data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Bharadwaj, Parimal' _publ_contact_author_email pkb@iitk.ac.in _publ_section_title ; Cryptand derived fluorescence signaling systems for sensing Hg(II) ion : a comparative study ; loop_ _publ_author_name K.Sadhu S.Sen P.Bharadwaj # Attachment '- L12.txt' data_L12 _database_code_depnum_ccdc_archive 'CCDC 787931' #TrackingRef '- L12.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H75 N5 O3, 2(C H2 Cl2)' _chemical_formula_sum 'C80 H79 Cl4 N5 O3' _chemical_formula_weight 1300.28 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.970(5) _cell_length_b 13.569(5) _cell_length_c 21.610(5) _cell_angle_alpha 74.456(5) _cell_angle_beta 87.681(5) _cell_angle_gamma 84.415(5) _cell_volume 3365(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 26.0 _exptl_crystal_description parallelopiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 0.230 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9685 _exptl_absorpt_correction_T_max 0.9773 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEX' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18815 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0747 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12899 _reflns_number_gt 9016 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 ( Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 2.1e' _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^)+(0.1644P)^2^+5.3377P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0037(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12899 _refine_ls_number_parameters 830 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1004 _refine_ls_R_factor_gt 0.0735 _refine_ls_wR_factor_ref 0.2354 _refine_ls_wR_factor_gt 0.1920 _refine_ls_goodness_of_fit_ref 0.849 _refine_ls_restrained_S_all 0.849 _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 Cl2 Cl 0.62669(9) -0.41538(8) 0.76980(5) 0.0438(3) Uani 1 1 d . . . Cl3 Cl 0.32192(8) -0.25287(8) 0.87221(5) 0.0413(3) Uani 1 1 d . . . Cl4 Cl 0.46354(10) -0.44578(9) 0.91483(6) 0.0517(3) Uani 1 1 d . . . Cl1 Cl 0.50674(10) -0.28292(10) 0.65931(6) 0.0554(3) Uani 1 1 d . . . O3 O 1.07577(19) 0.16478(16) 0.75963(10) 0.0219(5) Uani 1 1 d . . . O2 O 0.67249(18) 0.38502(16) 0.69921(11) 0.0220(5) Uani 1 1 d . . . O1 O 0.90603(19) 0.42763(17) 0.52727(11) 0.0246(5) Uani 1 1 d . . . N5 N 0.6504(2) -0.07259(19) 0.77788(12) 0.0184(5) Uani 1 1 d . . . N4 N 0.9257(2) -0.23005(19) 0.81426(12) 0.0182(5) Uani 1 1 d . . . N2 N 0.7204(2) 0.07511(19) 0.60759(12) 0.0198(6) Uani 1 1 d . . . C42 C 1.0184(3) -0.2083(3) 0.57856(17) 0.0337(9) Uani 1 1 d . . . H42 H 1.0744 -0.2623 0.5841 0.040 Uiso 1 1 calc R . . N3 N 0.4616(2) 0.06330(19) 0.81165(12) 0.0173(5) Uani 1 1 d . . . N1 N 0.9257(2) 0.35240(19) 0.70332(13) 0.0198(6) Uani 1 1 d . . . C26 C 1.0870(3) 0.0661(2) 0.87221(15) 0.0207(7) Uani 1 1 d . . . H26 H 1.0978 0.1235 0.8863 0.025 Uiso 1 1 calc R . . C63 C 0.9472(2) -0.4722(2) 0.88304(15) 0.0179(6) Uani 1 1 d . . . C65 C 0.4850(3) 0.0885(2) 0.91911(15) 0.0194(6) Uani 1 1 d . . . C19 C 0.5283(2) 0.2699(2) 0.74404(15) 0.0178(6) Uani 1 1 d . . . H19 H 0.5658 0.2445 0.7827 0.021 Uiso 1 1 calc R . . C18 C 0.4266(3) 0.2326(2) 0.73563(15) 0.0186(6) Uani 1 1 d . . . C78 C 0.5945(3) 0.1200(2) 0.91455(15) 0.0198(6) Uani 1 1 d . . . C20 C 0.3801(2) 0.1530(2) 0.79159(15) 0.0194(6) Uani 1 1 d . . . H20A H 0.3628 0.1829 0.8273 0.023 Uiso 1 1 calc R . . H20B H 0.3111 0.1321 0.7790 0.023 Uiso 1 1 calc R . . C3 C 0.8123(3) 0.3826(2) 0.51836(15) 0.0218(7) Uani 1 1 d . . . C22 C 0.5342(3) -0.0990(2) 0.78191(16) 0.0202(6) Uani 1 1 d . . . H22A H 0.5221 -0.1464 0.8235 0.024 Uiso 1 1 calc R . . H22B H 0.5238 -0.1345 0.7494 0.024 Uiso 1 1 calc R . . C50 C 0.9885(3) -0.4134(2) 0.82392(15) 0.0185(6) Uani 1 1 d . . . C15 C 0.5169(3) 0.3829(2) 0.63670(15) 0.0220(7) Uani 1 1 d . . . H15 H 0.5463 0.4336 0.6039 0.026 Uiso 1 1 calc R . . C51 C 1.0943(3) -0.4462(2) 0.80008(15) 0.0188(6) Uani 1 1 d . . . C21 C 0.4456(3) -0.0082(2) 0.77307(16) 0.0205(6) Uani 1 1 d . . . H21A H 0.4447 0.0296 0.7281 0.025 Uiso 1 1 calc R . . H21B H 0.3727 -0.0343 0.7838 0.025 Uiso 1 1 calc R . . C67 C 0.2927(3) 0.0938(2) 0.96886(15) 0.0221(7) Uani 1 1 d . . . H67 H 0.2720 0.0459 0.9487 0.027 Uiso 1 1 calc R . . C25 C 1.0757(2) 0.0746(2) 0.80723(15) 0.0197(6) Uani 1 1 d . . . C29 C 1.0563(3) -0.1065(2) 0.83023(16) 0.0205(7) Uani 1 1 d . . . C43 C 0.9144(3) -0.2209(3) 0.55767(17) 0.0327(8) Uani 1 1 d . . . C14 C 0.5735(3) 0.3445(2) 0.69484(15) 0.0196(6) Uani 1 1 d . . . C71 C 0.4315(3) 0.2007(2) 0.99020(15) 0.0217(7) Uani 1 1 d . . . C58 C 1.0117(3) -0.5622(2) 0.91877(16) 0.0217(7) Uani 1 1 d . . . C56 C 1.1574(3) -0.5366(2) 0.83622(16) 0.0224(7) Uani 1 1 d . . . C49 C 0.9194(3) -0.3190(2) 0.78733(15) 0.0189(6) Uani 1 1 d . . . H49A H 0.9453 -0.3010 0.7429 0.023 Uiso 1 1 calc R . . H49B H 0.8417 -0.3340 0.7879 0.023 Uiso 1 1 calc R . . C16 C 0.4178(3) 0.3451(2) 0.62844(16) 0.0232(7) Uani 1 1 d . . . H16 H 0.3809 0.3700 0.5895 0.028 Uiso 1 1 calc R . . C7 C 0.6776(3) 0.2559(2) 0.54505(15) 0.0202(7) Uani 1 1 d . . . C10 C 0.6759(3) -0.0094(2) 0.65648(15) 0.0202(6) Uani 1 1 d . . . H10A H 0.7214 -0.0729 0.6574 0.024 Uiso 1 1 calc R . . H10B H 0.5999 -0.0171 0.6458 0.024 Uiso 1 1 calc R . . C57 C 1.1154(3) -0.5921(2) 0.89455(17) 0.0247(7) Uani 1 1 d . . . H57 H 1.1573 -0.6506 0.9180 0.030 Uiso 1 1 calc R . . C17 C 0.3710(3) 0.2694(2) 0.67783(15) 0.0209(7) Uani 1 1 d . . . H17 H 0.3038 0.2444 0.6717 0.025 Uiso 1 1 calc R . . C70 C 0.3483(3) 0.2382(3) 1.03044(16) 0.0252(7) Uani 1 1 d . . . H70 H 0.3659 0.2872 1.0506 0.030 Uiso 1 1 calc R . . C9 C 0.6347(3) 0.1614(2) 0.59083(16) 0.0220(7) Uani 1 1 d . . . H9A H 0.6068 0.1785 0.6298 0.026 Uiso 1 1 calc R . . H9B H 0.5724 0.1410 0.5713 0.026 Uiso 1 1 calc R . . C66 C 0.4030(3) 0.1267(2) 0.95813(14) 0.0191(6) Uani 1 1 d . . . C35 C 0.8487(3) -0.0443(3) 0.56129(16) 0.0252(7) Uani 1 1 d . . . C32 C 0.8485(3) -0.1430(2) 0.78157(15) 0.0191(6) Uani 1 1 d . . . H32A H 0.8719 -0.1206 0.7369 0.023 Uiso 1 1 calc R . . H32B H 0.8545 -0.0867 0.8006 0.023 Uiso 1 1 calc R . . C33 C 0.7264(2) -0.1656(2) 0.78436(15) 0.0178(6) Uani 1 1 d . . . H33A H 0.7127 -0.1966 0.7502 0.021 Uiso 1 1 calc R . . H33B H 0.7113 -0.2144 0.8250 0.021 Uiso 1 1 calc R . . C30 C 1.0615(3) -0.0118(2) 0.78649(16) 0.0209(7) Uani 1 1 d . . . H30 H 1.0553 -0.0059 0.7429 0.025 Uiso 1 1 calc R . . C69 C 0.2446(3) 0.2034(3) 1.03947(16) 0.0262(7) Uani 1 1 d . . . H69 H 0.1922 0.2272 1.0663 0.031 Uiso 1 1 calc R . . C8 C 0.7716(3) 0.2975(2) 0.56135(15) 0.0208(7) Uani 1 1 d . . . H8 H 0.8064 0.2683 0.6006 0.025 Uiso 1 1 calc R . . C11 C 0.6761(3) 0.0116(2) 0.72294(15) 0.0188(6) Uani 1 1 d . . . H11A H 0.7496 0.0315 0.7292 0.023 Uiso 1 1 calc R . . H11B H 0.6222 0.0698 0.7227 0.023 Uiso 1 1 calc R . . C55 C 1.2642(3) -0.5692(3) 0.81182(18) 0.0275(8) Uani 1 1 d . . . H55 H 1.3053 -0.6281 0.8353 0.033 Uiso 1 1 calc R . . C1 C 0.9077(3) 0.4244(3) 0.64026(16) 0.0238(7) Uani 1 1 d . . . H1A H 0.9353 0.4892 0.6403 0.029 Uiso 1 1 calc R . . H1B H 0.8277 0.4368 0.6322 0.029 Uiso 1 1 calc R . . C2 C 0.9662(3) 0.3853(3) 0.58586(16) 0.0246(7) Uani 1 1 d . . . H2A H 1.0425 0.4051 0.5801 0.029 Uiso 1 1 calc R . . H2B H 0.9696 0.3109 0.5969 0.029 Uiso 1 1 calc R . . C64 C 0.4578(3) 0.0144(2) 0.88143(15) 0.0192(6) Uani 1 1 d . . . H64A H 0.5115 -0.0458 0.8916 0.023 Uiso 1 1 calc R . . H64B H 0.3836 -0.0078 0.8938 0.023 Uiso 1 1 calc R . . C48 C 0.8255(3) -0.1380(3) 0.54921(16) 0.0285(8) Uani 1 1 d . . . C73 C 0.6216(3) 0.1933(3) 0.94782(16) 0.0244(7) Uani 1 1 d . . . C62 C 0.8413(3) -0.4440(2) 0.91036(16) 0.0225(7) Uani 1 1 d . . . H62 H 0.7971 -0.3862 0.8881 0.027 Uiso 1 1 calc R . . C12 C 0.8489(3) 0.3846(3) 0.75047(16) 0.0229(7) Uani 1 1 d . . . H12A H 0.8355 0.4589 0.7381 0.027 Uiso 1 1 calc R . . H12B H 0.8842 0.3643 0.7921 0.027 Uiso 1 1 calc R . . C68 C 0.2171(3) 0.1305(3) 1.00763(16) 0.0247(7) Uani 1 1 d . . . H68 H 0.1458 0.1073 1.0134 0.030 Uiso 1 1 calc R . . C4 C 0.7569(3) 0.4291(2) 0.46069(15) 0.0234(7) Uani 1 1 d . . . H4 H 0.7832 0.4871 0.4324 0.028 Uiso 1 1 calc R . . C77 C 0.6833(3) 0.0811(2) 0.87844(15) 0.0227(7) Uani 1 1 d . . . H77 H 0.6678 0.0353 0.8554 0.027 Uiso 1 1 calc R . . C27 C 1.0820(3) -0.0295(3) 0.91595(16) 0.0227(7) Uani 1 1 d . . . H27 H 1.0892 -0.0358 0.9596 0.027 Uiso 1 1 calc R . . C59 C 0.9700(3) -0.6177(2) 0.98002(17) 0.0258(7) Uani 1 1 d . . . H59 H 1.0124 -0.6757 1.0037 0.031 Uiso 1 1 calc R . . C31 C 1.0415(3) -0.1993(2) 0.80620(16) 0.0212(7) Uani 1 1 d . . . H31A H 1.0624 -0.1843 0.7610 0.025 Uiso 1 1 calc R . . H31B H 1.0920 -0.2565 0.8292 0.025 Uiso 1 1 calc R . . C5 C 0.6630(3) 0.3888(3) 0.44587(16) 0.0254(7) Uani 1 1 d . . . H5 H 0.6254 0.4202 0.4078 0.031 Uiso 1 1 calc R . . C53 C 1.2436(3) -0.4254(3) 0.71912(18) 0.0309(8) Uani 1 1 d . . . H53 H 1.2727 -0.3888 0.6801 0.037 Uiso 1 1 calc R . . C34 C 0.7608(3) 0.0459(2) 0.54895(15) 0.0242(7) Uani 1 1 d . . . H34A H 0.7918 0.1044 0.5195 0.029 Uiso 1 1 calc R . . H34B H 0.6974 0.0293 0.5283 0.029 Uiso 1 1 calc R . . C36 C 0.9558(3) -0.0336(3) 0.58193(16) 0.0277(8) Uani 1 1 d . . . C52 C 1.1425(3) -0.3914(3) 0.74043(16) 0.0250(7) Uani 1 1 d . . . H52 H 1.1041 -0.3318 0.7159 0.030 Uiso 1 1 calc R . . C74 C 0.7334(3) 0.2222(3) 0.94417(17) 0.0292(8) Uani 1 1 d . . . H74 H 0.7508 0.2703 0.9651 0.035 Uiso 1 1 calc R . . C76 C 0.7890(3) 0.1095(3) 0.87709(16) 0.0253(7) Uani 1 1 d . . . H76 H 0.8451 0.0820 0.8539 0.030 Uiso 1 1 calc R . . C61 C 0.8049(3) -0.5005(3) 0.96825(17) 0.0276(7) Uani 1 1 d . . . H61 H 0.7355 -0.4815 0.9846 0.033 Uiso 1 1 calc R . . C24 C 1.0760(3) 0.2574(2) 0.77870(16) 0.0214(7) Uani 1 1 d . . . H24A H 1.1501 0.2637 0.7931 0.026 Uiso 1 1 calc R . . H24B H 1.0228 0.2573 0.8138 0.026 Uiso 1 1 calc R . . C13 C 0.7372(3) 0.3385(3) 0.75614(16) 0.0233(7) Uani 1 1 d . . . H13A H 0.7500 0.2650 0.7616 0.028 Uiso 1 1 calc R . . H13B H 0.6960 0.3499 0.7935 0.028 Uiso 1 1 calc R . . C6 C 0.6245(3) 0.3013(2) 0.48753(15) 0.0224(7) Uani 1 1 d . . . H6 H 0.5627 0.2733 0.4766 0.027 Uiso 1 1 calc R . . C41 C 1.0423(3) -0.1178(3) 0.59150(16) 0.0310(8) Uani 1 1 d . . . C75 C 0.8150(3) 0.1810(3) 0.91087(16) 0.0265(7) Uani 1 1 d . . . H75 H 0.8879 0.1995 0.9100 0.032 Uiso 1 1 calc R . . C38 C 1.0901(3) 0.0694(3) 0.61174(18) 0.0353(9) Uani 1 1 d . . . H38 H 1.1066 0.1315 0.6182 0.042 Uiso 1 1 calc R . . C23 C 1.0436(3) 0.3459(2) 0.72133(16) 0.0215(7) Uani 1 1 d . . . H23A H 1.0578 0.4095 0.7308 0.026 Uiso 1 1 calc R . . H23B H 1.0911 0.3390 0.6850 0.026 Uiso 1 1 calc R . . C47 C 0.7207(3) -0.1560(3) 0.52804(19) 0.0346(9) Uani 1 1 d . . . H47 H 0.6615 -0.1049 0.5234 0.042 Uiso 1 1 calc R . . C60 C 0.8711(3) -0.5880(3) 1.00402(17) 0.0284(8) Uani 1 1 d . . . H60 H 0.8461 -0.6247 1.0441 0.034 Uiso 1 1 calc R . . C72 C 0.5386(3) 0.2332(3) 0.98322(16) 0.0260(7) Uani 1 1 d . . . H72 H 0.5553 0.2831 1.0028 0.031 Uiso 1 1 calc R . . C54 C 1.3055(3) -0.5149(3) 0.75501(19) 0.0316(8) Uani 1 1 d . . . H54 H 1.3746 -0.5365 0.7396 0.038 Uiso 1 1 calc R . . C37 C 0.9850(3) 0.0596(3) 0.59309(16) 0.0304(8) Uani 1 1 d . . . H37 H 0.9310 0.1152 0.5875 0.036 Uiso 1 1 calc R . . C28 C 1.0665(3) -0.1148(2) 0.89567(15) 0.0213(7) Uani 1 1 d . . . H28 H 1.0627 -0.1782 0.9255 0.026 Uiso 1 1 calc R . . C0 C 1.1504(3) -0.1048(3) 0.61177(18) 0.0378(9) Uani 1 1 d . . . H0 H 1.2058 -0.1594 0.6186 0.045 Uiso 1 1 calc R . . C44 C 0.8918(4) -0.3132(3) 0.54283(19) 0.0394(10) Uani 1 1 d . . . H44 H 0.9487 -0.3664 0.5477 0.047 Uiso 1 1 calc R . . C39 C 1.1742(3) -0.0141(4) 0.62142(18) 0.0418(10) Uani 1 1 d . . . H39 H 1.2455 -0.0068 0.6343 0.050 Uiso 1 1 calc R . . C45 C 0.7915(4) -0.3263(3) 0.5220(2) 0.0423(10) Uani 1 1 d . . . H45 H 0.7797 -0.3875 0.5128 0.051 Uiso 1 1 calc R . . C46 C 0.7036(4) -0.2457(3) 0.5143(2) 0.0431(10) Uani 1 1 d . . . H46 H 0.6340 -0.2543 0.4997 0.052 Uiso 1 1 calc R . . C79 C 0.6304(4) -0.3646(4) 0.6856(2) 0.0464(10) Uani 1 1 d . . . H79A H 0.6369 -0.4203 0.6651 0.056 Uiso 1 1 calc R . . H79B H 0.6956 -0.3261 0.6733 0.056 Uiso 1 1 calc R . . C80 C 0.3753(4) -0.3660(4) 0.8543(2) 0.0582(13) Uani 1 1 d . . . H80A H 0.4174 -0.3492 0.8141 0.070 Uiso 1 1 calc R . . H80B H 0.3133 -0.4035 0.8484 0.070 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 Cl2 0.0438(6) 0.0386(6) 0.0506(6) -0.0147(5) 0.0002(5) -0.0038(4) Cl3 0.0346(5) 0.0423(6) 0.0467(6) -0.0096(4) 0.0026(4) -0.0098(4) Cl4 0.0598(7) 0.0485(6) 0.0450(6) -0.0133(5) 0.0025(5) 0.0054(5) Cl1 0.0524(7) 0.0702(8) 0.0466(7) -0.0195(6) -0.0080(5) -0.0058(6) O3 0.0286(12) 0.0145(11) 0.0220(12) -0.0032(9) -0.0011(9) -0.0033(9) O2 0.0192(11) 0.0210(11) 0.0234(12) -0.0016(9) -0.0013(9) -0.0020(9) O1 0.0260(12) 0.0250(12) 0.0201(12) -0.0007(9) 0.0012(9) -0.0041(10) N5 0.0188(13) 0.0160(13) 0.0190(13) -0.0035(10) 0.0041(10) 0.0003(10) N4 0.0180(13) 0.0144(12) 0.0224(14) -0.0051(10) -0.0016(10) -0.0009(10) N2 0.0220(13) 0.0180(13) 0.0171(13) -0.0033(10) 0.0043(10) 0.0035(11) C42 0.043(2) 0.0276(19) 0.0223(18) 0.0000(14) 0.0098(16) 0.0142(16) N3 0.0160(12) 0.0175(13) 0.0183(13) -0.0059(10) -0.0004(10) 0.0027(10) N1 0.0196(13) 0.0173(13) 0.0214(14) -0.0027(11) -0.0010(11) -0.0023(10) C26 0.0197(15) 0.0201(16) 0.0229(17) -0.0071(13) -0.0004(13) -0.0012(12) C63 0.0184(15) 0.0165(15) 0.0197(15) -0.0051(12) -0.0016(12) -0.0042(12) C65 0.0202(15) 0.0184(15) 0.0172(15) -0.0015(12) 0.0018(12) -0.0003(12) C19 0.0191(15) 0.0145(14) 0.0171(15) -0.0019(12) 0.0003(12) 0.0044(12) C18 0.0177(15) 0.0149(14) 0.0220(16) -0.0049(12) -0.0002(12) 0.0038(12) C78 0.0209(15) 0.0189(15) 0.0177(15) -0.0020(12) -0.0024(12) 0.0001(12) C20 0.0159(15) 0.0196(15) 0.0232(16) -0.0072(13) 0.0017(12) 0.0000(12) C3 0.0229(16) 0.0182(15) 0.0229(17) -0.0048(13) 0.0023(13) 0.0024(13) C22 0.0185(15) 0.0185(15) 0.0243(17) -0.0071(13) 0.0035(12) -0.0033(12) C50 0.0215(15) 0.0148(15) 0.0209(16) -0.0070(12) -0.0034(12) -0.0021(12) C15 0.0232(16) 0.0171(15) 0.0220(16) -0.0009(12) 0.0018(13) 0.0039(12) C51 0.0215(15) 0.0148(15) 0.0214(16) -0.0069(12) -0.0022(12) -0.0009(12) C21 0.0200(15) 0.0195(16) 0.0226(16) -0.0071(13) 0.0003(12) -0.0012(12) C67 0.0215(16) 0.0224(16) 0.0221(16) -0.0060(13) 0.0011(13) -0.0008(13) C25 0.0141(14) 0.0183(15) 0.0251(17) -0.0038(13) 0.0018(12) -0.0010(12) C29 0.0152(14) 0.0184(15) 0.0274(17) -0.0060(13) 0.0016(12) -0.0004(12) C43 0.046(2) 0.0227(18) 0.0224(18) 0.0002(14) 0.0155(16) 0.0058(16) C14 0.0185(15) 0.0177(15) 0.0218(16) -0.0053(12) 0.0020(12) 0.0017(12) C71 0.0238(16) 0.0225(16) 0.0165(15) -0.0032(12) -0.0014(12) 0.0045(13) C58 0.0259(17) 0.0150(15) 0.0247(17) -0.0054(13) -0.0013(13) -0.0032(12) C56 0.0218(16) 0.0185(16) 0.0295(18) -0.0110(13) -0.0005(13) -0.0017(13) C49 0.0211(15) 0.0174(15) 0.0185(15) -0.0051(12) 0.0002(12) -0.0023(12) C16 0.0264(17) 0.0230(16) 0.0180(16) -0.0035(13) -0.0044(13) 0.0046(13) C7 0.0240(16) 0.0141(15) 0.0211(16) -0.0046(12) 0.0045(13) 0.0025(12) C10 0.0224(16) 0.0163(15) 0.0195(16) -0.0016(12) 0.0028(12) 0.0003(12) C57 0.0268(17) 0.0141(15) 0.0320(19) -0.0042(13) -0.0061(14) 0.0005(13) C17 0.0205(15) 0.0156(15) 0.0254(17) -0.0047(13) -0.0009(13) 0.0024(12) C70 0.0304(18) 0.0270(18) 0.0195(16) -0.0099(14) -0.0020(13) 0.0021(14) C9 0.0212(16) 0.0188(16) 0.0242(17) -0.0049(13) 0.0022(13) 0.0029(13) C66 0.0217(15) 0.0178(15) 0.0153(15) -0.0011(12) -0.0017(12) 0.0011(12) C35 0.0299(18) 0.0233(17) 0.0188(16) -0.0029(13) 0.0089(13) 0.0035(14) C32 0.0207(16) 0.0144(15) 0.0201(16) -0.0016(12) 0.0030(12) -0.0015(12) C33 0.0197(15) 0.0162(15) 0.0170(15) -0.0039(12) 0.0025(12) -0.0008(12) C30 0.0185(15) 0.0229(16) 0.0209(16) -0.0060(13) 0.0005(12) 0.0002(12) C69 0.0234(17) 0.0361(19) 0.0173(16) -0.0076(14) 0.0013(13) 0.0072(14) C8 0.0233(16) 0.0180(15) 0.0194(16) -0.0037(12) 0.0015(13) 0.0020(12) C11 0.0186(15) 0.0148(15) 0.0212(16) -0.0034(12) 0.0021(12) 0.0018(12) C55 0.0215(17) 0.0228(17) 0.041(2) -0.0149(15) -0.0032(15) 0.0052(13) C1 0.0219(16) 0.0236(17) 0.0225(17) -0.0005(13) -0.0001(13) -0.0014(13) C2 0.0230(16) 0.0241(17) 0.0231(17) -0.0008(13) -0.0009(13) 0.0001(13) C64 0.0220(15) 0.0150(15) 0.0187(16) -0.0016(12) 0.0025(12) -0.0009(12) C48 0.038(2) 0.0212(17) 0.0231(18) -0.0042(13) 0.0129(15) 0.0032(15) C73 0.0245(17) 0.0270(17) 0.0204(16) -0.0028(13) -0.0029(13) -0.0043(14) C62 0.0215(16) 0.0188(16) 0.0269(17) -0.0052(13) -0.0011(13) -0.0018(13) C12 0.0222(16) 0.0249(17) 0.0199(16) -0.0024(13) -0.0032(13) -0.0025(13) C68 0.0195(16) 0.0282(18) 0.0238(17) -0.0039(14) 0.0007(13) 0.0006(13) C4 0.0300(18) 0.0166(15) 0.0203(16) -0.0002(12) 0.0054(13) -0.0008(13) C77 0.0228(16) 0.0226(16) 0.0195(16) -0.0015(13) 0.0007(13) 0.0014(13) C27 0.0190(15) 0.0265(17) 0.0215(17) -0.0044(13) 0.0004(13) -0.0018(13) C59 0.0305(18) 0.0149(15) 0.0283(18) 0.0019(13) -0.0067(14) -0.0036(13) C31 0.0180(15) 0.0177(15) 0.0270(17) -0.0051(13) 0.0003(13) -0.0001(12) C5 0.0293(18) 0.0255(17) 0.0193(16) -0.0049(13) -0.0012(13) 0.0056(14) C53 0.0315(19) 0.0301(19) 0.033(2) -0.0131(15) 0.0088(15) 0.0002(15) C34 0.0304(18) 0.0202(16) 0.0196(16) -0.0045(13) 0.0072(13) 0.0046(14) C36 0.0303(18) 0.0282(18) 0.0186(16) 0.0001(13) 0.0104(14) 0.0048(14) C52 0.0275(17) 0.0231(17) 0.0241(17) -0.0072(14) 0.0054(14) -0.0002(14) C74 0.0307(19) 0.0327(19) 0.0249(18) -0.0069(15) 0.0003(14) -0.0086(15) C76 0.0197(16) 0.0290(18) 0.0229(17) -0.0013(14) -0.0004(13) 0.0025(13) C61 0.0233(17) 0.0289(18) 0.0307(19) -0.0079(15) 0.0056(14) -0.0059(14) C24 0.0218(16) 0.0158(15) 0.0277(17) -0.0071(13) -0.0032(13) -0.0018(12) C13 0.0219(16) 0.0250(17) 0.0206(16) -0.0027(13) 0.0002(13) -0.0001(13) C6 0.0214(16) 0.0224(16) 0.0225(17) -0.0055(13) -0.0003(13) 0.0019(13) C41 0.0331(19) 0.033(2) 0.0180(17) 0.0028(14) 0.0080(14) 0.0086(15) C75 0.0199(16) 0.0318(19) 0.0239(17) 0.0001(14) -0.0020(13) -0.0048(14) C38 0.032(2) 0.042(2) 0.030(2) -0.0084(17) 0.0052(16) -0.0023(17) C23 0.0197(16) 0.0158(15) 0.0286(18) -0.0044(13) 0.0010(13) -0.0037(12) C47 0.034(2) 0.0270(19) 0.042(2) -0.0105(16) 0.0134(17) 0.0010(16) C60 0.0344(19) 0.0245(17) 0.0259(18) -0.0032(14) 0.0008(15) -0.0114(15) C72 0.0279(18) 0.0264(17) 0.0270(18) -0.0122(14) -0.0034(14) -0.0030(14) C54 0.0243(17) 0.036(2) 0.040(2) -0.0201(17) 0.0072(15) 0.0002(15) C37 0.0280(18) 0.036(2) 0.0230(18) -0.0023(15) 0.0083(14) -0.0001(15) C28 0.0207(15) 0.0175(15) 0.0232(17) -0.0010(13) 0.0019(13) -0.0031(12) C0 0.035(2) 0.047(2) 0.0241(19) -0.0046(17) 0.0074(15) 0.0139(18) C44 0.059(3) 0.0172(17) 0.034(2) -0.0007(15) 0.0199(19) 0.0078(17) C39 0.029(2) 0.067(3) 0.0231(19) -0.0047(18) 0.0037(15) 0.0050(19) C45 0.063(3) 0.0218(19) 0.044(2) -0.0135(17) 0.021(2) -0.0070(18) C46 0.048(2) 0.031(2) 0.053(3) -0.0164(19) 0.021(2) -0.0076(18) C79 0.049(3) 0.047(3) 0.047(3) -0.019(2) 0.011(2) -0.004(2) C80 0.052(3) 0.077(4) 0.056(3) -0.040(3) -0.007(2) 0.010(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 Cl2 C79 1.765(5) . ? Cl3 C80 1.739(5) . ? Cl4 C80 1.770(5) . ? Cl1 C79 1.775(5) . ? O3 C25 1.372(4) . ? O3 C24 1.424(4) . ? O2 C14 1.370(4) . ? O2 C13 1.442(4) . ? O1 C3 1.372(4) . ? O1 C2 1.434(4) . ? N5 C33 1.460(4) . ? N5 C11 1.456(4) . ? N5 C22 1.463(4) . ? N4 C32 1.463(4) . ? N4 C31 1.476(4) . ? N4 C49 1.483(4) . ? N2 C10 1.462(4) . ? N2 C9 1.457(4) . ? N2 C34 1.476(4) . ? C42 C43 1.383(6) . ? C42 C41 1.387(5) . ? N3 C21 1.468(4) . ? N3 C20 1.464(4) . ? N3 C64 1.477(4) . ? N1 C1 1.458(4) . ? N1 C23 1.467(4) . ? N1 C12 1.469(4) . ? C26 C25 1.389(4) . ? C26 C27 1.390(5) . ? C63 C50 1.412(4) . ? C63 C58 1.429(4) . ? C63 C62 1.437(4) . ? C65 C66 1.419(4) . ? C65 C78 1.409(4) . ? C65 C64 1.518(4) . ? C19 C14 1.390(4) . ? C19 C18 1.399(4) . ? C18 C17 1.386(4) . ? C18 C20 1.517(4) . ? C78 C77 1.436(4) . ? C78 C73 1.440(4) . ? C3 C8 1.390(5) . ? C3 C4 1.398(5) . ? C22 C21 1.522(4) . ? C50 C51 1.423(4) . ? C50 C49 1.501(4) . ? C15 C16 1.374(5) . ? C15 C14 1.399(4) . ? C51 C56 1.429(4) . ? C51 C52 1.434(5) . ? C67 C68 1.357(5) . ? C67 C66 1.425(4) . ? C25 C30 1.390(4) . ? C29 C30 1.381(5) . ? C29 C28 1.397(5) . ? C29 C31 1.513(4) . ? C43 C44 1.426(5) . ? C43 C48 1.450(5) . ? C71 C72 1.385(5) . ? C71 C70 1.440(4) . ? C71 C66 1.437(4) . ? C58 C57 1.395(5) . ? C58 C59 1.434(5) . ? C56 C57 1.386(5) . ? C56 C55 1.438(5) . ? C16 C17 1.409(5) . ? C7 C6 1.380(5) . ? C7 C8 1.404(5) . ? C7 C9 1.515(4) . ? C10 C11 1.537(4) . ? C70 C69 1.360(5) . ? C35 C36 1.407(5) . ? C35 C48 1.419(5) . ? C35 C34 1.508(4) . ? C32 C33 1.517(4) . ? C69 C68 1.417(5) . ? C55 C54 1.353(5) . ? C1 C2 1.532(5) . ? C48 C47 1.418(6) . ? C73 C72 1.386(5) . ? C73 C74 1.425(5) . ? C62 C61 1.360(5) . ? C12 C13 1.517(4) . ? C4 C5 1.382(5) . ? C77 C76 1.355(5) . ? C27 C28 1.374(4) . ? C59 C60 1.342(5) . ? C5 C6 1.389(5) . ? C53 C52 1.360(5) . ? C53 C54 1.411(5) . ? C36 C37 1.428(5) . ? C36 C41 1.443(5) . ? C74 C75 1.355(5) . ? C76 C75 1.425(5) . ? C61 C60 1.417(5) . ? C24 C23 1.510(4) . ? C41 C0 1.424(6) . ? C38 C37 1.365(5) . ? C38 C39 1.417(6) . ? C47 C46 1.364(5) . ? C0 C39 1.361(6) . ? C44 C45 1.343(6) . ? C45 C46 1.423(6) . ? 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 C25 O3 C24 117.5(2) . . ? C14 O2 C13 116.5(2) . . ? C3 O1 C2 117.9(2) . . ? C33 N5 C11 113.9(2) . . ? C33 N5 C22 109.4(2) . . ? C11 N5 C22 114.9(2) . . ? C32 N4 C31 109.2(2) . . ? C32 N4 C49 111.0(2) . . ? C31 N4 C49 109.0(2) . . ? C10 N2 C9 109.7(2) . . ? C10 N2 C34 113.2(2) . . ? C9 N2 C34 109.6(2) . . ? C43 C42 C41 122.4(3) . . ? C21 N3 C20 108.6(2) . . ? C21 N3 C64 112.9(2) . . ? C20 N3 C64 113.2(2) . . ? C1 N1 C23 110.0(2) . . ? C1 N1 C12 109.4(2) . . ? C23 N1 C12 112.0(2) . . ? C25 C26 C27 119.0(3) . . ? C50 C63 C58 120.3(3) . . ? C50 C63 C62 122.3(3) . . ? C58 C63 C62 117.4(3) . . ? C66 C65 C78 119.7(3) . . ? C66 C65 C64 121.6(3) . . ? C78 C65 C64 118.7(3) . . ? C14 C19 C18 120.3(3) . . ? C17 C18 C19 120.0(3) . . ? C17 C18 C20 122.1(3) . . ? C19 C18 C20 117.9(3) . . ? C65 C78 C77 122.9(3) . . ? C65 C78 C73 119.9(3) . . ? C77 C78 C73 117.1(3) . . ? N3 C20 C18 110.5(2) . . ? O1 C3 C8 125.1(3) . . ? O1 C3 C4 114.7(3) . . ? C8 C3 C4 120.2(3) . . ? N5 C22 C21 115.0(2) . . ? C63 C50 C51 119.0(3) . . ? C63 C50 C49 119.4(3) . . ? C51 C50 C49 121.6(3) . . ? C16 C15 C14 119.5(3) . . ? C50 C51 C56 120.0(3) . . ? C50 C51 C52 122.8(3) . . ? C56 C51 C52 117.2(3) . . ? N3 C21 C22 115.0(3) . . ? C68 C67 C66 121.8(3) . . ? O3 C25 C26 124.7(3) . . ? O3 C25 C30 115.2(3) . . ? C26 C25 C30 120.2(3) . . ? C30 C29 C28 119.4(3) . . ? C30 C29 C31 119.3(3) . . ? C28 C29 C31 121.4(3) . . ? C42 C43 C44 121.8(3) . . ? C42 C43 C48 119.8(3) . . ? C44 C43 C48 118.3(4) . . ? O2 C14 C19 123.9(3) . . ? O2 C14 C15 116.1(3) . . ? C19 C14 C15 119.9(3) . . ? C72 C71 C70 121.1(3) . . ? C72 C71 C66 119.8(3) . . ? C70 C71 C66 119.1(3) . . ? C57 C58 C63 119.6(3) . . ? C57 C58 C59 121.3(3) . . ? C63 C58 C59 119.1(3) . . ? C57 C56 C51 119.8(3) . . ? C57 C56 C55 120.6(3) . . ? C51 C56 C55 119.7(3) . . ? N4 C49 C50 112.7(2) . . ? C15 C16 C17 121.2(3) . . ? C6 C7 C8 120.0(3) . . ? C6 C7 C9 120.3(3) . . ? C8 C7 C9 119.7(3) . . ? N2 C10 C11 110.4(2) . . ? C56 C57 C58 121.4(3) . . ? C18 C17 C16 119.0(3) . . ? C69 C70 C71 121.2(3) . . ? N2 C9 C7 113.0(3) . . ? C65 C66 C67 123.4(3) . . ? C65 C66 C71 119.4(3) . . ? C67 C66 C71 117.2(3) . . ? C36 C35 C48 120.1(3) . . ? C36 C35 C34 119.6(3) . . ? C48 C35 C34 120.3(3) . . ? N4 C32 C33 114.6(2) . . ? N5 C33 C32 111.8(2) . . ? C29 C30 C25 120.5(3) . . ? C70 C69 C68 119.4(3) . . ? C3 C8 C7 119.4(3) . . ? N5 C11 C10 116.7(2) . . ? C54 C55 C56 120.6(3) . . ? N1 C1 C2 112.9(3) . . ? O1 C2 C1 110.0(3) . . ? N3 C64 C65 110.9(2) . . ? C35 C48 C47 124.2(3) . . ? C35 C48 C43 118.7(3) . . ? C47 C48 C43 117.1(3) . . ? C72 C73 C74 121.5(3) . . ? C72 C73 C78 119.3(3) . . ? C74 C73 C78 119.2(3) . . ? C61 C62 C63 121.0(3) . . ? N1 C12 C13 112.8(3) . . ? C67 C68 C69 121.3(3) . . ? C5 C4 C3 119.7(3) . . ? C76 C77 C78 121.7(3) . . ? C28 C27 C26 120.9(3) . . ? C60 C59 C58 121.5(3) . . ? N4 C31 C29 113.4(2) . . ? C6 C5 C4 120.3(3) . . ? C52 C53 C54 121.4(3) . . ? N2 C34 C35 113.8(3) . . ? C35 C36 C37 122.6(3) . . ? C35 C36 C41 120.4(3) . . ? C37 C36 C41 117.0(3) . . ? C53 C52 C51 121.1(3) . . ? C75 C74 C73 121.3(3) . . ? C77 C76 C75 120.5(3) . . ? C62 C61 C60 121.0(3) . . ? O3 C24 C23 107.8(2) . . ? O2 C13 C12 109.9(3) . . ? C7 C6 C5 120.3(3) . . ? C42 C41 C36 118.6(3) . . ? C42 C41 C0 122.0(3) . . ? C36 C41 C0 119.3(3) . . ? C74 C75 C76 120.0(3) . . ? C37 C38 C39 120.7(4) . . ? N1 C23 C24 113.7(3) . . ? C46 C47 C48 122.2(4) . . ? C59 C60 C61 119.9(3) . . ? C73 C72 C71 121.8(3) . . ? C55 C54 C53 120.0(3) . . ? C38 C37 C36 121.8(3) . . ? C27 C28 C29 120.0(3) . . ? C39 C0 C41 121.4(4) . . ? C45 C44 C43 122.5(4) . . ? C0 C39 C38 119.7(4) . . ? C44 C45 C46 119.5(4) . . ? C47 C46 C45 120.4(4) . . ? Cl2 C79 Cl1 110.6(2) . . ? Cl3 C80 Cl4 112.8(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.008 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.131