0009(12) C15 0.0215(14) 0.0248(15) 0.0370(18) -0.0011(13) -0.0003(13) 0.0006(12) C16 0.051(2) 0.0318(17) 0.0251(16) 0.0014(14) -0.0019(16) -0.0020(16) C17 0.0397(18) 0.0309(17) 0.0211(16) -0.0038(13) -0.0063(13) -0.0043(14) C18 0.0375(17) 0.0289(16) 0.0285(17) -0.0030(13) -0.0005(14) -0.0029(14) C19 0.0425(18) 0.0265(16) 0.0311(17) 0.0016(13) -0.0072(15) -0.0016(15) C20 0.0422(18) 0.0261(16) 0.0330(18) -0.0026(14) -0.0004(15) -0.0057(14) C21 0.0345(18) 0.0321(18) 0.048(2) 0.0004(16) 0.0015(16) -0.0044(15) C22 0.0380(18) 0.0285(17) 0.0363(19) 0.0020(14) -0.0045(15) -0.0018(14) N1 0.0343(14) 0.0270(13) 0.0333(15) 0.0014(12) -0.0069(12) 0.0011(12) N2 0.0380(15) 0.0228(13) 0.0304(15) 0.0014(11) -0.0039(12) 0.0014(12) N3 0.0358(15) 0.0264(14) 0.0280(14) -0.0008(11) 0.0015(11) 0.0016(12) N4 0.0305(14) 0.0270(13) 0.0317(15) -0.0034(12) -0.0028(12) -0.0003(11) N5 0.0367(15) 0.0284(14) 0.0336(15) -0.0016(12) -0.0059(12) -0.0009(12) N6 0.0290(13) 0.0244(13) 0.0331(15) 0.0023(11) -0.0002(11) 0.0001(11) N7 0.0286(13) 0.0228(13) 0.0296(15) -0.0007(11) 0.0020(11) -0.0008(11) N8 0.0262(13) 0.0257(14) 0.0327(15) -0.0003(11) -0.0001(11) 0.0030(11) N9 0.0278(13) 0.0284(14) 0.0264(14) 0.0003(11) -0.0011(11) -0.0017(11) N10 0.0283(13) 0.0274(13) 0.0298(14) 0.0005(11) 0.0045(11) -0.0009(11) O1 0.0453(14) 0.0271(12) 0.0381(14) 0.0010(11) -0.0065(11) -0.0005(10) O2 0.0327(12) 0.0213(11) 0.0424(14) -0.0004(10) -0.0003(10) -0.0035(9) O1W 0.0480(15) 0.0468(16) 0.0579(18) -0.0004(14) 0.0004(14) -0.0027(13) O3 0.0390(13) 0.0219(11) 0.0408(14) -0.0041(10) -0.0048(10) -0.0021(10) O2W 0.194(14) 0.32(2) 0.241(17) 0.000 0.000 -0.001(16) O4 0.0401(13) 0.0243(12) 0.0359(13) -0.0024(10) 0.0015(10) -0.0039(10) O3W 0.066(2) 0.073(2) 0.067(2) 0.005(2) -0.0048(17) 0.0132(19) O5 0.0385(12) 0.0239(11) 0.0366(13) -0.0030(10) -0.0004(10) -0.0025(10) O4W 0.154(6) 0.128(6) 0.221(10) 0.036(6) 0.053(7) 0.045(5) O6 0.0623(17) 0.0320(13) 0.0403(14) 0.0062(11) -0.0053(13) 0.0006(13) O5W 0.080(3) 0.0301(18) 0.307(9) 0.002(3) 0.080(4) -0.0075(18) O7 0.0567(19) 0.074(2) 0.073(2) 0.036(2) 0.0267(18) 0.0195(17) O6W 0.47(3) 0.133(7) 0.262(12) 0.021(8) -0.126(16) 0.029(12) O8 0.0519(16) 0.0349(14) 0.0507(17) 0.0102(12) 0.0118(13) 0.0012(12) O7W 0.160(6) 0.089(4) 0.168(6) 0.019(4) -0.016(5) -0.007(4) O8W 0.144(6) 0.177(7) 0.156(7) 0.001(6) -0.029(5) 0.017(6) O9W 0.166(7) 0.135(6) 0.209(8) 0.056(6) 0.035(6) 0.075(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O4 1.217(4) . ? C1 N9 1.360(4) . ? C1 N10 1.375(4) . ? C2 N8 1.446(4) . ? C2 N9 1.449(4) . ? C3 O3 1.217(4) . ? C3 N8 1.358(4) . ? C3 N7 1.366(4) . ? C4 N6 1.442(4) . ? C4 N7 1.447(4) . ? C5 O2 1.210(4) . ? C5 N6 1.370(4) . ? C5 N5 1.376(4) . ? C6 N1 1.442(5) . ? C6 N5 1.450(4) . ? C7 O1 1.211(4) . ? C7 N1 1.362(5) . ? C7 N2 1.369(5) . ? C8 N2 1.440(5) . ? C8 N3 1.453(5) 2 ? C9 N3 1.442(4) . ? C9 N2 1.445(4) . ? C9 C10 1.551(5) . ? C10 N4 1.442(4) . ? C10 N1 1.452(4) . ? C11 O5 1.214(4) . ? C11 N4 1.365(4) . ? C11 N3 1.367(4) . ? C12 N10 1.449(4) 2 ? C12 N4 1.450(4) . ? C13 N8 1.443(4) 2 ? C13 N7 1.454(4) . ? C13 C13 1.537(6) 2 ? C14 N6 1.440(4) 2 ? C14 N9 1.453(4) . ? C14 C15 1.562(5) . ? C15 N10 1.439(4) . ? C15 N5 1.452(4) 2 ? C16 O7 1.231(5) . ? C16 O6 1.268(5) . ? C16 C17 1.497(5) . ? C17 C18 1.388(5) . ? C17 C22 1.392(5) . ? C18 C19 1.382(5) . ? C19 C20 1.394(5) . ? C20 O8 1.353(5) . ? C20 C21 1.392(5) . ? C21 C22 1.385(5) . ? N3 C8 1.453(5) 2 ? N5 C15 1.452(4) 2 ? N6 C14 1.440(4) 2 ? N8 C13 1.443(4) 2 ? N10 C12 1.449(4) 2 ? O4W O8W 1.455(11) . ? O6W O6W 1.53(3) 2_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 C1 N9 126.6(3) . . ? O4 C1 N10 125.2(3) . . ? N9 C1 N10 108.2(3) . . ? N8 C2 N9 113.2(3) . . ? O3 C3 N8 126.6(3) . . ? O3 C3 N7 125.9(3) . . ? N8 C3 N7 107.5(3) . . ? N6 C4 N7 114.3(3) . . ? O2 C5 N6 126.2(3) . . ? O2 C5 N5 125.9(3) . . ? N6 C5 N5 107.9(3) . . ? N1 C6 N5 113.6(3) . . ? O1 C7 N1 126.3(3) . . ? O1 C7 N2 125.6(3) . . ? N1 C7 N2 108.1(3) . . ? N2 C8 N3 114.1(3) . 2 ? N3 C9 N2 115.8(3) . . ? N3 C9 C10 103.2(3) . . ? N2 C9 C10 103.4(3) . . ? N4 C10 N1 115.9(3) . . ? N4 C10 C9 103.1(3) . . ? N1 C10 C9 102.9(3) . . ? O5 C11 N4 126.1(3) . . ? O5 C11 N3 126.0(3) . . ? N4 C11 N3 107.8(3) . . ? N10 C12 N4 114.0(3) 2 . ? N8 C13 N7 115.1(2) 2 . ? N8 C13 C13 103.4(3) 2 2 ? N7 C13 C13 102.9(3) . 2 ? N6 C14 N9 114.9(3) 2 . ? N6 C14 C15 103.8(3) 2 . ? N9 C14 C15 102.9(3) . . ? N10 C15 N5 115.8(3) . 2 ? N10 C15 C14 103.0(3) . . ? N5 C15 C14 102.3(3) 2 . ? O7 C16 O6 122.2(4) . . ? O7 C16 C17 119.3(3) . . ? O6 C16 C17 118.4(4) . . ? C18 C17 C22 118.1(3) . . ? C18 C17 C16 120.4(3) . . ? C22 C17 C16 121.4(3) . . ? C19 C18 C17 121.6(3) . . ? C18 C19 C20 119.7(3) . . ? O8 C20 C21 118.3(3) . . ? O8 C20 C19 122.3(3) . . ? C21 C20 C19 119.4(3) . . ? C22 C21 C20 120.0(3) . . ? C21 C22 C17 121.1(3) . . ? C7 N1 C6 122.9(3) . . ? C7 N1 C10 112.9(3) . . ? C6 N1 C10 124.2(3) . . ? C7 N2 C8 121.8(3) . . ? C7 N2 C9 112.6(3) . . ? C8 N2 C9 124.7(3) . . ? C11 N3 C9 112.9(3) . . ? C11 N3 C8 122.8(3) . 2 ? C9 N3 C8 124.4(3) . 2 ? C11 N4 C10 112.9(3) . . ? C11 N4 C12 122.5(3) . . ? C10 N4 C12 124.4(3) . . ? C5 N5 C6 121.6(3) . . ? C5 N5 C15 112.9(3) . 2 ? C6 N5 C15 125.1(3) . 2 ? C5 N6 C14 112.7(3) . 2 ? C5 N6 C4 121.4(3) . . ? C14 N6 C4 125.7(3) 2 . ? C3 N7 C4 122.0(3) . . ? C3 N7 C13 112.6(3) . . ? C4 N7 C13 124.2(3) . . ? C3 N8 C13 113.2(3) . 2 ? C3 N8 C2 122.6(3) . . ? C13 N8 C2 124.2(3) 2 . ? C1 N9 C2 121.9(3) . . ? C1 N9 C14 112.4(3) . . ? C2 N9 C14 123.4(3) . . ? C1 N10 C15 112.8(3) . . ? C1 N10 C12 122.0(3) . 2 ? C15 N10 C12 125.1(3) . 2 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.670 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.094