# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Gromov, Sergey' _publ_contact_author_email spgromov@mail.ru _publ_section_title ; Controlled self-assembly of bis(crown)stilbenes into unusual bis sandwich complexes: structure and stereoselective [2+2] photocycloaddition ; loop_ _publ_author_name S.Gromov A.Vedernikov N.Lobova L.Kuzmina S.Basok Yu.Strelenko ; M.Alfimov ; J.Howard #===END data_1b+Ca _database_code_depnum_ccdc_archive 'CCDC 780035' #TrackingRef 'all-CIFs-revised.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H54 Ca2 Cl4 N2 O30' _chemical_formula_weight 1192.75 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.1196(2) _cell_length_b 16.2585(5) _cell_length_c 19.1065(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.303(1) _cell_angle_gamma 90.00 _cell_volume 2501.84(12) _cell_formula_units_Z 2 _cell_measurement_temperature 120.0(2) _cell_measurement_reflns_used 6394 _cell_measurement_theta_min 2.488 _cell_measurement_theta_max 30.243 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.538 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8056 _exptl_absorpt_correction_T_max 0.8299 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120.0(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' _diffrn_measurement_method /W _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17932 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 29.00 _reflns_number_total 6562 _reflns_number_gt 6044 _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 ; The both independent perchlorate anions are disordered over two positions with occupancies 0.62:0.38 and 0.70:0.30. The ISOR command was applied for atom O(25) of perchlorate anion Cl(2)O4- to avoid N.P.D. for its thermal anisotropic displacement parameters. 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^)+(0.0449P)^2^+1.8231P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6562 _refine_ls_number_parameters 498 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0940 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 Ca1 Ca 0.71424(3) 0.242197(17) 0.122322(14) 0.01695(7) Uani 1 1 d . . . Cl1 Cl 0.25003(5) 0.38838(3) 0.28023(2) 0.02896(10) Uani 1 1 d . . . O11 O 0.2379(4) 0.3881(2) 0.20692(12) 0.0658(10) Uani 0.624(3) 1 d P A 1 O12 O 0.0796(3) 0.36703(16) 0.29781(12) 0.0411(6) Uani 0.624(3) 1 d P A 1 O13 O 0.2982(3) 0.46131(15) 0.31228(14) 0.0512(7) Uani 0.624(3) 1 d P A 1 O14 O 0.3530(3) 0.31918(16) 0.30895(15) 0.0506(7) Uani 0.624(3) 1 d P A 1 O15 O 0.2362(6) 0.4035(3) 0.3506(2) 0.0567(13) Uani 0.376(3) 1 d P A 2 O16 O 0.1648(6) 0.3245(4) 0.2527(4) 0.080(2) Uani 0.376(3) 1 d P A 2 O17 O 0.1902(8) 0.4653(4) 0.2418(4) 0.090(2) Uani 0.376(3) 1 d P A 2 O18 O 0.4300(5) 0.3841(3) 0.2684(2) 0.0481(11) Uani 0.376(3) 1 d P A 2 Cl2 Cl 0.83824(5) 0.57315(2) 0.12793(2) 0.02902(10) Uani 1 1 d . . . O21 O 0.73743(19) 0.51774(9) 0.16250(8) 0.0420(3) Uani 1 1 d . B . O22 O 0.9365(7) 0.5273(4) 0.0802(2) 0.0280(8) Uani 0.70(2) 1 d P B 1 O23 O 0.9596(6) 0.6086(7) 0.1828(4) 0.069(3) Uani 0.70(2) 1 d P B 1 O24 O 0.7393(13) 0.6332(6) 0.0944(6) 0.100(3) Uani 0.70(2) 1 d P B 1 O25 O 0.932(2) 0.5436(10) 0.0901(9) 0.052(3) Uani 0.30(2) 1 d PU B 2 O26 O 0.887(3) 0.6458(9) 0.1614(5) 0.065(5) Uani 0.30(2) 1 d P B 2 O27 O 0.7081(12) 0.6117(9) 0.0718(7) 0.049(3) Uani 0.30(2) 1 d P B 2 O1 O 0.61638(13) 0.20841(6) -0.00519(5) 0.0207(2) Uani 1 1 d . . . O2 O 0.85598(13) 0.31563(7) 0.03240(6) 0.0218(2) Uani 1 1 d . . . O3 O 1.01188(13) 0.21932(7) 0.13697(6) 0.0233(2) Uani 1 1 d . . . O4 O 0.80869(12) 0.12257(6) 0.20158(5) 0.0195(2) Uani 1 1 d . . . O5 O 0.58749(12) 0.10421(6) 0.08779(5) 0.0199(2) Uani 1 1 d . . . C1 C 0.01902(17) 0.02924(9) -0.02217(8) 0.0215(3) Uani 1 1 d . . . C2 C 0.17763(17) 0.07360(9) -0.01930(7) 0.0193(3) Uani 1 1 d . . . C3 C 0.19560(18) 0.13250(9) -0.07074(8) 0.0211(3) Uani 1 1 d . . . C4 C 0.34042(18) 0.17955(9) -0.06927(8) 0.0211(3) Uani 1 1 d . . . C5 C 0.46776(17) 0.16694(8) -0.01521(7) 0.0184(3) Uani 1 1 d . . . C6 C 0.45182(16) 0.10769(8) 0.03662(7) 0.0169(2) Uani 1 1 d . . . C7 C 0.30995(17) 0.06051(9) 0.03508(7) 0.0183(3) Uani 1 1 d . . . C8 C 0.65045(19) 0.26793(9) -0.05768(8) 0.0219(3) Uani 1 1 d . . . C9 C 0.83161(19) 0.28865(10) -0.03984(8) 0.0237(3) Uani 1 1 d . . . C10 C 1.02842(18) 0.33082(10) 0.05826(8) 0.0238(3) Uani 1 1 d . . . C11 C 1.11183(19) 0.25281(10) 0.08715(9) 0.0235(3) Uani 1 1 d . . . C12 C 1.08808(19) 0.15142(10) 0.17629(9) 0.0259(3) Uani 1 1 d . . . C13 C 0.97820(19) 0.13230(11) 0.23263(8) 0.0248(3) Uani 1 1 d . . . C14 C 0.77390(18) 0.04130(9) 0.17437(8) 0.0201(3) Uani 1 1 d . . . C15 C 0.59615(18) 0.04019(9) 0.14024(7) 0.0193(3) Uani 1 1 d . . . O1W O 0.52523(15) 0.22756(8) 0.20727(7) 0.0268(2) Uani 1 1 d . . . O2W O 0.81264(18) 0.35302(9) 0.19470(8) 0.0329(3) Uani 1 1 d . . . N1S N 0.50395(16) 0.35302(9) 0.08591(8) 0.0267(3) Uani 1 1 d . . . C1S C 0.43508(19) 0.41419(10) 0.08139(9) 0.0255(3) Uani 1 1 d . . . C2S C 0.3476(2) 0.49246(11) 0.07636(12) 0.0342(4) Uani 1 1 d . . . H1A H -0.062(3) 0.0473(14) -0.0608(12) 0.036(6) Uiso 1 1 d . . . H3A H 0.107(2) 0.1429(12) -0.1098(10) 0.025(5) Uiso 1 1 d . . . H4A H 0.351(2) 0.2205(13) -0.1043(11) 0.024(5) Uiso 1 1 d . . . H7A H 0.300(2) 0.0187(12) 0.0704(10) 0.021(4) Uiso 1 1 d . . . H8A H 0.575(2) 0.3146(11) -0.0559(9) 0.013(4) Uiso 1 1 d . . . H8B H 0.628(2) 0.2444(12) -0.1047(11) 0.022(5) Uiso 1 1 d . . . H9A H 0.898(3) 0.2431(13) -0.0452(11) 0.028(5) Uiso 1 1 d . . . H9B H 0.862(2) 0.3305(12) -0.0704(10) 0.024(5) Uiso 1 1 d . . . H10A H 1.027(2) 0.3722(12) 0.0971(10) 0.020(4) Uiso 1 1 d . . . H10B H 1.082(3) 0.3537(14) 0.0199(12) 0.035(5) Uiso 1 1 d . . . H11A H 1.119(2) 0.2161(13) 0.0518(11) 0.024(5) Uiso 1 1 d . . . H11B H 1.222(3) 0.2650(13) 0.1106(11) 0.031(5) Uiso 1 1 d . . . H12A H 1.200(3) 0.1682(14) 0.2005(12) 0.035(6) Uiso 1 1 d . . . H12B H 1.098(3) 0.1061(13) 0.1461(11) 0.026(5) Uiso 1 1 d . . . H13A H 1.015(2) 0.0832(13) 0.2589(11) 0.025(5) Uiso 1 1 d . . . H13B H 0.977(2) 0.1761(13) 0.2646(11) 0.024(5) Uiso 1 1 d . . . H14A H 0.791(2) 0.0027(12) 0.2143(10) 0.023(5) Uiso 1 1 d . . . H14B H 0.848(2) 0.0284(12) 0.1430(11) 0.024(5) Uiso 1 1 d . . . H15A H 0.569(2) -0.0112(12) 0.1183(10) 0.019(4) Uiso 1 1 d . . . H15B H 0.518(2) 0.0532(12) 0.1743(10) 0.021(4) Uiso 1 1 d . . . H1WA H 0.550(3) 0.1993(18) 0.2385(15) 0.048(7) Uiso 1 1 d . . . H1WB H 0.485(4) 0.2640(19) 0.2249(16) 0.058(8) Uiso 1 1 d . . . H2WA H 0.888(4) 0.3537(19) 0.2186(17) 0.060(9) Uiso 1 1 d . . . H2WB H 0.791(4) 0.400(2) 0.1849(16) 0.062(9) Uiso 1 1 d . . . H2SA H 0.276(3) 0.4962(18) 0.1129(15) 0.057(8) Uiso 1 1 d . . . H2SB H 0.422(4) 0.5330(19) 0.0863(15) 0.062(8) Uiso 1 1 d . . . H2SC H 0.287(4) 0.4987(18) 0.0351(16) 0.062(8) Uiso 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 Ca1 0.01393(12) 0.01741(13) 0.01943(13) -0.00178(9) 0.00178(9) -0.00157(9) Cl1 0.02569(18) 0.0366(2) 0.02316(18) -0.00833(14) -0.00238(13) 0.00545(15) O11 0.079(2) 0.099(2) 0.0192(10) -0.0098(12) 0.0050(11) -0.0337(18) O12 0.0285(10) 0.0555(14) 0.0396(12) 0.0062(10) 0.0050(8) -0.0009(10) O13 0.0583(16) 0.0377(13) 0.0543(15) -0.0172(11) -0.0059(12) -0.0071(11) O14 0.0365(12) 0.0457(14) 0.0681(17) 0.0025(12) 0.0000(11) 0.0183(10) O15 0.072(3) 0.069(3) 0.032(2) -0.016(2) 0.0148(19) 0.004(2) O16 0.038(2) 0.079(4) 0.120(5) -0.067(4) -0.003(3) -0.012(2) O17 0.092(4) 0.091(4) 0.094(5) 0.052(4) 0.036(4) 0.051(4) O18 0.0256(17) 0.057(3) 0.063(3) -0.016(2) 0.0073(16) 0.0021(16) Cl2 0.0374(2) 0.02256(17) 0.02973(19) -0.00243(14) 0.01456(16) -0.00360(15) O21 0.0488(8) 0.0332(7) 0.0483(8) -0.0014(6) 0.0229(7) -0.0114(6) O22 0.0352(13) 0.027(2) 0.0246(13) -0.0092(13) 0.0128(10) 0.0105(12) O23 0.045(2) 0.107(5) 0.059(3) -0.053(3) 0.0221(17) -0.038(2) O24 0.117(5) 0.081(5) 0.112(6) 0.057(4) 0.059(5) 0.072(4) O25 0.062(5) 0.030(5) 0.074(7) -0.025(4) 0.043(5) 0.005(3) O26 0.106(12) 0.059(6) 0.032(3) -0.017(3) 0.019(5) -0.054(7) O27 0.029(3) 0.055(5) 0.063(5) 0.030(4) 0.010(3) 0.012(3) O1 0.0192(5) 0.0208(5) 0.0210(5) 0.0031(4) -0.0014(4) -0.0067(4) O2 0.0181(5) 0.0247(5) 0.0227(5) -0.0008(4) 0.0034(4) -0.0052(4) O3 0.0163(5) 0.0244(5) 0.0298(5) 0.0042(4) 0.0050(4) 0.0000(4) O4 0.0167(4) 0.0212(5) 0.0199(5) -0.0011(4) -0.0001(4) -0.0010(4) O5 0.0178(5) 0.0204(5) 0.0201(5) 0.0041(4) -0.0028(4) -0.0039(4) C1 0.0152(6) 0.0255(7) 0.0233(7) -0.0051(6) 0.0000(5) -0.0034(5) C2 0.0155(6) 0.0209(6) 0.0212(6) -0.0047(5) 0.0012(5) -0.0022(5) C3 0.0179(6) 0.0240(7) 0.0204(6) -0.0024(5) -0.0012(5) -0.0005(5) C4 0.0209(6) 0.0210(6) 0.0205(6) 0.0010(5) -0.0001(5) -0.0014(5) C5 0.0169(6) 0.0176(6) 0.0202(6) -0.0011(5) 0.0009(5) -0.0030(5) C6 0.0150(6) 0.0177(6) 0.0174(6) -0.0026(5) -0.0004(5) -0.0011(5) C7 0.0162(6) 0.0184(6) 0.0201(6) -0.0015(5) 0.0020(5) -0.0020(5) C8 0.0230(7) 0.0224(7) 0.0201(6) 0.0035(5) 0.0023(5) -0.0041(5) C9 0.0221(7) 0.0276(7) 0.0216(7) 0.0005(6) 0.0042(5) -0.0050(6) C10 0.0186(6) 0.0252(7) 0.0276(7) 0.0003(6) 0.0029(5) -0.0081(5) C11 0.0170(6) 0.0266(7) 0.0279(7) -0.0022(6) 0.0065(5) -0.0035(5) C12 0.0165(6) 0.0278(7) 0.0327(8) 0.0036(6) 0.0006(6) 0.0006(6) C13 0.0201(7) 0.0305(8) 0.0224(7) 0.0006(6) -0.0033(5) -0.0033(6) C14 0.0196(6) 0.0200(6) 0.0199(6) -0.0005(5) -0.0011(5) 0.0016(5) C15 0.0195(6) 0.0179(6) 0.0201(6) 0.0033(5) 0.0006(5) -0.0024(5) O1W 0.0258(6) 0.0285(6) 0.0275(6) 0.0030(5) 0.0093(5) 0.0057(5) O2W 0.0305(7) 0.0299(7) 0.0374(7) -0.0126(5) 0.0016(5) -0.0045(5) N1S 0.0209(6) 0.0265(7) 0.0327(7) 0.0031(5) 0.0037(5) 0.0006(5) C1S 0.0194(6) 0.0256(7) 0.0315(8) 0.0032(6) 0.0034(6) -0.0034(6) C2S 0.0272(8) 0.0238(8) 0.0505(11) 0.0017(7) 0.0005(8) 0.0023(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 Ca1 O2W 2.3488(13) . ? Ca1 O1W 2.3831(12) . ? Ca1 O3 2.4260(11) . ? Ca1 O2 2.4908(11) . ? Ca1 N1S 2.5187(14) . ? Ca1 O5 2.5209(10) . ? Ca1 O4 2.5237(11) . ? Ca1 O1 2.5251(11) . ? Cl1 O16 1.320(4) . ? Cl1 O13 1.369(2) . ? Cl1 O15 1.386(4) . ? Cl1 O11 1.392(2) . ? Cl1 O14 1.466(2) . ? Cl1 O17 1.499(5) . ? Cl1 O12 1.505(2) . ? Cl1 O18 1.508(4) . ? Cl2 O25 1.215(16) . ? Cl2 O24 1.370(7) . ? Cl2 O26 1.378(7) . ? Cl2 O21 1.4336(13) . ? Cl2 O23 1.463(4) . ? Cl2 O22 1.486(6) . ? Cl2 O27 1.540(11) . ? O1 C5 1.3743(16) . ? O1 C8 1.4455(17) . ? O2 C9 1.4379(18) . ? O2 C10 1.4455(17) . ? O3 C12 1.4311(19) . ? O3 C11 1.4344(18) . ? O4 C14 1.4347(17) . ? O4 C13 1.4366(17) . ? O5 C6 1.3780(16) . ? O5 C15 1.4403(17) . ? C1 C1 1.336(3) 3 ? C1 C2 1.4709(19) . ? C2 C3 1.393(2) . ? C2 C7 1.4125(19) . ? C3 C4 1.400(2) . ? C4 C5 1.3807(19) . ? C5 C6 1.3994(19) . ? C6 C7 1.3811(18) . ? C8 C9 1.505(2) . ? C10 C11 1.509(2) . ? C12 C13 1.515(2) . ? C14 C15 1.5064(19) . ? N1S C1S 1.139(2) . ? C1S C2S 1.455(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2W Ca1 O1W 82.87(5) . . ? O2W Ca1 O3 77.90(5) . . ? O1W Ca1 O3 128.64(4) . . ? O2W Ca1 O2 83.45(4) . . ? O1W Ca1 O2 155.73(4) . . ? O3 Ca1 O2 67.18(4) . . ? O2W Ca1 N1S 77.40(5) . . ? O1W Ca1 N1S 77.70(5) . . ? O3 Ca1 N1S 140.53(4) . . ? O2 Ca1 N1S 79.81(4) . . ? O2W Ca1 O5 159.04(5) . . ? O1W Ca1 O5 79.20(4) . . ? O3 Ca1 O5 105.15(4) . . ? O2 Ca1 O5 117.07(4) . . ? N1S Ca1 O5 108.93(4) . . ? O2W Ca1 O4 100.56(5) . . ? O1W Ca1 O4 71.78(4) . . ? O3 Ca1 O4 65.82(3) . . ? O2 Ca1 O4 130.65(4) . . ? N1S Ca1 O4 149.40(4) . . ? O5 Ca1 O4 63.51(3) . . ? O2W Ca1 O1 140.96(5) . . ? O1W Ca1 O1 118.98(4) . . ? O3 Ca1 O1 105.34(4) . . ? O2 Ca1 O1 63.58(3) . . ? N1S Ca1 O1 76.70(4) . . ? O5 Ca1 O1 59.07(3) . . ? O4 Ca1 O1 116.46(3) . . ? O16 Cl1 O13 165.0(2) . . ? O16 Cl1 O15 115.1(4) . . ? O13 Cl1 O15 57.7(2) . . ? O16 Cl1 O11 68.2(3) . . ? O13 Cl1 O11 115.66(19) . . ? O15 Cl1 O11 166.8(3) . . ? O16 Cl1 O14 77.9(3) . . ? O13 Cl1 O14 112.36(16) . . ? O15 Cl1 O14 83.5(2) . . ? O11 Cl1 O14 109.7(2) . . ? O16 Cl1 O17 109.9(4) . . ? O13 Cl1 O17 63.4(3) . . ? O15 Cl1 O17 105.4(3) . . ? O11 Cl1 O17 62.2(3) . . ? O14 Cl1 O17 163.2(3) . . ? O16 Cl1 O12 57.2(3) . . ? O13 Cl1 O12 108.57(16) . . ? O15 Cl1 O12 68.5(2) . . ? O11 Cl1 O12 105.93(16) . . ? O14 Cl1 O12 103.67(15) . . ? O17 Cl1 O12 93.0(3) . . ? O16 Cl1 O18 111.9(3) . . ? O13 Cl1 O18 83.1(2) . . ? O15 Cl1 O18 110.7(3) . . ? O11 Cl1 O18 78.2(2) . . ? O14 Cl1 O18 60.2(2) . . ? O17 Cl1 O18 103.0(3) . . ? O12 Cl1 O18 163.4(2) . . ? O25 Cl2 O24 112.3(8) . . ? O25 Cl2 O26 116.6(9) . . ? O24 Cl2 O26 74.0(6) . . ? O25 Cl2 O21 117.7(8) . . ? O24 Cl2 O21 109.1(4) . . ? O26 Cl2 O21 118.3(4) . . ? O25 Cl2 O23 99.5(8) . . ? O24 Cl2 O23 110.8(4) . . ? O26 Cl2 O23 36.9(7) . . ? O21 Cl2 O23 106.8(4) . . ? O25 Cl2 O22 8.0(10) . . ? O24 Cl2 O22 113.6(5) . . ? O26 Cl2 O22 124.6(8) . . ? O21 Cl2 O22 110.5(2) . . ? O23 Cl2 O22 105.8(2) . . ? O25 Cl2 O27 100.0(9) . . ? O24 Cl2 O27 22.4(7) . . ? O26 Cl2 O27 96.2(9) . . ? O21 Cl2 O27 101.3(4) . . ? O23 Cl2 O27 132.8(5) . . ? O22 Cl2 O27 98.7(6) . . ? C5 O1 C8 118.28(11) . . ? C5 O1 Ca1 113.85(8) . . ? C8 O1 Ca1 117.34(8) . . ? C9 O2 C10 112.91(11) . . ? C9 O2 Ca1 119.78(8) . . ? C10 O2 Ca1 111.01(8) . . ? C12 O3 C11 113.44(11) . . ? C12 O3 Ca1 122.46(9) . . ? C11 O3 Ca1 120.31(9) . . ? C14 O4 C13 112.66(11) . . ? C14 O4 Ca1 117.48(8) . . ? C13 O4 Ca1 111.41(9) . . ? C6 O5 C15 119.16(11) . . ? C6 O5 Ca1 114.34(8) . . ? C15 O5 Ca1 118.61(8) . . ? C1 C1 C2 126.68(17) 3 . ? C3 C2 C7 118.97(13) . . ? C3 C2 C1 118.71(13) . . ? C7 C2 C1 122.28(13) . . ? C2 C3 C4 121.63(13) . . ? C5 C4 C3 118.75(13) . . ? O1 C5 C4 126.32(13) . . ? O1 C5 C6 113.43(12) . . ? C4 C5 C6 120.25(13) . . ? O5 C6 C7 125.57(13) . . ? O5 C6 C5 113.13(11) . . ? C7 C6 C5 121.28(12) . . ? C6 C7 C2 119.10(13) . . ? O1 C8 C9 105.10(12) . . ? O2 C9 C8 107.27(12) . . ? O2 C10 C11 110.58(12) . . ? O3 C11 C10 107.23(12) . . ? O3 C12 C13 106.07(12) . . ? O4 C13 C12 110.42(12) . . ? O4 C14 C15 107.55(11) . . ? O5 C15 C14 104.59(11) . . ? C1S N1S Ca1 162.69(13) . . ? N1S C1S C2S 179.4(2) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.631 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.061 #===END data_1b+K _database_code_depnum_ccdc_archive 'CCDC 780036' #TrackingRef 'all-CIFs-revised.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H48 K N3 O17' _chemical_formula_weight 905.93 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' K K 0.2009 0.2494 '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 12.3927(10) _cell_length_b 13.7956(11) _cell_length_c 14.7748(12) _cell_angle_alpha 104.967(4) _cell_angle_beta 108.561(4) _cell_angle_gamma 105.014(4) _cell_volume 2146.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120.0(2) _cell_measurement_reflns_used 863 _cell_measurement_theta_min 2.572 _cell_measurement_theta_max 25.526 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.203 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120.0(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-1K' _diffrn_measurement_method /W _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15990 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.2052 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 29.00 _reflns_number_total 10796 _reflns_number_gt 4212 _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 ; The solvate benzene molecule is disordered over two positions with occupancies 0.63:0.37. The ISOR command was applied for all carbon atoms of the disordered benzene molecule to avoid N.P.D. for their thermal anisotropic displacement parameters. 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^)+(0.1133P)^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 10796 _refine_ls_number_parameters 599 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.2583 _refine_ls_R_factor_gt 0.1104 _refine_ls_wR_factor_ref 0.2690 _refine_ls_wR_factor_gt 0.2224 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.958 _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 K1 K 0.80213(11) 0.41312(10) 0.17445(8) 0.0321(3) Uani 1 1 d . . . O1 O 0.5507(3) 0.3800(3) 0.1423(3) 0.0383(9) Uani 1 1 d . . . O2 O 0.6186(4) 0.2050(3) 0.1013(3) 0.0537(11) Uani 1 1 d . . . O3 O 0.7321(4) 0.2748(4) -0.0259(3) 0.0549(12) Uani 1 1 d . . . O4 O 0.8302(3) 0.5056(3) 0.0254(3) 0.0455(10) Uani 1 1 d . . . O5 O 0.6497(3) 0.5296(3) 0.0919(3) 0.0391(9) Uani 1 1 d . . . O6 O 0.1500(4) 0.6810(3) 0.6656(3) 0.0442(10) Uani 1 1 d . . . O7 O 0.0712(3) 0.7345(3) 0.8197(3) 0.0387(9) Uani 1 1 d . . . O8 O -0.0506(3) 0.5078(3) 0.7799(3) 0.0360(9) Uani 1 1 d . . . O9 O 0.0618(3) 0.3615(3) 0.7040(3) 0.0368(9) Uani 1 1 d . . . O10 O 0.1561(4) 0.4927(3) 0.6130(3) 0.0429(10) Uani 1 1 d . . . C1 C 0.4941(6) 0.2895(5) 0.1617(4) 0.0429(14) Uani 1 1 d . . . H1A H 0.4090 0.2819 0.1516 0.052 Uiso 1 1 calc R . . H1B H 0.5403 0.2968 0.2330 0.052 Uiso 1 1 calc R . . C2 C 0.4950(6) 0.1932(5) 0.0851(5) 0.0520(17) Uani 1 1 d . . . H2A H 0.4542 0.1261 0.0932 0.062 Uiso 1 1 calc R . . H2B H 0.4492 0.1875 0.0142 0.062 Uiso 1 1 calc R . . C3 C 0.6311(7) 0.1379(5) 0.0170(6) 0.066(2) Uani 1 1 d . . . H3A H 0.5639 0.0661 -0.0130 0.080 Uiso 1 1 calc R . . H3B H 0.7094 0.1272 0.0436 0.080 Uiso 1 1 calc R . . C4 C 0.6288(8) 0.1794(6) -0.0654(5) 0.068(2) Uani 1 1 d . . . H4A H 0.6300 0.1251 -0.1235 0.082 Uiso 1 1 calc R . . H4B H 0.5531 0.1943 -0.0910 0.082 Uiso 1 1 calc R . . C5 C 0.7380(6) 0.3195(6) -0.1005(5) 0.0562(18) Uani 1 1 d . . . H5A H 0.6604 0.3295 -0.1325 0.067 Uiso 1 1 calc R . . H5B H 0.7498 0.2701 -0.1551 0.067 Uiso 1 1 calc R . . C6 C 0.8415(6) 0.4245(6) -0.0506(5) 0.0548(18) Uani 1 1 d . . . H6A H 0.9176 0.4129 -0.0176 0.066 Uiso 1 1 calc R . . H6B H 0.8502 0.4523 -0.1044 0.066 Uiso 1 1 calc R . . C7 C 0.7492(6) 0.5543(5) -0.0183(5) 0.0489(16) Uani 1 1 d . . . H7A H 0.6750 0.4984 -0.0776 0.059 Uiso 1 1 calc R . . H7B H 0.7904 0.6070 -0.0428 0.059 Uiso 1 1 calc R . . C8 C 0.7145(5) 0.6104(5) 0.0628(4) 0.0417(14) Uani 1 1 d . . . H8A H 0.7889 0.6645 0.1233 0.050 Uiso 1 1 calc R . . H8B H 0.6615 0.6481 0.0358 0.050 Uiso 1 1 calc R . . C9 C 0.6098(5) 0.5616(5) 0.1656(4) 0.0359(13) Uani 1 1 d . . . C10 C 0.6196(5) 0.6676(5) 0.2135(5) 0.0408(14) Uani 1 1 d . . . H10A H 0.6579 0.7243 0.1954 0.049 Uiso 1 1 calc R . . C11 C 0.5734(5) 0.6892(5) 0.2870(4) 0.0431(15) Uani 1 1 d . . . H11A H 0.5786 0.7608 0.3177 0.052 Uiso 1 1 calc R . . C12 C 0.5204(5) 0.6100(5) 0.3165(4) 0.0423(15) Uani 1 1 d . . . C13 C 0.5089(5) 0.5007(5) 0.2677(4) 0.0365(13) Uani 1 1 d . . . H13A H 0.4706 0.4443 0.2859 0.044 Uiso 1 1 calc R . . C14 C 0.5544(5) 0.4795(4) 0.1939(4) 0.0315(12) Uani 1 1 d . . . C15 C 0.4715(5) 0.6389(5) 0.3943(4) 0.0447(15) Uani 1 1 d . . . H15A H 0.4754 0.7113 0.4159 0.054 Uiso 1 1 calc R . . C16 C 0.4243(5) 0.5796(5) 0.4370(4) 0.0393(14) Uani 1 1 d . . . H16A H 0.4260 0.5089 0.4225 0.047 Uiso 1 1 calc R . . C17 C 0.3663(5) 0.6158(5) 0.5087(4) 0.0402(14) Uani 1 1 d . . . C18 C 0.3706(5) 0.7191(5) 0.5452(4) 0.0407(14) Uani 1 1 d . . . H18A H 0.4225 0.7739 0.5335 0.049 Uiso 1 1 calc R . . C19 C 0.3013(5) 0.7478(5) 0.5994(4) 0.0423(14) Uani 1 1 d . . . H19A H 0.3048 0.8200 0.6222 0.051 Uiso 1 1 calc R . . C20 C 0.2270(5) 0.6672(4) 0.6190(4) 0.0353(13) Uani 1 1 d . . . C21 C 0.2269(5) 0.5633(5) 0.5867(4) 0.0356(13) Uani 1 1 d . . . C22 C 0.2968(5) 0.5376(5) 0.5327(4) 0.0341(13) Uani 1 1 d . . . H22A H 0.2968 0.4664 0.5124 0.041 Uiso 1 1 calc R . . C23 C 0.1459(6) 0.7862(5) 0.7010(5) 0.0467(15) Uani 1 1 d . . . H23A H 0.1295 0.8141 0.6447 0.056 Uiso 1 1 calc R . . H23B H 0.2248 0.8373 0.7585 0.056 Uiso 1 1 calc R . . C24 C 0.0428(5) 0.7726(5) 0.7365(4) 0.0407(14) Uani 1 1 d . . . H24A H 0.0332 0.8426 0.7597 0.049 Uiso 1 1 calc R . . H24B H -0.0352 0.7200 0.6788 0.049 Uiso 1 1 calc R . . C25 C -0.0330(6) 0.6903(5) 0.8391(4) 0.0438(15) Uani 1 1 d . . . H25A H -0.0807 0.7378 0.8362 0.053 Uiso 1 1 calc R . . H25B H -0.0044 0.6895 0.9095 0.053 Uiso 1 1 calc R . . C26 C -0.1152(5) 0.5783(5) 0.7645(4) 0.0405(14) Uani 1 1 d . . . H26A H -0.1908 0.5551 0.7758 0.049 Uiso 1 1 calc R . . H26B H -0.1387 0.5762 0.6932 0.049 Uiso 1 1 calc R . . C27 C -0.1209(5) 0.4011(5) 0.7030(5) 0.0428(14) Uani 1 1 d . . . H27A H -0.1386 0.4032 0.6335 0.051 Uiso 1 1 calc R . . H27B H -0.1997 0.3707 0.7077 0.051 Uiso 1 1 calc R . . C28 C -0.0449(5) 0.3320(5) 0.7226(4) 0.0398(14) Uani 1 1 d . . . H28A H -0.0205 0.3377 0.7950 0.048 Uiso 1 1 calc R . . H28B H -0.0966 0.2555 0.6781 0.048 Uiso 1 1 calc R . . C29 C 0.0371(5) 0.3211(5) 0.5975(4) 0.0443(15) Uani 1 1 d . . . H29A H -0.0378 0.3300 0.5569 0.053 Uiso 1 1 calc R . . H29B H 0.0228 0.2431 0.5742 0.053 Uiso 1 1 calc R . . C30 C 0.1434(5) 0.3811(4) 0.5801(4) 0.0382(14) Uani 1 1 d . . . H30A H 0.2191 0.3731 0.6205 0.046 Uiso 1 1 calc R . . H30B H 0.1273 0.3529 0.5063 0.046 Uiso 1 1 calc R . . O1P O 0.3821(5) 0.0644(4) 0.2436(4) 0.0762(15) Uani 1 1 d . . . O2P O 0.2609(5) 0.1978(5) 0.2150(5) 0.0783(17) Uani 1 1 d . . . O3P O 0.2696(5) 0.3021(4) 0.3573(4) 0.0737(15) Uani 1 1 d . . . O4P O 0.1382(5) 0.1072(4) 0.5585(4) 0.0861(17) Uani 1 1 d . . . O5P O 0.1841(6) -0.0331(5) 0.5645(5) 0.096(2) Uani 1 1 d . . . O6P O 0.3879(6) -0.1629(4) 0.3617(4) 0.0899(19) Uani 1 1 d . . . O7P O 0.5102(5) -0.0422(5) 0.3340(4) 0.0790(16) Uani 1 1 d . . . N1 N 0.2718(5) 0.2176(4) 0.3033(5) 0.0513(14) Uani 1 1 d . . . N2 N 0.1834(5) 0.0419(5) 0.5333(5) 0.0640(16) Uani 1 1 d . . . N3 N 0.4209(6) -0.0757(5) 0.3536(4) 0.0591(16) Uani 1 1 d . . . C1P C 0.3437(5) 0.0669(5) 0.3155(5) 0.0474(15) Uani 1 1 d . . . C2P C 0.2829(5) 0.1359(4) 0.3488(5) 0.0422(14) Uani 1 1 d . . . C3P C 0.2323(6) 0.1307(5) 0.4172(5) 0.0510(16) Uani 1 1 d . . . H3PA H 0.1922 0.1784 0.4339 0.061 Uiso 1 1 calc R . . C4P C 0.2399(6) 0.0533(5) 0.4633(5) 0.0457(15) Uani 1 1 d . . . C5P C 0.2988(6) -0.0148(4) 0.4383(5) 0.0462(15) Uani 1 1 d . . . H5PA H 0.3018 -0.0688 0.4670 0.055 Uiso 1 1 calc R . . C6P C 0.3538(5) -0.0042(5) 0.3713(4) 0.0424(14) Uani 1 1 d . . . C1S C 0.1469(14) 0.0755(9) 0.9514(6) 0.077(6) Uani 0.626(18) 1 d PGU A -1 H1S H 0.1844 0.0658 1.0137 0.092 Uiso 0.626(18) 1 calc PR A -1 C2S C 0.1938(8) 0.0602(7) 0.8773(8) 0.056(4) Uani 0.626(18) 1 d PGU A -1 H2S H 0.2633 0.0401 0.8888 0.068 Uiso 0.626(18) 1 calc PR A -1 C3S C 0.1390(10) 0.0743(7) 0.7862(6) 0.054(4) Uani 0.626(18) 1 d PGU A -1 H3S H 0.1710 0.0639 0.7355 0.065 Uiso 0.626(18) 1 calc PR A -1 C4S C 0.0373(10) 0.1038(9) 0.7693(8) 0.066(5) Uani 0.626(18) 1 d PGU A -1 H4S H -0.0001 0.1135 0.7071 0.079 Uiso 0.626(18) 1 calc PR A -1 C5S C -0.0095(9) 0.1191(10) 0.8435(13) 0.095(6) Uani 0.626(18) 1 d PGU A -1 H5S H -0.0790 0.1392 0.8320 0.114 Uiso 0.626(18) 1 calc PR A -1 C6S C 0.0453(15) 0.1049(9) 0.9346(11) 0.088(6) Uani 0.626(18) 1 d PGU A -1 H6S H 0.0132 0.1154 0.9853 0.105 Uiso 0.626(18) 1 calc PR A -1 C7S C -0.0145(18) 0.1134(16) 0.8057(13) 0.065(7) Uani 0.374(18) 1 d PGU A -2 H7S H -0.0782 0.1282 0.7624 0.078 Uiso 0.374(18) 1 calc PR A -2 C8S C -0.0124(13) 0.1089(12) 0.8991(14) 0.057(6) Uani 0.374(18) 1 d PGU A -2 H8S H -0.0747 0.1206 0.9197 0.068 Uiso 0.374(18) 1 calc PR A -2 C9S C 0.0807(17) 0.0873(13) 0.9624(9) 0.055(6) Uani 0.374(18) 1 d PGU A -2 H9S H 0.0822 0.0843 1.0263 0.066 Uiso 0.374(18) 1 calc PR A -2 C10S C 0.1719(13) 0.0702(16) 0.9323(19) 0.053(7) Uani 0.374(18) 1 d PGU A -2 H10S H 0.2355 0.0555 0.9756 0.064 Uiso 0.374(18) 1 calc PR A -2 C11S C 0.170(2) 0.0747(18) 0.839(2) 0.122(13) Uani 0.374(18) 1 d PGU A -2 H11S H 0.2320 0.0630 0.8183 0.146 Uiso 0.374(18) 1 calc PR A -2 C12S C 0.077(3) 0.0963(19) 0.7756(13) 0.078(9) Uani 0.374(18) 1 d PGU A -2 H12S H 0.0751 0.0994 0.7117 0.093 Uiso 0.374(18) 1 calc PR A -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0350(7) 0.0462(7) 0.0249(6) 0.0170(5) 0.0170(5) 0.0203(6) O1 0.039(2) 0.037(2) 0.043(2) 0.0155(19) 0.0210(19) 0.0134(19) O2 0.067(3) 0.047(3) 0.055(3) 0.018(2) 0.033(2) 0.026(2) O3 0.060(3) 0.071(3) 0.034(2) 0.020(2) 0.022(2) 0.023(3) O4 0.039(2) 0.072(3) 0.036(2) 0.028(2) 0.0180(19) 0.027(2) O5 0.042(2) 0.043(2) 0.038(2) 0.0148(19) 0.0204(19) 0.019(2) O6 0.068(3) 0.035(2) 0.049(3) 0.020(2) 0.038(2) 0.025(2) O7 0.043(2) 0.049(2) 0.029(2) 0.0132(18) 0.0154(18) 0.023(2) O8 0.034(2) 0.052(2) 0.031(2) 0.022(2) 0.0145(17) 0.022(2) O9 0.037(2) 0.041(2) 0.031(2) 0.0148(18) 0.0119(17) 0.0142(19) O10 0.068(3) 0.041(2) 0.034(2) 0.0178(19) 0.030(2) 0.027(2) C1 0.045(4) 0.042(3) 0.041(4) 0.015(3) 0.020(3) 0.013(3) C2 0.047(4) 0.033(3) 0.066(5) 0.012(3) 0.024(3) 0.006(3) C3 0.082(6) 0.046(4) 0.068(5) 0.006(4) 0.043(4) 0.020(4) C4 0.085(6) 0.063(5) 0.037(4) 0.001(4) 0.026(4) 0.015(5) C5 0.061(4) 0.085(5) 0.036(4) 0.026(4) 0.028(3) 0.032(4) C6 0.057(4) 0.096(6) 0.039(4) 0.038(4) 0.030(3) 0.045(4) C7 0.045(4) 0.073(5) 0.047(4) 0.039(4) 0.023(3) 0.028(4) C8 0.036(3) 0.043(3) 0.045(4) 0.025(3) 0.012(3) 0.010(3) C9 0.028(3) 0.045(3) 0.034(3) 0.015(3) 0.008(2) 0.018(3) C10 0.036(3) 0.041(3) 0.053(4) 0.023(3) 0.018(3) 0.021(3) C11 0.040(3) 0.048(4) 0.041(4) 0.014(3) 0.012(3) 0.025(3) C12 0.037(3) 0.068(4) 0.030(3) 0.017(3) 0.012(3) 0.035(3) C13 0.032(3) 0.051(4) 0.031(3) 0.018(3) 0.011(2) 0.023(3) C14 0.027(3) 0.042(3) 0.028(3) 0.010(3) 0.011(2) 0.019(3) C15 0.037(3) 0.053(4) 0.044(4) 0.016(3) 0.010(3) 0.026(3) C16 0.027(3) 0.049(4) 0.041(4) 0.021(3) 0.008(3) 0.016(3) C17 0.038(3) 0.045(4) 0.035(3) 0.016(3) 0.008(3) 0.021(3) C18 0.035(3) 0.054(4) 0.026(3) 0.018(3) 0.011(3) 0.006(3) C19 0.050(4) 0.049(4) 0.029(3) 0.019(3) 0.011(3) 0.024(3) C20 0.042(3) 0.044(3) 0.028(3) 0.021(3) 0.018(3) 0.018(3) C21 0.040(3) 0.046(4) 0.027(3) 0.016(3) 0.015(3) 0.021(3) C22 0.034(3) 0.051(4) 0.022(3) 0.020(3) 0.006(2) 0.022(3) C23 0.061(4) 0.035(3) 0.045(4) 0.013(3) 0.023(3) 0.018(3) C24 0.049(4) 0.034(3) 0.034(3) 0.009(3) 0.014(3) 0.015(3) C25 0.056(4) 0.070(4) 0.032(3) 0.028(3) 0.029(3) 0.040(4) C26 0.036(3) 0.059(4) 0.036(3) 0.021(3) 0.017(3) 0.026(3) C27 0.037(3) 0.055(4) 0.045(4) 0.027(3) 0.020(3) 0.017(3) C28 0.029(3) 0.043(3) 0.042(4) 0.015(3) 0.013(3) 0.008(3) C29 0.045(4) 0.050(4) 0.032(3) 0.008(3) 0.012(3) 0.022(3) C30 0.047(4) 0.044(3) 0.021(3) 0.008(3) 0.010(3) 0.022(3) O1P 0.088(4) 0.076(4) 0.067(4) 0.026(3) 0.036(3) 0.031(3) O2P 0.083(4) 0.110(4) 0.102(5) 0.077(4) 0.062(4) 0.059(4) O3P 0.073(4) 0.032(2) 0.091(4) 0.018(3) 0.007(3) 0.019(3) O4P 0.091(4) 0.076(4) 0.110(5) 0.029(3) 0.062(4) 0.040(4) O5P 0.125(5) 0.101(4) 0.126(5) 0.087(4) 0.076(4) 0.064(4) O6P 0.150(6) 0.070(4) 0.090(4) 0.050(3) 0.054(4) 0.078(4) O7P 0.075(4) 0.092(4) 0.062(4) 0.012(3) 0.019(3) 0.047(4) N1 0.044(3) 0.047(3) 0.069(4) 0.030(3) 0.020(3) 0.021(3) N2 0.056(4) 0.057(4) 0.078(5) 0.020(3) 0.029(3) 0.023(3) N3 0.064(4) 0.068(4) 0.037(3) 0.011(3) 0.004(3) 0.041(4) C1P 0.036(3) 0.040(4) 0.052(4) 0.016(3) 0.007(3) 0.008(3) C2P 0.035(3) 0.028(3) 0.050(4) 0.016(3) 0.005(3) 0.006(3) C3P 0.045(4) 0.036(4) 0.063(4) 0.016(3) 0.013(3) 0.014(3) C4P 0.041(4) 0.039(4) 0.046(4) 0.013(3) 0.012(3) 0.010(3) C5P 0.049(4) 0.027(3) 0.046(4) 0.012(3) 0.004(3) 0.011(3) C6P 0.033(3) 0.035(3) 0.040(4) 0.002(3) 0.000(3) 0.014(3) C1S 0.088(9) 0.068(8) 0.065(8) 0.013(6) 0.036(7) 0.019(6) C2S 0.065(7) 0.044(6) 0.039(6) 0.008(5) 0.015(5) 0.005(5) C3S 0.058(7) 0.030(5) 0.048(6) 0.015(5) 0.004(5) 0.000(5) C4S 0.053(7) 0.056(7) 0.070(8) 0.024(6) 0.009(5) 0.010(6) C5S 0.103(9) 0.080(9) 0.090(9) 0.051(7) 0.028(7) 0.009(6) C6S 0.095(9) 0.072(8) 0.088(9) 0.029(6) 0.017(7) 0.045(7) C7S 0.071(11) 0.053(10) 0.056(10) 0.024(8) 0.016(7) 0.009(8) C8S 0.064(9) 0.044(8) 0.048(9) 0.031(7) -0.001(7) 0.015(7) C9S 0.043(9) 0.058(9) 0.057(9) 0.016(7) 0.008(7) 0.031(7) C10S 0.055(9) 0.042(9) 0.062(11) 0.020(7) 0.026(8) 0.013(7) C11S 0.135(16) 0.109(15) 0.120(16) 0.057(10) 0.049(10) 0.033(9) C12S 0.066(12) 0.073(12) 0.085(12) 0.025(8) 0.025(8) 0.024(9) _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 K1 O8 2.772(4) 2_666 ? K1 O3 2.783(4) . ? K1 O2 2.834(4) . ? K1 O9 2.865(4) 2_666 ? K1 O7 2.877(4) 2_666 ? K1 O4 2.882(4) . ? K1 O10 2.885(4) 2_666 ? K1 O1 2.890(4) . ? K1 O6 2.953(4) 2_666 ? K1 O5 2.959(4) . ? K1 C14 3.497(5) . ? K1 C9 3.516(5) . ? O1 C14 1.368(6) . ? O1 C1 1.411(6) . ? O2 C3 1.427(7) . ? O2 C2 1.430(7) . ? O3 C4 1.401(8) . ? O3 C5 1.407(7) . ? O4 C7 1.427(6) . ? O4 C6 1.437(7) . ? O5 C9 1.353(6) . ? O5 C8 1.440(6) . ? O6 C20 1.366(6) . ? O6 C23 1.429(6) . ? O6 K1 2.953(4) 2_666 ? O7 C25 1.429(6) . ? O7 C24 1.437(6) . ? O7 K1 2.877(4) 2_666 ? O8 C26 1.428(6) . ? O8 C27 1.435(7) . ? O8 K1 2.772(4) 2_666 ? O9 C28 1.414(6) . ? O9 C29 1.425(6) . ? O9 K1 2.865(4) 2_666 ? O10 C21 1.357(6) . ? O10 C30 1.439(6) . ? O10 K1 2.885(4) 2_666 ? C1 C2 1.513(8) . ? C3 C4 1.469(9) . ? C5 C6 1.473(9) . ? C7 C8 1.497(8) . ? C9 C14 1.398(7) . ? C9 C10 1.405(8) . ? C10 C11 1.383(8) . ? C11 C12 1.370(8) . ? C12 C13 1.440(8) . ? C12 C15 1.476(8) . ? C13 C14 1.380(7) . ? C15 C16 1.290(8) . ? C16 C17 1.512(8) . ? C17 C18 1.368(8) . ? C17 C22 1.394(8) . ? C18 C19 1.409(8) . ? C19 C20 1.404(8) . ? C20 C21 1.388(7) . ? C21 C22 1.402(7) . ? C23 C24 1.515(8) . ? C25 C26 1.493(8) . ? C27 C28 1.521(7) . ? C29 C30 1.499(8) . ? O1P C1P 1.292(7) . ? O2P N1 1.216(7) . ? O3P N1 1.244(6) . ? O4P N2 1.218(7) . ? O5P N2 1.238(7) . ? O6P N3 1.215(8) . ? O7P N3 1.236(7) . ? N1 C2P 1.470(7) . ? N2 C4P 1.439(8) . ? N3 C6P 1.472(7) . ? C1P C6P 1.439(8) . ? C1P C2P 1.442(8) . ? C2P C3P 1.356(8) . ? C3P C4P 1.414(8) . ? C4P C5P 1.379(8) . ? C5P C6P 1.385(8) . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C2S C3S 1.3900 . ? C3S C4S 1.3900 . ? C4S C5S 1.3900 . ? C5S C6S 1.3900 . ? C7S C8S 1.3900 . ? C7S C12S 1.3900 . ? C8S C9S 1.3900 . ? C9S C10S 1.3900 . ? C10S C11S 1.3900 . ? C11S C12S 1.3900 . ? 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 O8 K1 O3 95.41(12) 2_666 . ? O8 K1 O2 135.24(12) 2_666 . ? O3 K1 O2 61.92(12) . . ? O8 K1 O9 62.50(11) 2_666 2_666 ? O3 K1 O9 137.02(12) . 2_666 ? O2 K1 O9 158.15(11) . 2_666 ? O8 K1 O7 61.87(11) 2_666 2_666 ? O3 K1 O7 71.26(12) . 2_666 ? O2 K1 O7 74.00(12) . 2_666 ? O9 K1 O7 118.81(11) 2_666 2_666 ? O8 K1 O4 72.95(10) 2_666 . ? O3 K1 O4 61.32(13) . . ? O2 K1 O4 117.84(12) . . ? O9 K1 O4 76.54(11) 2_666 . ? O7 K1 O4 108.83(11) 2_666 . ? O8 K1 O10 92.54(11) 2_666 2_666 ? O3 K1 O10 165.65(13) . 2_666 ? O2 K1 O10 104.22(12) . 2_666 ? O9 K1 O10 57.32(10) 2_666 2_666 ? O7 K1 O10 102.36(10) 2_666 2_666 ? O4 K1 O10 132.74(12) . 2_666 ? O8 K1 O1 167.51(11) 2_666 . ? O3 K1 O1 92.22(12) . . ? O2 K1 O1 57.24(11) . . ? O9 K1 O1 105.34(11) 2_666 . ? O7 K1 O1 130.27(11) 2_666 . ? O4 K1 O1 102.38(11) . . ? O10 K1 O1 82.18(11) 2_666 . ? O8 K1 O6 90.08(11) 2_666 2_666 ? O3 K1 O6 116.35(12) . 2_666 ? O2 K1 O6 70.40(12) . 2_666 ? O9 K1 O6 100.96(11) 2_666 2_666 ? O7 K1 O6 56.42(10) 2_666 2_666 ? O4 K1 O6 162.11(11) . 2_666 ? O10 K1 O6 51.60(10) 2_666 2_666 ? O1 K1 O6 95.38(11) . 2_666 ? O8 K1 O5 118.94(11) 2_666 . ? O3 K1 O5 89.15(12) . . ? O2 K1 O5 99.92(12) . . ? O9 K1 O5 73.48(10) 2_666 . ? O7 K1 O5 160.17(10) 2_666 . ? O4 K1 O5 56.67(10) . . ? O10 K1 O5 97.42(10) 2_666 . ? O1 K1 O5 51.18(10) . . ? O6 K1 O5 140.20(10) 2_666 . ? O8 K1 C14 145.49(13) 2_666 . ? O3 K1 C14 109.30(13) . . ? O2 K1 C14 78.82(13) . . ? O9 K1 C14 83.09(12) 2_666 . ? O7 K1 C14 148.50(12) 2_666 . ? O4 K1 C14 97.74(12) . . ? O10 K1 C14 69.13(12) 2_666 . ? O1 K1 C14 22.24(11) . . ? O6 K1 C14 99.55(11) 2_666 . ? O5 K1 C14 41.11(11) . . ? O8 K1 C9 126.77(13) 2_666 . ? O3 K1 C9 107.54(13) . . ? O2 K1 C9 97.63(13) . . ? O9 K1 C9 68.28(12) 2_666 . ? O7 K1 C9 171.19(13) 2_666 . ? O4 K1 C9 77.29(12) . . ? O10 K1 C9 76.72(12) 2_666 . ? O1 K1 C9 41.01(12) . . ? O6 K1 C9 118.66(12) 2_666 . ? O5 K1 C9 22.05(11) . . ? C14 K1 C9 23.00(12) . . ? C14 O1 C1 119.6(4) . . ? C14 O1 K1 104.7(3) . . ? C1 O1 K1 113.0(3) . . ? C3 O2 C2 114.7(5) . . ? C3 O2 K1 107.1(4) . . ? C2 O2 K1 120.4(3) . . ? C4 O3 C5 112.3(5) . . ? C4 O3 K1 116.8(3) . . ? C5 O3 K1 118.9(4) . . ? C7 O4 C6 113.0(4) . . ? C7 O4 K1 121.8(3) . . ? C6 O4 K1 105.5(3) . . ? C9 O5 C8 118.6(4) . . ? C9 O5 K1 102.8(3) . . ? C8 O5 K1 111.9(3) . . ? C20 O6 C23 118.5(4) . . ? C20 O6 K1 106.8(3) . 2_666 ? C23 O6 K1 113.6(3) . 2_666 ? C25 O7 C24 113.0(4) . . ? C25 O7 K1 106.1(3) . 2_666 ? C24 O7 K1 121.6(3) . 2_666 ? C26 O8 C27 110.5(4) . . ? C26 O8 K1 117.3(3) . 2_666 ? C27 O8 K1 116.2(3) . 2_666 ? C28 O9 C29 113.0(4) . . ? C28 O9 K1 107.0(3) . 2_666 ? C29 O9 K1 120.0(3) . 2_666 ? C21 O10 C30 120.0(4) . . ? C21 O10 K1 110.9(3) . 2_666 ? C30 O10 K1 114.2(3) . 2_666 ? O1 C1 C2 105.4(4) . . ? O2 C2 C1 109.9(5) . . ? O2 C3 C4 115.3(6) . . ? O2 C3 K1 50.1(3) . . ? C4 C3 K1 82.4(4) . . ? O3 C4 C3 108.6(6) . . ? O3 C5 C6 108.9(5) . . ? O4 C6 C5 114.9(5) . . ? O4 C7 C8 108.2(4) . . ? O5 C8 C7 107.8(5) . . ? O5 C9 C14 115.1(5) . . ? O5 C9 C10 125.6(5) . . ? C14 C9 C10 119.3(5) . . ? O5 C9 K1 55.2(2) . . ? C14 C9 K1 77.7(3) . . ? C10 C9 K1 138.0(4) . . ? C11 C10 C9 119.8(5) . . ? C12 C11 C10 121.6(5) . . ? C11 C12 C13 119.2(5) . . ? C11 C12 C15 118.5(5) . . ? C13 C12 C15 122.2(6) . . ? C14 C13 C12 118.9(5) . . ? O1 C14 C13 124.9(5) . . ? O1 C14 C9 113.9(4) . . ? C13 C14 C9 121.2(5) . . ? O1 C14 K1 53.1(2) . . ? C13 C14 K1 136.8(3) . . ? C9 C14 K1 79.3(3) . . ? C16 C15 C12 129.0(6) . . ? C15 C16 C17 123.9(6) . . ? C18 C17 C22 118.1(5) . . ? C18 C17 C16 123.8(5) . . ? C22 C17 C16 118.0(5) . . ? C17 C18 C19 122.9(5) . . ? C20 C19 C18 118.5(5) . . ? O6 C20 C21 115.6(5) . . ? O6 C20 C19 125.4(5) . . ? C21 C20 C19 119.0(5) . . ? O10 C21 C20 114.4(4) . . ? O10 C21 C22 124.6(5) . . ? C20 C21 C22 121.0(5) . . ? C17 C22 C21 120.4(5) . . ? O6 C23 C24 105.9(5) . . ? O7 C24 C23 109.0(5) . . ? O7 C25 C26 113.3(4) . . ? O8 C26 C25 108.2(4) . . ? O8 C27 C28 107.3(4) . . ? O9 C28 C27 113.8(4) . . ? O9 C29 C30 110.0(5) . . ? O10 C30 C29 106.2(4) . . ? O2P N1 O3P 124.0(6) . . ? O2P N1 C2P 118.9(6) . . ? O3P N1 C2P 117.0(6) . . ? O4P N2 O5P 124.0(7) . . ? O4P N2 C4P 117.8(6) . . ? O5P N2 C4P 118.2(6) . . ? O6P N3 O7P 123.7(6) . . ? O6P N3 C6P 118.5(7) . . ? O7P N3 C6P 117.8(6) . . ? O1P C1P C6P 122.8(6) . . ? O1P C1P C2P 126.2(6) . . ? C6P C1P C2P 111.0(6) . . ? C3P C2P C1P 125.8(5) . . ? C3P C2P N1 116.5(5) . . ? C1P C2P N1 117.7(6) . . ? C2P C3P C4P 119.0(6) . . ? C5P C4P C3P 119.5(6) . . ? C5P C4P N2 119.4(6) . . ? C3P C4P N2 121.1(6) . . ? C4P C5P C6P 119.8(5) . . ? C5P C6P C1P 124.4(5) . . ? C5P C6P N3 116.2(5) . . ? C1P C6P N3 119.2(6) . . ? C2S C1S C6S 120.0 . . ? C1S C2S C3S 120.0 . . ? C4S C3S C2S 120.0 . . ? C5S C4S C3S 120.0 . . ? C4S C5S C6S 120.0 . . ? C5S C6S C1S 120.0 . . ? C8S C7S C12S 120.0 . . ? C7S C8S C9S 120.0 . . ? C10S C9S C8S 120.0 . . ? C9S C10S C11S 120.0 . . ? C12S C11S C10S 120.0 . . ? C11S C12S C7S 120.0 . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.888 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.080 # Attachment 'all-CIFs.CIF' data_1b+Na _database_code_depnum_ccdc_archive 'CCDC 780037' #TrackingRef 'all-CIFs.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H40 Cl2 Na2 O18' _chemical_formula_weight 805.50 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' Na Na 0.0362 0.0249 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 26.083(2) _cell_length_b 9.2443(9) _cell_length_c 15.8150(13) _cell_angle_alpha 90.00 _cell_angle_beta 96.659(5) _cell_angle_gamma 90.00 _cell_volume 3787.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120.0(2) _cell_measurement_reflns_used 855 _cell_measurement_theta_min 2.339 _cell_measurement_theta_max 19.796 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 0.269 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120.0(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-6K' _diffrn_measurement_method /W _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45379 _diffrn_reflns_av_R_equivalents 0.5344 _diffrn_reflns_av_sigmaI/netI 0.4776 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 29.00 _reflns_number_total 9987 _reflns_number_gt 3733 _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^)+(0.0500P)^2^+70.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0011(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9987 _refine_ls_number_parameters 470 _refine_ls_number_restraints 222 _refine_ls_R_factor_all 0.4133 _refine_ls_R_factor_gt 0.2426 _refine_ls_wR_factor_ref 0.4098 _refine_ls_wR_factor_gt 0.3541 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.111 _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 Na1 Na 0.6368(2) 0.6554(5) 0.6691(3) 0.0209(13) Uani 1 1 d . . . Na2 Na 0.1096(2) 0.9689(6) 0.3571(3) 0.0277(14) Uani 1 1 d . . . Cl1 Cl 0.62976(12) 0.9344(3) 0.77028(18) 0.0114(7) Uani 1 1 d . . . O11 O 0.6709(4) 0.8265(10) 0.7881(6) 0.029(2) Uani 1 1 d U . . O12 O 0.5929(4) 0.8813(12) 0.7031(7) 0.047(3) Uani 1 1 d . . . O13 O 0.6049(4) 0.9600(12) 0.8454(6) 0.043(3) Uani 1 1 d . . . O14 O 0.6525(4) 1.0634(11) 0.7433(7) 0.039(3) Uani 1 1 d U . . Cl2 Cl 0.10292(13) 1.2697(4) 0.4401(2) 0.0221(8) Uani 1 1 d . . . O21 O 0.1147(4) 1.2455(12) 0.3550(6) 0.043(3) Uani 1 1 d . . . O22 O 0.0897(5) 1.1319(13) 0.4742(8) 0.056(4) Uani 1 1 d U . . O23 O 0.0608(4) 1.3647(12) 0.4452(6) 0.039(3) Uani 1 1 d . . . O24 O 0.1490(4) 1.3185(13) 0.4939(7) 0.045(3) Uani 1 1 d U . . O1 O 0.5536(3) 0.5741(10) 0.6182(5) 0.021(2) Uani 1 1 d . . . O2 O 0.6068(3) 0.4971(9) 0.7694(5) 0.020(2) Uani 1 1 d U . . O3 O 0.7067(3) 0.5072(10) 0.7277(5) 0.020(2) Uani 1 1 d U . . O4 O 0.7101(4) 0.7211(11) 0.6032(6) 0.029(2) Uani 1 1 d U . . O5 O 0.6128(3) 0.7086(9) 0.5239(5) 0.016(2) Uani 1 1 d U . . O6 O 0.1453(3) 0.8158(10) 0.4654(5) 0.020(2) Uani 1 1 d U . . O7 O 0.0461(3) 0.7997(10) 0.3949(6) 0.022(2) Uani 1 1 d U . . O8 O 0.0343(4) 0.9844(10) 0.2590(6) 0.029(2) Uani 1 1 d U . . O9 O 0.1341(3) 0.9779(9) 0.2116(5) 0.017(2) Uani 1 1 d U . . O10 O 0.1993(3) 0.9412(10) 0.3578(5) 0.024(2) Uani 1 1 d U . . C1 C 0.5253(6) 0.5226(16) 0.6839(9) 0.033(4) Uani 1 1 d . . . H1A H 0.4940 0.4707 0.6589 0.040 Uiso 1 1 calc R . . H1B H 0.5146 0.6046 0.7181 0.040 Uiso 1 1 calc R . . C2 C 0.5604(5) 0.4203(15) 0.7401(8) 0.020(3) Uani 1 1 d U . . H2A H 0.5430 0.3880 0.7892 0.024 Uiso 1 1 calc R . . H2B H 0.5686 0.3340 0.7072 0.024 Uiso 1 1 calc R . . C3 C 0.6462(5) 0.4029(15) 0.8110(9) 0.024(3) Uani 1 1 d U . . H3A H 0.6466 0.3104 0.7796 0.029 Uiso 1 1 calc R . . H3B H 0.6387 0.3815 0.8697 0.029 Uiso 1 1 calc R . . C4 C 0.6980(5) 0.4765(15) 0.8134(9) 0.026(3) Uani 1 1 d U . . H4A H 0.6981 0.5672 0.8467 0.032 Uiso 1 1 calc R . . H4B H 0.7255 0.4125 0.8406 0.032 Uiso 1 1 calc R . . C5 C 0.7532(6) 0.5837(18) 0.7201(9) 0.033(4) Uani 1 1 d . . . H5A H 0.7832 0.5209 0.7387 0.040 Uiso 1 1 calc R . . H5B H 0.7552 0.6699 0.7574 0.040 Uiso 1 1 calc R . . C6 C 0.7554(6) 0.6299(18) 0.6294(9) 0.033(4) Uani 1 1 d . . . H6A H 0.7875 0.6849 0.6247 0.039 Uiso 1 1 calc R . . H6B H 0.7551 0.5439 0.5920 0.039 Uiso 1 1 calc R . . C7 C 0.7016(5) 0.7348(15) 0.5123(7) 0.016(3) Uani 1 1 d U . . H7A H 0.7037 0.6386 0.4854 0.019 Uiso 1 1 calc R . . H7B H 0.7282 0.7981 0.4921 0.019 Uiso 1 1 calc R . . C8 C 0.6479(5) 0.8000(14) 0.4880(9) 0.026(3) Uani 1 1 d U . . H8A H 0.6463 0.8993 0.5109 0.031 Uiso 1 1 calc R . . H8B H 0.6397 0.8039 0.4253 0.031 Uiso 1 1 calc R . . C9 C 0.5606(5) 0.7356(14) 0.5063(8) 0.017(3) Uani 1 1 d U . . C10 C 0.5392(5) 0.8333(13) 0.4410(7) 0.012(3) Uani 1 1 d U . . H10A H 0.5604 0.8850 0.4065 0.014 Uiso 1 1 calc R . . C11 C 0.4850(5) 0.8485(15) 0.4306(8) 0.021(3) Uani 1 1 d U . . H11A H 0.4703 0.9164 0.3897 0.025 Uiso 1 1 calc R . . C12 C 0.4523(5) 0.7720(14) 0.4755(7) 0.012(3) Uani 1 1 d U . . C13 C 0.4763(5) 0.6780(14) 0.5417(8) 0.018(3) Uani 1 1 d U . . H13A H 0.4553 0.6272 0.5770 0.022 Uiso 1 1 calc R . . C14 C 0.5284(5) 0.6613(14) 0.5543(7) 0.014(3) Uani 1 1 d U . . C15 C 0.3960(5) 0.7888(14) 0.4602(7) 0.014(3) Uani 1 1 d U . . H15A H 0.3836 0.8631 0.4217 0.017 Uiso 1 1 calc R . . C16 C 0.3607(5) 0.7123(15) 0.4939(9) 0.024(3) Uani 1 1 d U . . H16A H 0.3729 0.6319 0.5279 0.029 Uiso 1 1 calc R . . C17 C 0.3061(6) 0.7374(16) 0.4849(9) 0.027(3) Uani 1 1 d U . . C18 C 0.2750(5) 0.6712(15) 0.5395(8) 0.024(3) Uani 1 1 d U . . H18A H 0.2912 0.6086 0.5822 0.028 Uiso 1 1 calc R . . C19 C 0.2213(5) 0.6908(15) 0.5358(8) 0.022(3) Uani 1 1 d U . . H19A H 0.2019 0.6429 0.5748 0.026 Uiso 1 1 calc R . . C20 C 0.1972(5) 0.7824(15) 0.4732(8) 0.019(3) Uani 1 1 d U . . C21 C 0.2268(5) 0.8511(15) 0.4160(8) 0.020(3) Uani 1 1 d U . . C22 C 0.2789(5) 0.8268(14) 0.4211(8) 0.017(3) Uani 1 1 d U . . H22A H 0.2978 0.8714 0.3804 0.020 Uiso 1 1 calc R . . C23 C 0.1113(6) 0.7161(18) 0.5025(10) 0.042(5) Uani 1 1 d . . . H23A H 0.1214 0.7069 0.5645 0.050 Uiso 1 1 calc R . . H23B H 0.1127 0.6192 0.4762 0.050 Uiso 1 1 calc R . . C24 C 0.0586(5) 0.7779(17) 0.4852(8) 0.025(3) Uani 1 1 d U . . H24A H 0.0332 0.7112 0.5063 0.030 Uiso 1 1 calc R . . H24B H 0.0569 0.8713 0.5154 0.030 Uiso 1 1 calc R . . C25 C -0.0020(5) 0.8740(15) 0.3740(8) 0.022(3) Uani 1 1 d U . . H25A H -0.0013 0.9695 0.4024 0.027 Uiso 1 1 calc R . . H25B H -0.0309 0.8167 0.3919 0.027 Uiso 1 1 calc R . . C26 C -0.0076(6) 0.8914(18) 0.2785(9) 0.034(4) Uani 1 1 d . . . H26A H -0.0054 0.7962 0.2505 0.041 Uiso 1 1 calc R . . H26B H -0.0413 0.9359 0.2582 0.041 Uiso 1 1 calc R . . C27 C 0.0435(5) 0.9817(14) 0.1706(8) 0.018(3) Uani 1 1 d U . . H27A H 0.0148 1.0291 0.1347 0.021 Uiso 1 1 calc R . . H27B H 0.0464 0.8806 0.1510 0.021 Uiso 1 1 calc R . . C28 C 0.0937(6) 1.0627(16) 0.1648(8) 0.029(4) Uani 1 1 d . . . H28A H 0.1002 1.0731 0.1047 0.035 Uiso 1 1 calc R . . H28B H 0.0922 1.1603 0.1901 0.035 Uiso 1 1 calc R . . C29 C 0.1822(5) 1.0587(15) 0.2246(8) 0.022(3) Uani 1 1 d U . . H29A H 0.1767 1.1521 0.2528 0.027 Uiso 1 1 calc R . . H29B H 0.1949 1.0788 0.1692 0.027 Uiso 1 1 calc R . . C30 C 0.2215(5) 0.9677(15) 0.2803(8) 0.023(3) Uani 1 1 d U . . H30A H 0.2280 0.8753 0.2516 0.028 Uiso 1 1 calc R . . H30B H 0.2546 1.0204 0.2921 0.028 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 Na1 0.029(3) 0.009(3) 0.025(3) 0.002(2) 0.003(2) 0.000(2) Na2 0.028(3) 0.027(3) 0.030(3) 0.015(3) 0.008(3) -0.006(3) Cl1 0.0209(17) 0.0067(14) 0.0069(14) 0.0017(12) 0.0021(12) 0.0019(14) O11 0.029(5) 0.023(5) 0.037(5) -0.009(4) 0.005(4) 0.010(4) O12 0.049(7) 0.038(7) 0.051(7) -0.014(6) -0.006(6) 0.012(6) O13 0.064(8) 0.047(7) 0.022(5) -0.001(5) 0.020(5) 0.013(6) O14 0.059(6) 0.015(5) 0.048(6) 0.012(5) 0.019(5) 0.001(5) Cl2 0.0215(18) 0.0213(19) 0.0251(18) -0.0039(16) 0.0103(14) 0.0012(16) O21 0.055(7) 0.043(7) 0.031(6) -0.017(6) 0.002(5) 0.015(6) O22 0.076(7) 0.041(6) 0.054(6) 0.010(5) 0.019(6) -0.002(6) O23 0.041(7) 0.046(7) 0.030(6) -0.008(5) -0.001(5) 0.027(6) O24 0.031(5) 0.052(6) 0.048(6) -0.024(5) -0.007(5) -0.011(5) O1 0.016(5) 0.031(6) 0.016(5) 0.004(4) 0.002(4) -0.001(4) O2 0.019(4) 0.014(4) 0.024(4) 0.006(3) 0.001(3) 0.002(3) O3 0.025(4) 0.020(4) 0.015(4) -0.006(3) 0.006(3) 0.002(3) O4 0.027(5) 0.041(6) 0.018(4) -0.008(4) -0.003(4) -0.003(5) O5 0.019(4) 0.012(4) 0.018(4) -0.005(3) 0.006(3) -0.004(3) O6 0.019(5) 0.022(5) 0.020(4) 0.012(4) 0.007(4) 0.003(4) O7 0.021(5) 0.020(5) 0.026(5) -0.008(4) 0.011(4) 0.000(4) O8 0.028(5) 0.024(5) 0.036(5) 0.000(4) 0.013(4) -0.010(4) O9 0.024(4) 0.011(4) 0.015(3) -0.001(3) 0.001(3) 0.007(3) O10 0.030(5) 0.016(5) 0.022(4) 0.007(4) -0.009(4) -0.003(4) C1 0.041(10) 0.025(9) 0.036(9) 0.004(7) 0.017(8) -0.006(8) C2 0.024(6) 0.016(6) 0.020(6) 0.006(5) 0.006(5) -0.003(5) C3 0.027(5) 0.019(5) 0.025(5) 0.008(4) 0.000(4) 0.004(4) C4 0.037(7) 0.015(6) 0.027(6) 0.007(5) 0.003(6) 0.010(6) C5 0.043(10) 0.033(10) 0.024(8) 0.000(7) 0.009(7) 0.008(8) C6 0.025(8) 0.054(11) 0.019(8) 0.003(8) 0.006(6) 0.010(8) C7 0.016(5) 0.018(5) 0.016(4) -0.001(4) 0.006(4) 0.004(4) C8 0.044(7) 0.009(6) 0.023(6) -0.003(5) -0.001(6) -0.005(6) C9 0.019(4) 0.014(4) 0.017(4) -0.003(3) 0.001(3) 0.003(3) C10 0.017(6) 0.008(5) 0.012(5) -0.002(5) 0.006(5) -0.002(5) C11 0.030(7) 0.013(6) 0.024(6) -0.005(5) 0.014(5) -0.007(5) C12 0.013(4) 0.011(4) 0.012(3) -0.003(3) 0.003(3) -0.001(3) C13 0.024(5) 0.018(5) 0.014(4) -0.003(4) 0.005(4) -0.007(4) C14 0.016(5) 0.015(5) 0.009(4) -0.004(4) -0.002(4) -0.002(4) C15 0.016(5) 0.014(5) 0.012(4) -0.002(4) -0.002(4) 0.008(4) C16 0.028(5) 0.017(5) 0.026(5) 0.004(4) 0.002(4) -0.001(4) C17 0.034(7) 0.022(7) 0.027(6) 0.009(6) 0.006(6) -0.008(6) C18 0.030(7) 0.017(6) 0.022(6) 0.009(5) -0.004(5) -0.001(6) C19 0.024(5) 0.019(5) 0.022(5) 0.008(4) 0.004(4) 0.001(4) C20 0.023(6) 0.018(6) 0.017(6) -0.008(5) 0.001(5) -0.005(5) C21 0.021(6) 0.016(6) 0.025(6) -0.002(5) 0.004(5) 0.005(5) C22 0.024(6) 0.010(6) 0.017(6) -0.002(5) 0.008(5) -0.003(5) C23 0.040(10) 0.039(10) 0.047(10) 0.033(9) 0.009(8) 0.014(8) C24 0.018(6) 0.034(7) 0.026(6) 0.000(6) 0.008(5) 0.002(6) C25 0.022(5) 0.019(5) 0.027(5) -0.004(4) 0.009(4) -0.003(4) C26 0.028(9) 0.041(10) 0.035(9) -0.001(8) 0.003(7) -0.017(8) C27 0.022(5) 0.013(5) 0.019(5) 0.004(4) 0.003(4) 0.002(4) C28 0.052(10) 0.017(8) 0.018(7) -0.002(6) 0.003(7) -0.002(8) C29 0.027(5) 0.024(5) 0.015(4) 0.005(4) 0.003(4) 0.004(4) C30 0.023(5) 0.024(5) 0.023(5) 0.006(4) 0.005(4) -0.001(4) _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 Na1 O1 2.350(10) . ? Na1 O2 2.358(10) . ? Na1 O4 2.361(11) . ? Na1 O5 2.362(9) . ? Na1 O3 2.379(10) . ? Na1 O12 2.471(12) . ? Na1 O11 2.539(11) . ? Na1 Cl1 3.052(6) . ? Na1 C4 3.105(14) . ? Na1 C5 3.120(16) . ? Na2 O6 2.331(10) . ? Na2 O10 2.353(11) . ? Na2 O8 2.361(11) . ? Na2 O7 2.404(10) . ? Na2 O9 2.460(10) . ? Na2 O22 2.488(14) . ? Na2 O21 2.561(13) . ? Na2 C25 3.080(15) . ? Na2 Cl2 3.088(7) . ? Na2 C29 3.097(14) . ? Na2 C24 3.101(15) . ? Cl1 O14 1.419(10) . ? Cl1 O12 1.434(11) . ? Cl1 O13 1.436(10) . ? Cl1 O11 1.469(10) . ? Cl2 O23 1.415(10) . ? Cl2 O21 1.432(10) . ? Cl2 O22 1.440(12) . ? Cl2 O24 1.462(10) . ? O1 C14 1.396(14) . ? O1 C1 1.424(16) . ? O2 C2 1.433(15) . ? O2 C3 1.446(15) . ? O3 C5 1.422(17) . ? O3 C4 1.429(15) . ? O4 C7 1.435(14) . ? O4 C6 1.470(17) . ? O5 C9 1.379(15) . ? O5 C8 1.413(16) . ? O6 C20 1.379(16) . ? O6 C23 1.450(17) . ? O7 C25 1.434(15) . ? O7 C24 1.442(15) . ? O8 C27 1.445(15) . ? O8 C26 1.451(16) . ? O9 C28 1.446(15) . ? O9 C29 1.454(16) . ? O10 C21 1.379(15) . ? O10 C30 1.437(15) . ? C1 C2 1.527(19) . ? C3 C4 1.508(19) . ? C5 C6 1.504(19) . ? C7 C8 1.532(18) . ? C9 C14 1.380(18) . ? C9 C10 1.436(17) . ? C10 C11 1.410(18) . ? C11 C12 1.368(17) . ? C12 C13 1.447(17) . ? C12 C15 1.467(17) . ? C13 C14 1.359(17) . ? C15 C16 1.321(18) . ? C16 C17 1.433(19) . ? C17 C18 1.393(19) . ? C17 C22 1.428(18) . ? C18 C19 1.408(19) . ? C19 C20 1.396(18) . ? C20 C21 1.409(18) . ? C21 C22 1.369(18) . ? C23 C24 1.484(19) . ? C25 C26 1.509(19) . ? C27 C28 1.520(19) . ? C29 C30 1.524(17) . ? 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 Na1 O2 70.5(3) . . ? O1 Na1 O4 134.0(4) . . ? O2 Na1 O4 143.7(4) . . ? O1 Na1 O5 66.6(3) . . ? O2 Na1 O5 135.4(4) . . ? O4 Na1 O5 69.8(3) . . ? O1 Na1 O3 125.8(4) . . ? O2 Na1 O3 71.3(3) . . ? O4 Na1 O3 72.4(3) . . ? O5 Na1 O3 127.2(4) . . ? O1 Na1 O12 84.9(4) . . ? O2 Na1 O12 100.3(4) . . ? O4 Na1 O12 107.4(4) . . ? O5 Na1 O12 87.6(4) . . ? O3 Na1 O12 139.0(4) . . ? O1 Na1 O11 133.1(4) . . ? O2 Na1 O11 90.2(4) . . ? O4 Na1 O11 86.3(4) . . ? O5 Na1 O11 128.4(4) . . ? O3 Na1 O11 83.3(3) . . ? O12 Na1 O11 56.2(3) . . ? O1 Na1 Cl1 109.9(3) . . ? O2 Na1 Cl1 97.3(3) . . ? O4 Na1 Cl1 96.6(3) . . ? O5 Na1 Cl1 107.9(3) . . ? O3 Na1 Cl1 111.9(3) . . ? O12 Na1 Cl1 27.6(3) . . ? O11 Na1 Cl1 28.6(2) . . ? O1 Na1 C4 117.2(4) . . ? O2 Na1 C4 50.0(3) . . ? O4 Na1 C4 95.1(4) . . ? O5 Na1 C4 151.9(4) . . ? O3 Na1 C4 26.2(3) . . ? O12 Na1 C4 120.1(4) . . ? O11 Na1 C4 71.4(4) . . ? Cl1 Na1 C4 97.0(3) . . ? O1 Na1 C5 148.6(4) . . ? O2 Na1 C5 94.8(4) . . ? O4 Na1 C5 49.9(4) . . ? O5 Na1 C5 115.9(4) . . ? O3 Na1 C5 25.7(4) . . ? O12 Na1 C5 125.8(4) . . ? O11 Na1 C5 72.2(4) . . ? Cl1 Na1 C5 99.2(3) . . ? C4 Na1 C5 45.2(4) . . ? O6 Na2 O10 67.5(3) . . ? O6 Na2 O8 138.6(4) . . ? O10 Na2 O8 139.5(4) . . ? O6 Na2 O7 69.5(3) . . ? O10 Na2 O7 129.9(4) . . ? O8 Na2 O7 70.0(3) . . ? O6 Na2 O9 125.6(4) . . ? O10 Na2 O9 69.0(3) . . ? O8 Na2 O9 70.7(3) . . ? O7 Na2 O9 121.1(4) . . ? O6 Na2 O22 85.5(4) . . ? O10 Na2 O22 110.8(4) . . ? O8 Na2 O22 102.9(4) . . ? O7 Na2 O22 90.0(4) . . ? O9 Na2 O22 140.8(4) . . ? O6 Na2 O21 126.8(4) . . ? O10 Na2 O21 93.2(4) . . ? O8 Na2 O21 88.4(4) . . ? O7 Na2 O21 133.8(4) . . ? O9 Na2 O21 86.3(3) . . ? O22 Na2 O21 54.6(4) . . ? O6 Na2 C25 93.7(4) . . ? O10 Na2 C25 156.6(4) . . ? O8 Na2 C25 49.7(3) . . ? O7 Na2 C25 26.9(3) . . ? O9 Na2 C25 116.2(4) . . ? O22 Na2 C25 80.1(4) . . ? O21 Na2 C25 109.7(4) . . ? O6 Na2 Cl2 105.8(3) . . ? O10 Na2 Cl2 101.6(3) . . ? O8 Na2 Cl2 98.1(3) . . ? O7 Na2 Cl2 114.0(3) . . ? O9 Na2 Cl2 113.6(3) . . ? O22 Na2 Cl2 27.3(3) . . ? O21 Na2 Cl2 27.4(2) . . ? C25 Na2 Cl2 96.9(3) . . ? O6 Na2 C29 115.8(4) . . ? O10 Na2 C29 49.2(3) . . ? O8 Na2 C29 93.8(4) . . ? O7 Na2 C29 146.7(4) . . ? O9 Na2 C29 27.4(3) . . ? O22 Na2 C29 122.5(4) . . ? O21 Na2 C29 71.8(4) . . ? C25 Na2 C29 142.5(4) . . ? Cl2 Na2 C29 96.6(3) . . ? O6 Na2 C24 48.7(3) . . ? O10 Na2 C24 115.9(4) . . ? O8 Na2 C24 94.4(4) . . ? O7 Na2 C24 26.7(3) . . ? O9 Na2 C24 143.9(4) . . ? O22 Na2 C24 73.5(4) . . ? O21 Na2 C24 127.1(4) . . ? C25 Na2 C24 45.6(3) . . ? Cl2 Na2 C24 100.7(3) . . ? C29 Na2 C24 159.6(4) . . ? O14 Cl1 O12 109.4(7) . . ? O14 Cl1 O13 110.8(7) . . ? O12 Cl1 O13 109.9(7) . . ? O14 Cl1 O11 107.9(6) . . ? O12 Cl1 O11 108.8(6) . . ? O13 Cl1 O11 110.0(6) . . ? O14 Cl1 Na1 120.0(5) . . ? O12 Cl1 Na1 53.0(4) . . ? O13 Cl1 Na1 129.2(5) . . ? O11 Cl1 Na1 55.9(4) . . ? Cl1 O11 Na1 95.5(5) . . ? Cl1 O12 Na1 99.4(6) . . ? O23 Cl2 O21 113.7(6) . . ? O23 Cl2 O22 107.9(7) . . ? O21 Cl2 O22 107.5(7) . . ? O23 Cl2 O24 111.5(7) . . ? O21 Cl2 O24 110.1(7) . . ? O22 Cl2 O24 105.8(7) . . ? O23 Cl2 Na2 131.7(5) . . ? O21 Cl2 Na2 55.4(5) . . ? O22 Cl2 Na2 52.5(5) . . ? O24 Cl2 Na2 116.3(5) . . ? Cl2 O21 Na2 97.3(6) . . ? Cl2 O22 Na2 100.2(6) . . ? C14 O1 C1 118.8(10) . . ? C14 O1 Na1 113.7(7) . . ? C1 O1 Na1 113.2(8) . . ? C2 O2 C3 112.2(10) . . ? C2 O2 Na1 115.1(7) . . ? C3 O2 Na1 113.9(7) . . ? C5 O3 C4 114.2(10) . . ? C5 O3 Na1 107.7(8) . . ? C4 O3 Na1 106.6(7) . . ? C7 O4 C6 111.1(10) . . ? C7 O4 Na1 115.1(7) . . ? C6 O4 Na1 113.1(8) . . ? C9 O5 C8 118.8(10) . . ? C9 O5 Na1 112.2(7) . . ? C8 O5 Na1 113.8(7) . . ? C20 O6 C23 117.5(10) . . ? C20 O6 Na2 120.4(8) . . ? C23 O6 Na2 118.2(8) . . ? C25 O7 C24 112.7(10) . . ? C25 O7 Na2 103.9(7) . . ? C24 O7 Na2 104.7(8) . . ? C27 O8 C26 114.1(10) . . ? C27 O8 Na2 114.6(7) . . ? C26 O8 Na2 114.4(8) . . ? C28 O9 C29 111.1(9) . . ? C28 O9 Na2 104.1(7) . . ? C29 O9 Na2 101.5(7) . . ? C21 O10 C30 116.2(10) . . ? C21 O10 Na2 120.7(8) . . ? C30 O10 Na2 118.4(7) . . ? O1 C1 C2 107.8(12) . . ? O2 C2 C1 108.0(11) . . ? O2 C3 C4 109.1(11) . . ? O3 C4 C3 107.8(11) . . ? O3 C4 Na1 47.3(6) . . ? C3 C4 Na1 80.8(7) . . ? O3 C5 C6 110.4(12) . . ? O3 C5 Na1 46.6(6) . . ? C6 C5 Na1 80.6(8) . . ? O4 C6 C5 108.3(12) . . ? O4 C7 C8 108.6(10) . . ? O5 C8 C7 106.2(10) . . ? O5 C9 C14 116.7(11) . . ? O5 C9 C10 123.5(11) . . ? C14 C9 C10 119.9(12) . . ? C11 C10 C9 116.6(12) . . ? C12 C11 C10 124.4(13) . . ? C11 C12 C13 116.2(12) . . ? C11 C12 C15 122.2(12) . . ? C13 C12 C15 121.5(11) . . ? C14 C13 C12 121.1(12) . . ? C13 C14 C9 121.7(12) . . ? C13 C14 O1 123.4(12) . . ? C9 C14 O1 114.8(11) . . ? C16 C15 C12 127.4(12) . . ? C15 C16 C17 127.2(13) . . ? C18 C17 C22 114.5(13) . . ? C18 C17 C16 120.7(13) . . ? C22 C17 C16 124.8(13) . . ? C17 C18 C19 124.5(13) . . ? C20 C19 C18 118.2(13) . . ? O6 C20 C19 123.8(12) . . ? O6 C20 C21 116.6(12) . . ? C19 C20 C21 119.5(13) . . ? C22 C21 O10 125.1(13) . . ? C22 C21 C20 120.2(12) . . ? O10 C21 C20 114.7(12) . . ? C21 C22 C17 123.1(13) . . ? O6 C23 C24 106.2(12) . . ? O7 C24 C23 109.5(11) . . ? O7 C24 Na2 48.6(6) . . ? C23 C24 Na2 83.2(8) . . ? O7 C25 C26 105.2(11) . . ? O7 C25 Na2 49.3(6) . . ? C26 C25 Na2 82.3(8) . . ? O8 C26 C25 106.7(11) . . ? O8 C27 C28 106.9(10) . . ? O9 C28 C27 106.5(11) . . ? O9 C29 C30 108.0(11) . . ? O9 C29 Na2 51.1(5) . . ? C30 C29 Na2 83.4(7) . . ? O10 C30 C29 106.1(11) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.728 _refine_diff_density_min -1.046 _refine_diff_density_rms 0.147 #===END data_1c+C3 _database_code_depnum_ccdc_archive 'CCDC 780038' #TrackingRef 'all-CIFs-revised.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H76 Cl2 N2 O20' _chemical_formula_weight 1132.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R32 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' _cell_length_a 21.0741(3) _cell_length_b 21.0741(3) _cell_length_c 33.4590(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 12868.9(3) _cell_formula_units_Z 9 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5418 _exptl_absorpt_coefficient_mu 1.659 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6538 _exptl_absorpt_correction_T_max 0.7544 _exptl_absorpt_process_details ? _exptl_special_details ; In this X-ray experiment, 5 ClO4- anions per 3 propanediammonium ions have been found, although 2 anions per organic dication are required for electrical neutrality of the diammonium compound. This discrepancy may only be eliminated if the formula unit H3N+(CH2)3NH3+ is partly statistically deprotonated. On the other hand, elemental analysis data for this complex agree well with complete protonation of this species. We cannot explain this disagreement now. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Microstar _diffrn_measurement_method /W _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14469 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 68.34 _reflns_number_total 4708 _reflns_number_gt 4541 _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 ; The bis(18-crown-6)stilbene molecule reveals a complicated disorder in crystal. This molecule is disordered over two close positions related by 2-fold axis with equal occupancies. Three crystallographically independent perchlorate anions are also disordered: they occupy two different positions with symmetry 3222 and special position in 2-fold axis. One solvate benzene molecule reveals rotation disorder over two positions with occupancies 0.66:0.34, whereas, the second benzene molecule is situated in 3-fold axis and because it has occupancy of 0.33333. The SADI commands were applied for the Cl(2)-O and Cl(3)-O bond lengths and for some bond lengths of the disordered bis(crown)stilbene molecule to attain realistic values for these parameters. The ISOR command was applied for the most non-hydrogen atoms of the strongly disordered bis(crown)stilbene molecule to avoid N.P.D. for their thermal anisotropic displacement parameters. 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^)+(0.1273P)^2^+12.5238P] 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 0.52(3) _refine_ls_number_reflns 4708 _refine_ls_number_parameters 580 _refine_ls_number_restraints 400 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1790 _refine_ls_wR_factor_gt 0.1753 _refine_ls_goodness_of_fit_ref 1.053 _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 Cl1 Cl 0.3333 0.10939(5) 0.1667 0.0681(4) Uani 1 2 d S . . O13 O 0.39455(19) 0.17863(17) 0.15639(13) 0.0859(10) Uani 1 1 d . . . O14 O 0.3161(2) 0.0616(2) 0.13253(14) 0.0974(13) Uani 1 1 d . . . Cl2 Cl 0.3333 0.6667 0.14384(10) 0.0474(6) Uani 0.50 3 d SPD . . O21 O 0.3943(2) 0.7277(2) 0.1667 0.126(2) Uani 1 2 d SDU . . O22 O 0.3333 0.6667 0.1025(4) 0.098(4) Uani 0.50 3 d SPDU . . Cl3 Cl 0.0000 0.0000 0.00847(7) 0.0509(10) Uani 0.50 3 d SPD . . O31 O 0.0000 0.0643(2) 0.0000 0.0978(18) Uani 1 2 d SDU . . O32 O 0.0000 0.0000 0.0509(2) 0.0501(18) Uani 0.50 3 d SPD . . O1 O 0.1199(10) 0.6647(12) 0.0825(7) 0.033(3) Uani 0.50 1 d PU A -1 O2 O 0.1620(11) 0.8098(9) 0.1080(6) 0.059(5) Uani 0.50 1 d PD A -1 O3 O 0.0684(5) 0.8636(4) 0.1175(2) 0.041(2) Uani 0.50 1 d PD A -1 O4 O -0.0488(15) 0.7865(16) 0.0586(10) 0.064(5) Uani 0.50 1 d P A -1 O5 O -0.0992(7) 0.6356(6) 0.0420(4) 0.042(2) Uani 0.50 1 d PU A -1 O6 O -0.0115(7) 0.5756(7) 0.0601(3) 0.035(2) Uani 0.50 1 d PU A -1 O7 O 0.3226(14) 0.4382(10) 0.2472(7) 0.042(4) Uani 0.50 1 d PU A -1 O8 O 0.4751(7) 0.5046(10) 0.2276(5) 0.045(3) Uani 0.50 1 d PDU A -1 O9 O 0.5359(11) 0.4063(11) 0.2156(6) 0.120(7) Uani 0.50 1 d PDU A -1 O10 O 0.4673(14) 0.2990(14) 0.2780(8) 0.051(3) Uani 0.50 1 d PU A -1 O11 O 0.3192(7) 0.2285(7) 0.2964(4) 0.043(2) Uani 0.50 1 d PU A -1 O12 O 0.2512(7) 0.3102(7) 0.2807(3) 0.033(2) Uani 0.50 1 d PU A -1 C1 C 0.1916(9) 0.7181(9) 0.0983(6) 0.035(3) Uani 0.50 1 d PU A -1 H1D H 0.1909 0.7150 0.1278 0.042 Uiso 0.50 1 calc PR A -1 H1E H 0.2292 0.7071 0.0882 0.042 Uiso 0.50 1 calc PR A -1 C2 C 0.2097(10) 0.7903(11) 0.0864(7) 0.036(3) Uani 0.50 1 d PDU A -1 H2A H 0.2026 0.7918 0.0573 0.043 Uiso 0.50 1 calc PR A -1 H2B H 0.2616 0.8254 0.0928 0.043 Uiso 0.50 1 calc PR A -1 C3 C 0.1805(10) 0.8856(9) 0.1027(7) 0.067(6) Uani 0.50 1 d PDU A -1 H3A H 0.2339 0.9183 0.1064 0.080 Uiso 0.50 1 calc PR A -1 H3B H 0.1677 0.8927 0.0752 0.080 Uiso 0.50 1 calc PR A -1 C4 C 0.1424(9) 0.9033(10) 0.1301(6) 0.056(4) Uani 0.50 1 d PDU A -1 H4A H 0.1605 0.9567 0.1300 0.067 Uiso 0.50 1 calc PR A -1 H4B H 0.1478 0.8885 0.1575 0.067 Uiso 0.50 1 calc PR A -1 C5 C 0.0365(9) 0.8969(9) 0.0933(5) 0.049(3) Uani 0.50 1 d PDU A -1 H5A H 0.0643 0.9147 0.0680 0.059 Uiso 0.50 1 calc PR A -1 H5B H 0.0397 0.9395 0.1077 0.059 Uiso 0.50 1 calc PR A -1 C6 C -0.0433(8) 0.8423(8) 0.0840(5) 0.055(3) Uani 0.50 1 d PU A -1 H6A H -0.0700 0.8203 0.1092 0.066 Uiso 0.50 1 calc PR A -1 H6B H -0.0663 0.8680 0.0711 0.066 Uiso 0.50 1 calc PR A -1 C7 C -0.1172(12) 0.7367(9) 0.0420(7) 0.068(5) Uani 0.50 1 d PU A -1 H7A H -0.1351 0.7639 0.0259 0.082 Uiso 0.50 1 calc PR A -1 H7B H -0.1527 0.7114 0.0639 0.082 Uiso 0.50 1 calc PR A -1 C8 C -0.1134(8) 0.6812(8) 0.0164(6) 0.050(4) Uani 0.50 1 d PU A -1 H8A H -0.1604 0.6516 0.0020 0.060 Uiso 0.50 1 calc PR A -1 H8B H -0.0738 0.7055 -0.0036 0.060 Uiso 0.50 1 calc PR A -1 C9 C -0.1046(6) 0.5756(6) 0.0194(4) 0.039(3) Uani 0.50 1 d PU A -1 H9A H -0.0702 0.5940 -0.0035 0.047 Uiso 0.50 1 calc PR A -1 H9B H -0.1550 0.5453 0.0089 0.047 Uiso 0.50 1 calc PR A -1 C10 C -0.0862(7) 0.5313(7) 0.0462(4) 0.044(2) Uani 0.50 1 d PU A -1 H10A H -0.1201 0.5138 0.0693 0.053 Uiso 0.50 1 calc PR A -1 H10B H -0.0914 0.4880 0.0317 0.053 Uiso 0.50 1 calc PR A -1 C11 C 0.0208(8) 0.5455(9) 0.0833(4) 0.037(3) Uani 0.50 1 d PU A -1 C12 C -0.0150(5) 0.4743(5) 0.0939(3) 0.0391(17) Uani 0.50 1 d PU A -1 H12A H -0.0635 0.4421 0.0850 0.047 Uiso 0.50 1 calc PR A -1 C13 C 0.0219(8) 0.4494(6) 0.1186(3) 0.034(2) Uani 0.50 1 d PU A -1 H13A H -0.0022 0.3990 0.1257 0.041 Uiso 0.50 1 calc PR A -1 C14 C 0.0916(5) 0.4950(4) 0.13290(19) 0.0340(14) Uani 0.50 1 d PU A -1 C15 C 0.1262(5) 0.5676(4) 0.1216(2) 0.0317(15) Uani 0.50 1 d PU A -1 H15A H 0.1745 0.5997 0.1310 0.038 Uiso 0.50 1 calc PR A -1 C16 C 0.0925(7) 0.5955(9) 0.0967(5) 0.035(3) Uani 0.50 1 d PU A -1 C17 C 0.1306(6) 0.4707(6) 0.1604(3) 0.033(3) Uani 0.50 1 d PU A -1 H17A H 0.1812 0.5038 0.1649 0.039 Uiso 0.50 1 calc PR A -1 C18 C 0.1006(3) 0.4067(3) 0.17914(16) 0.0376(12) Uani 0.50 1 d PU A -1 H18A H 0.0499 0.3737 0.1749 0.045 Uiso 0.50 1 calc PR A -1 C19 C 0.1398(6) 0.3833(8) 0.2058(3) 0.035(2) Uani 0.50 1 d PU A -1 C20 C 0.2141(5) 0.4260(5) 0.2150(2) 0.0350(19) Uani 0.50 1 d PU A -1 H20A H 0.2412 0.4738 0.2039 0.042 Uiso 0.50 1 calc PR A -1 C21 C 0.2494(8) 0.4015(7) 0.2395(4) 0.031(3) Uani 0.50 1 d PU A -1 C22 C 0.2118(7) 0.3308(6) 0.2567(4) 0.030(3) Uani 0.50 1 d PU A -1 C23 C 0.1340(5) 0.2879(5) 0.2493(2) 0.0420(18) Uani 0.50 1 d PU A -1 H23A H 0.1057 0.2411 0.2613 0.050 Uiso 0.50 1 calc PR A -1 C24 C 0.1010(5) 0.3157(6) 0.2245(3) 0.0416(16) Uani 0.50 1 d PU A -1 H24A H 0.0496 0.2873 0.2200 0.050 Uiso 0.50 1 calc PR A -1 C25 C 0.3656(10) 0.5132(11) 0.2321(7) 0.048(4) Uani 0.50 1 d PU A -1 H25A H 0.3455 0.5437 0.2423 0.057 Uiso 0.50 1 calc PR A -1 H25B H 0.3641 0.5134 0.2025 0.057 Uiso 0.50 1 calc PR A -1 C26 C 0.4428(14) 0.5430(15) 0.2463(9) 0.059(6) Uani 0.50 1 d PDU A -1 H26A H 0.4720 0.5958 0.2398 0.070 Uiso 0.50 1 calc PR A -1 H26B H 0.4430 0.5375 0.2757 0.070 Uiso 0.50 1 calc PR A -1 C27 C 0.5513(7) 0.5298(8) 0.2363(5) 0.042(3) Uani 0.50 1 d PDU A -1 H27A H 0.5573 0.5241 0.2652 0.050 Uiso 0.50 1 calc PR A -1 H27B H 0.5815 0.5824 0.2294 0.050 Uiso 0.50 1 calc PR A -1 C28 C 0.5762(15) 0.4853(11) 0.2122(6) 0.068(6) Uani 0.50 1 d PDU A -1 H28A H 0.5759 0.4977 0.1836 0.082 Uiso 0.50 1 calc PR A -1 H28B H 0.6277 0.5023 0.2195 0.082 Uiso 0.50 1 calc PR A -1 C29 C 0.5747(12) 0.3907(10) 0.2459(6) 0.067(5) Uani 0.50 1 d PDU A -1 H29A H 0.5796 0.4188 0.2705 0.080 Uiso 0.50 1 calc PR A -1 H29B H 0.6242 0.4037 0.2364 0.080 Uiso 0.50 1 calc PR A -1 C30 C 0.5302(9) 0.3109(10) 0.2536(5) 0.062(4) Uani 0.50 1 d PU A -1 H30A H 0.5132 0.2838 0.2281 0.075 Uiso 0.50 1 calc PR A -1 H30B H 0.5597 0.2936 0.2680 0.075 Uiso 0.50 1 calc PR A -1 C31 C 0.4274(9) 0.2238(9) 0.2907(5) 0.054(3) Uani 0.50 1 d PU A -1 H31A H 0.4062 0.1912 0.2672 0.065 Uiso 0.50 1 calc PR A -1 H31B H 0.4604 0.2105 0.3047 0.065 Uiso 0.50 1 calc PR A -1 C32 C 0.3703(9) 0.2158(9) 0.3169(6) 0.052(3) Uani 0.50 1 d PU A -1 H32A H 0.3450 0.1657 0.3282 0.063 Uiso 0.50 1 calc PR A -1 H32B H 0.3918 0.2510 0.3393 0.063 Uiso 0.50 1 calc PR A -1 C33 C 0.2650(7) 0.2253(7) 0.3206(4) 0.045(3) Uani 0.50 1 d PU A -1 H33A H 0.2868 0.2642 0.3412 0.054 Uiso 0.50 1 calc PR A -1 H33B H 0.2394 0.1773 0.3343 0.054 Uiso 0.50 1 calc PR A -1 C34 C 0.2124(8) 0.2353(6) 0.2961(4) 0.046(3) Uani 0.50 1 d PU A -1 H34A H 0.1941 0.1997 0.2738 0.055 Uiso 0.50 1 calc PR A -1 H34B H 0.1702 0.2276 0.3126 0.055 Uiso 0.50 1 calc PR A -1 N1 N 0.01237(16) 0.71409(17) 0.09744(7) 0.0474(6) Uani 1 1 d U . . H1A H -0.0072 0.7295 0.0781 0.071 Uiso 1 1 calc R . . H1B H 0.0156 0.6752 0.0882 0.071 Uiso 1 1 calc R . . H1C H 0.0579 0.7512 0.1039 0.071 Uiso 1 1 calc R . . C35 C -0.0345(2) 0.6922(3) 0.13281(9) 0.0605(10) Uani 1 1 d U . . H35A H -0.0840 0.6523 0.1253 0.073 Uiso 1 1 calc R . . H35B H -0.0392 0.7343 0.1420 0.073 Uiso 1 1 calc R . . C36 C -0.0066(2) 0.6667 0.1667 0.0442(10) Uani 1 2 d SU . . H36A H 0.0006 0.6261 0.1575 0.053 Uiso 1 1 d R . . C1S C 0.6605(3) 0.4420(3) -0.0001(2) 0.052(2) Uani 0.663(17) 1 d PGU B 1 H1SA H 0.6506 0.3963 -0.0110 0.062 Uiso 0.663(17) 1 calc PR B 1 C2S C 0.6936(4) 0.4639(4) 0.03713(18) 0.087(3) Uani 0.663(17) 1 d PGU B 1 H2SA H 0.7064 0.4333 0.0517 0.105 Uiso 0.663(17) 1 calc PR B 1 C3S C 0.7080(3) 0.5307(4) 0.05308(14) 0.074(3) Uani 0.663(17) 1 d PGU B 1 H3SA H 0.7307 0.5457 0.0785 0.089 Uiso 0.663(17) 1 calc PR B 1 C4S C 0.6893(4) 0.5756(3) 0.0318(2) 0.101(3) Uani 0.663(17) 1 d PGU B 1 H4SA H 0.6991 0.6213 0.0427 0.121 Uiso 0.663(17) 1 calc PR B 1 C5S C 0.6561(4) 0.5537(5) -0.0055(2) 0.093(4) Uani 0.663(17) 1 d PGU B 1 H5SA H 0.6433 0.5843 -0.0200 0.112 Uiso 0.663(17) 1 calc PR B 1 C6S C 0.6417(3) 0.4869(5) -0.02142(13) 0.093(4) Uani 0.663(17) 1 d PGU B 1 H6SA H 0.6191 0.4719 -0.0469 0.111 Uiso 0.663(17) 1 calc PR B 1 C7S C 0.6514(8) 0.4573(7) -0.0088(4) 0.052(5) Uani 0.337(17) 1 d PGU B 2 H7SA H 0.6331 0.4202 -0.0287 0.062 Uiso 0.337(17) 1 calc PR B 2 C8S C 0.6799(12) 0.4473(9) 0.0265(6) 0.181(18) Uani 0.337(17) 1 d PGU B 2 H8SA H 0.6811 0.4033 0.0308 0.217 Uiso 0.337(17) 1 calc PR B 2 C9S C 0.7067(11) 0.5016(13) 0.0557(4) 0.110(9) Uani 0.337(17) 1 d PGU B 2 H9SA H 0.7262 0.4948 0.0798 0.132 Uiso 0.337(17) 1 calc PR B 2 C10S C 0.7050(11) 0.5659(10) 0.0494(5) 0.117(10) Uani 0.337(17) 1 d PGU B 2 H10C H 0.7233 0.6031 0.0693 0.140 Uiso 0.337(17) 1 calc PR B 2 C11S C 0.6764(12) 0.5760(7) 0.0141(6) 0.150(13) Uani 0.337(17) 1 d PGU B 2 H11A H 0.6752 0.6199 0.0098 0.180 Uiso 0.337(17) 1 calc PR B 2 C12S C 0.6496(9) 0.5216(9) -0.0151(4) 0.073(5) Uani 0.337(17) 1 d PGU B 2 H12B H 0.6301 0.5285 -0.0392 0.088 Uiso 0.337(17) 1 calc PR B 2 C13S C 1.0183(11) 0.9318(8) 0.1905(4) 0.090(5) Uiso 0.33 1 d PG C -1 H13B H 1.0190 0.8870 0.1900 0.108 Uiso 0.33 1 calc PR C -1 C14S C 1.0838(7) 0.9982(12) 0.1914(4) 0.121(8) Uiso 0.33 1 d PG C -1 H14A H 1.1292 0.9988 0.1915 0.145 Uiso 0.33 1 calc PR C -1 C15S C 1.0829(6) 1.0636(8) 0.1922(4) 0.073(3) Uiso 0.33 1 d PG C -1 H15B H 1.1276 1.1090 0.1929 0.087 Uiso 0.33 1 calc PR C -1 C16S C 1.0164(8) 1.0627(6) 0.1921(4) 0.082(4) Uiso 0.33 1 d PG C -1 H16A H 1.0158 1.1075 0.1927 0.098 Uiso 0.33 1 calc PR C -1 C17S C 0.9510(5) 0.9963(8) 0.1912(4) 0.091(5) Uiso 0.33 1 d PG C -1 H17B H 0.9056 0.9957 0.1911 0.109 Uiso 0.33 1 calc PR C -1 C18S C 0.9519(7) 0.9308(6) 0.1904(3) 0.068(3) Uiso 0.33 1 d PG C -1 H18B H 0.9072 0.8855 0.1898 0.082 Uiso 0.33 1 calc PR C -1 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 Cl1 0.0587(8) 0.0322(4) 0.1222(11) -0.0061(4) -0.0122(7) 0.0294(4) O13 0.0645(19) 0.0491(16) 0.140(3) -0.0111(18) 0.0157(18) 0.0251(15) O14 0.094(3) 0.0634(19) 0.145(3) -0.033(2) -0.042(2) 0.047(2) Cl2 0.0289(7) 0.0289(7) 0.0843(17) 0.000 0.000 0.0144(4) O21 0.078(2) 0.078(2) 0.144(5) -0.019(2) 0.019(2) -0.019(3) O22 0.069(4) 0.069(4) 0.157(12) 0.000 0.000 0.034(2) Cl3 0.0495(8) 0.0495(8) 0.054(3) 0.000 0.000 0.0247(4) O31 0.141(5) 0.079(2) 0.094(3) 0.0292(15) 0.058(3) 0.070(2) O32 0.046(3) 0.046(3) 0.058(4) 0.000 0.000 0.0230(13) O1 0.030(6) 0.029(4) 0.032(5) 0.003(3) 0.006(4) 0.009(4) O2 0.070(10) 0.059(8) 0.068(7) -0.024(5) -0.024(5) 0.047(8) O3 0.061(4) 0.030(3) 0.044(3) -0.009(2) -0.035(3) 0.032(3) O4 0.066(12) 0.062(9) 0.057(6) 0.013(5) -0.010(7) 0.027(8) O5 0.047(4) 0.057(5) 0.026(3) -0.005(3) -0.014(2) 0.029(3) O6 0.034(4) 0.040(4) 0.037(5) 0.002(3) -0.010(3) 0.022(3) O7 0.047(7) 0.042(8) 0.030(4) -0.003(5) -0.003(4) 0.017(6) O8 0.043(6) 0.029(3) 0.048(5) 0.010(3) -0.010(4) 0.006(4) O9 0.112(10) 0.126(11) 0.134(10) 0.012(8) -0.014(7) 0.068(8) O10 0.064(9) 0.045(6) 0.045(5) 0.011(5) -0.005(6) 0.027(6) O11 0.065(6) 0.044(3) 0.028(4) 0.007(2) -0.010(3) 0.034(3) O12 0.043(4) 0.032(4) 0.028(4) 0.007(3) 0.000(3) 0.022(3) C1 0.040(5) 0.038(8) 0.032(5) -0.002(5) -0.010(4) 0.024(5) C2 0.032(5) 0.033(5) 0.035(5) -0.005(4) -0.015(4) 0.011(4) C3 0.051(9) 0.060(7) 0.087(9) -0.012(5) -0.013(6) 0.025(6) C4 0.065(7) 0.038(5) 0.063(8) -0.011(5) -0.027(5) 0.024(5) C5 0.063(8) 0.044(5) 0.053(5) 0.010(4) -0.011(5) 0.036(5) C6 0.056(7) 0.046(6) 0.067(6) 0.010(5) -0.016(5) 0.028(5) C7 0.072(7) 0.061(8) 0.071(7) -0.001(6) -0.019(5) 0.032(6) C8 0.052(5) 0.057(6) 0.043(5) -0.009(6) -0.007(4) 0.028(5) C9 0.035(4) 0.041(6) 0.035(5) -0.009(4) -0.008(3) 0.015(4) C10 0.037(5) 0.044(5) 0.051(5) -0.010(4) -0.006(4) 0.020(4) C11 0.044(7) 0.049(6) 0.038(5) 0.004(4) 0.003(5) 0.038(6) C12 0.032(4) 0.037(4) 0.042(4) -0.017(3) -0.009(3) 0.012(4) C13 0.029(6) 0.028(4) 0.040(4) -0.011(3) -0.003(4) 0.012(4) C14 0.030(4) 0.036(3) 0.037(3) -0.012(3) 0.002(3) 0.017(3) C15 0.029(4) 0.032(4) 0.031(3) -0.009(2) 0.001(3) 0.012(3) C16 0.030(6) 0.034(6) 0.036(4) -0.016(4) -0.001(5) 0.012(5) C17 0.030(4) 0.033(3) 0.028(6) -0.008(3) 0.007(3) 0.010(2) C18 0.033(3) 0.032(3) 0.044(3) -0.007(2) 0.010(2) 0.013(2) C19 0.042(5) 0.031(6) 0.033(4) 0.000(4) 0.014(3) 0.018(4) C20 0.044(5) 0.027(4) 0.028(3) 0.002(3) 0.011(3) 0.014(4) C21 0.035(6) 0.023(7) 0.028(4) 0.002(5) 0.005(4) 0.009(5) C22 0.038(4) 0.027(5) 0.027(4) 0.003(4) 0.010(3) 0.018(4) C23 0.047(4) 0.029(4) 0.042(3) 0.007(3) 0.014(3) 0.013(3) C24 0.043(4) 0.030(4) 0.040(3) -0.003(3) 0.007(3) 0.010(3) C25 0.036(8) 0.061(7) 0.038(5) 0.014(4) -0.005(5) 0.018(5) C26 0.064(11) 0.060(8) 0.056(7) 0.023(5) 0.005(7) 0.033(7) C27 0.036(5) 0.027(5) 0.054(5) 0.010(4) -0.007(3) 0.010(3) C28 0.067(8) 0.070(8) 0.057(8) 0.019(5) -0.006(5) 0.026(6) C29 0.064(7) 0.070(9) 0.072(7) 0.010(6) -0.010(5) 0.038(6) C30 0.063(8) 0.070(8) 0.062(5) 0.008(6) -0.008(6) 0.039(6) C31 0.063(8) 0.053(6) 0.048(4) 0.020(4) -0.001(6) 0.030(6) C32 0.068(7) 0.058(5) 0.043(5) 0.015(3) 0.003(6) 0.040(5) C33 0.055(6) 0.041(4) 0.041(5) 0.007(3) 0.001(4) 0.026(4) C34 0.050(6) 0.034(5) 0.045(5) 0.005(4) 0.002(4) 0.016(4) N1 0.0526(16) 0.0560(16) 0.0329(11) -0.0032(11) -0.0051(11) 0.0266(14) C35 0.059(2) 0.098(3) 0.0382(14) 0.0090(17) 0.0051(14) 0.050(2) C36 0.0408(16) 0.056(3) 0.0409(19) -0.0011(18) -0.0006(9) 0.0281(13) C1S 0.033(3) 0.072(4) 0.048(4) 0.025(3) 0.004(2) 0.024(3) C2S 0.068(4) 0.119(7) 0.076(4) 0.002(5) 0.014(3) 0.048(4) C3S 0.046(4) 0.105(7) 0.071(4) 0.017(4) 0.005(3) 0.038(4) C4S 0.080(5) 0.138(8) 0.088(6) 0.019(5) 0.021(5) 0.058(5) C5S 0.068(5) 0.142(8) 0.069(5) 0.029(6) 0.021(4) 0.053(5) C6S 0.072(5) 0.122(8) 0.062(5) 0.015(5) -0.010(4) 0.032(5) C7S 0.035(6) 0.072(8) 0.026(5) 0.016(5) 0.007(4) 0.011(5) C8S 0.18(2) 0.19(2) 0.19(2) 0.009(10) -0.011(10) 0.103(13) C9S 0.106(12) 0.105(12) 0.132(13) 0.008(9) 0.010(8) 0.063(9) C10S 0.109(12) 0.120(13) 0.121(13) -0.013(9) -0.001(9) 0.057(9) C11S 0.142(16) 0.158(16) 0.135(16) -0.022(10) 0.016(10) 0.063(10) C12S 0.062(8) 0.069(8) 0.072(8) -0.019(7) 0.005(6) 0.021(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 Cl1 O13 1.425(3) 12 ? Cl1 O13 1.425(3) . ? Cl1 O14 1.444(4) 12 ? Cl1 O14 1.444(4) . ? Cl2 O22 1.384(13) . ? Cl2 O21 1.495(5) 2_665 ? Cl2 O21 1.495(5) . ? Cl2 O21 1.495(5) 3_565 ? Cl2 Cl2 1.528(7) 10_455 ? O21 Cl2 1.495(5) 10_455 ? Cl3 Cl3 0.567(5) 4 ? Cl3 O31 1.384(5) 3 ? Cl3 O31 1.384(5) 2 ? Cl3 O31 1.384(5) . ? Cl3 O32 1.419(8) . ? Cl3 O32 1.986(8) 4 ? O31 Cl3 1.384(5) 4 ? O32 Cl3 1.986(8) 4 ? O1 C16 1.36(3) . ? O1 C1 1.46(3) . ? O2 C3 1.453(13) . ? O2 C2 1.454(12) . ? O3 C4 1.417(11) . ? O3 C5 1.439(10) . ? O4 C7 1.40(3) . ? O4 C6 1.41(4) . ? O5 C8 1.426(16) . ? O5 C9 1.428(17) . ? O6 C11 1.379(11) . ? O6 C10 1.447(17) . ? O7 C21 1.36(3) . ? O7 C25 1.46(3) . ? O8 C26 1.436(13) . ? O8 C27 1.446(10) . ? O9 C29 1.439(13) . ? O9 C28 1.447(14) . ? O10 C31 1.44(3) . ? O10 C30 1.47(4) . ? O11 C33 1.375(19) . ? O11 C32 1.410(15) . ? O12 C22 1.372(13) . ? O12 C34 1.462(16) . ? C1 C2 1.43(3) . ? C3 C4 1.39(3) . ? C5 C6 1.52(2) . ? C7 C8 1.49(2) . ? C9 C10 1.481(14) . ? C11 C12 1.347(17) . ? C11 C16 1.415(15) . ? C12 C13 1.404(15) . ? C13 C14 1.378(13) . ? C14 C15 1.378(12) . ? C14 C17 1.483(14) . ? C15 C16 1.40(2) . ? C17 C18 1.328(11) . ? C18 C19 1.461(12) . ? C19 C24 1.386(13) . ? C19 C20 1.395(15) . ? C20 C21 1.369(19) . ? C21 C22 1.414(13) . ? C22 C23 1.443(16) . ? C23 C24 1.389(13) . ? C25 C26 1.50(3) . ? C27 C28 1.52(3) . ? C29 C30 1.48(2) . ? C31 C32 1.43(2) . ? C33 C34 1.475(14) . ? N1 C35 1.460(4) . ? C35 C36 1.495(4) . ? C36 C35 1.495(4) 11_565 ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C2S C3S 1.3900 . ? C3S C4S 1.3900 . ? C4S C5S 1.3900 . ? C5S C6S 1.3900 . ? C7S C8S 1.3900 . ? C7S C12S 1.3900 . ? C8S C9S 1.3900 . ? C9S C10S 1.3900 . ? C10S C11S 1.3900 . ? C11S C12S 1.3900 . ? C13S C14S 1.3900 . ? C13S C18S 1.3900 . ? C14S C15S 1.3900 . ? C15S C16S 1.3900 . ? C16S C17S 1.3900 . ? C17S C18S 1.3900 . ? 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 O13 Cl1 O13 110.3(3) 12 . ? O13 Cl1 O14 107.8(3) 12 12 ? O13 Cl1 O14 110.3(2) . 12 ? O13 Cl1 O14 110.3(2) 12 . ? O13 Cl1 O14 107.8(3) . . ? O14 Cl1 O14 110.3(3) 12 . ? O22 Cl2 O21 120.72(15) . 2_665 ? O22 Cl2 O21 120.72(15) . . ? O21 Cl2 O21 96.2(2) 2_665 . ? O22 Cl2 O21 120.72(15) . 3_565 ? O21 Cl2 O21 96.2(2) 2_665 3_565 ? O21 Cl2 O21 96.2(2) . 3_565 ? O22 Cl2 Cl2 180.0 . 10_455 ? O21 Cl2 Cl2 59.28(15) 2_665 10_455 ? O21 Cl2 Cl2 59.28(15) . 10_455 ? O21 Cl2 Cl2 59.28(15) 3_565 10_455 ? Cl2 O21 Cl2 61.4(3) 10_455 . ? Cl3 Cl3 O31 78.18(11) 4 3 ? Cl3 Cl3 O31 78.18(11) 4 2 ? O31 Cl3 O31 115.92(7) 3 2 ? Cl3 Cl3 O31 78.18(11) 4 . ? O31 Cl3 O31 115.92(7) 3 . ? O31 Cl3 O31 115.92(7) 2 . ? Cl3 Cl3 O32 180.0 4 . ? O31 Cl3 O32 101.82(11) 3 . ? O31 Cl3 O32 101.82(11) 2 . ? O31 Cl3 O32 101.82(11) . . ? Cl3 Cl3 O32 0.0 4 4 ? O31 Cl3 O32 78.18(11) 3 4 ? O31 Cl3 O32 78.18(11) 2 4 ? O31 Cl3 O32 78.18(11) . 4 ? O32 Cl3 O32 180.0 . 4 ? Cl3 O31 Cl3 23.6(2) . 4 ? Cl3 O32 Cl3 0.0 . 4 ? C16 O1 C1 115(2) . . ? C3 O2 C2 113.9(16) . . ? C4 O3 C5 121.6(13) . . ? C7 O4 C6 119(3) . . ? C8 O5 C9 109.1(12) . . ? C11 O6 C10 120.7(12) . . ? C21 O7 C25 118(2) . . ? C26 O8 C27 117.1(16) . . ? C29 O9 C28 104.2(19) . . ? C31 O10 C30 110(2) . . ? C33 O11 C32 113.5(12) . . ? C22 O12 C34 116.7(12) . . ? C2 C1 O1 110.1(18) . . ? C1 C2 O2 108.0(15) . . ? C4 C3 O2 109.9(16) . . ? C3 C4 O3 104.9(15) . . ? O3 C5 C6 110.8(12) . . ? O4 C6 C5 110.7(18) . . ? O4 C7 C8 112(2) . . ? O5 C8 C7 107.1(15) . . ? O5 C9 C10 108.0(10) . . ? O6 C10 C9 109.3(10) . . ? C12 C11 O6 122.0(14) . . ? C12 C11 C16 122.7(13) . . ? O6 C11 C16 115.2(14) . . ? C11 C12 C13 117.7(10) . . ? C14 C13 C12 122.7(9) . . ? C13 C14 C15 117.9(8) . . ? C13 C14 C17 123.8(7) . . ? C15 C14 C17 118.3(8) . . ? C14 C15 C16 122.1(9) . . ? O1 C16 C15 128.8(14) . . ? O1 C16 C11 114.2(16) . . ? C15 C16 C11 116.9(14) . . ? C18 C17 C14 125.4(8) . . ? C17 C18 C19 124.8(9) . . ? C24 C19 C20 117.4(9) . . ? C24 C19 C18 118.6(10) . . ? C20 C19 C18 124.0(12) . . ? C21 C20 C19 122.3(10) . . ? O7 C21 C20 125.0(15) . . ? O7 C21 C22 113.6(16) . . ? C20 C21 C22 121.1(13) . . ? O12 C22 C21 117.6(13) . . ? O12 C22 C23 125.4(12) . . ? C21 C22 C23 116.9(14) . . ? C24 C23 C22 119.4(10) . . ? C19 C24 C23 122.6(9) . . ? O7 C25 C26 107(2) . . ? O8 C26 C25 110(2) . . ? O8 C27 C28 109.1(16) . . ? O9 C28 C27 119(2) . . ? O9 C29 C30 105.8(16) . . ? O10 C30 C29 107.3(18) . . ? C32 C31 O10 107.8(18) . . ? O11 C32 C31 110.9(15) . . ? O11 C33 C34 109.4(11) . . ? O12 C34 C33 107.3(11) . . ? N1 C35 C36 113.7(3) . . ? C35 C36 C35 110.1(4) 11_565 . ? C2S C1S C6S 120.0 . . ? C3S C2S C1S 120.0 . . ? C2S C3S C4S 120.0 . . ? C5S C4S C3S 120.0 . . ? C4S C5S C6S 120.0 . . ? C5S C6S C1S 120.0 . . ? C8S C7S C12S 120.0 . . ? C7S C8S C9S 120.0 . . ? C10S C9S C8S 120.0 . . ? C11S C10S C9S 120.0 . . ? C12S C11S C10S 120.0 . . ? C11S C12S C7S 120.0 . . ? C14S C13S C18S 120.0 . . ? C13S C14S C15S 120.0 . . ? C14S C15S C16S 120.0 . . ? C17S C16S C15S 120.0 . . ? C18S C17S C16S 120.0 . . ? C17S C18S C13S 120.0 . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 68.34 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.434 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.062 #===END data_1c+Cs _database_code_depnum_ccdc_archive 'CCDC 780039' #TrackingRef 'all-CIFs-revised.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H56 Cs N3 O19' _chemical_formula_weight 1087.85 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' Cs Cs -0.3680 2.1192 '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 12.7413(3) _cell_length_b 17.2121(4) _cell_length_c 23.8339(5) _cell_angle_alpha 83.200(1) _cell_angle_beta 80.486(1) _cell_angle_gamma 70.437(1) _cell_volume 4846.22(19) _cell_formula_units_Z 4 _cell_measurement_temperature 120.0(2) _cell_measurement_reflns_used 8888 _cell_measurement_theta_min 2.247 _cell_measurement_theta_max 30.212 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 0.844 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8105 _exptl_absorpt_correction_T_max 0.9511 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120.0(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-6K' _diffrn_measurement_method /W _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62607 _diffrn_reflns_av_R_equivalents 0.0774 _diffrn_reflns_av_sigmaI/netI 0.1214 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 29.00 _reflns_number_total 25689 _reflns_number_gt 11775 _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 ; Some atoms of all four independent crown-ether fragments are disordered over two positions with occupancies 0.59:0.41 [C(2), O(2), C(3), O(4) and C(2'), O(2'), C(3'), O(4')], 0.68:0.32 [C(30), C(31) and C(30'), C(31')], 0.59:0.41 [O(16) and O(16')], 0.86:0.14 [C(43) and C(43')], 0.52:0.48 [C(66), O(23), C(67), C(68) and C(66'), O(23'), C(67'), C(68')]. Two of three independent picrate anions have occupancies 0.5 and are strongly disordered about symmetry centers. One of two independent benzene molecules is also disordered with equal occupancies. The SADI commands were applied for the disordered parts of crown-ether fragments and for the strongly disordered picrate anions to attain realistic bond lengths and bond angles. The FLAT command was applied to atoms N(4), N(5), N(6), C(7P), ... ,C(12P) of one of the picrate anions to keep these atoms in plane. The ISOR command was applied for some oxygen and carbon atoms (totally 22 atoms) to avoid N.P.D. for their thermal anisotropic displacement parameters. 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^)+(0.1264P)^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 25689 _refine_ls_number_parameters 1284 _refine_ls_number_restraints 323 _refine_ls_R_factor_all 0.1801 _refine_ls_R_factor_gt 0.0808 _refine_ls_wR_factor_ref 0.2340 _refine_ls_wR_factor_gt 0.2017 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.948 _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 Cs1 Cs -0.06030(4) 0.51103(2) 0.250141(17) 0.04378(13) Uani 1 1 d . A . Cs2 Cs 1.14406(4) -0.08188(3) 0.228916(18) 0.05053(14) Uani 1 1 d . . . O1 O 0.1781(4) 0.4841(3) 0.29407(17) 0.0480(11) Uani 1 1 d . A . O3 O -0.2077(7) 0.6157(6) 0.3557(3) 0.121(3) Uani 1 1 d DU A . O5 O -0.0451(5) 0.6804(3) 0.1715(2) 0.0566(13) Uani 1 1 d . A . O6 O 0.1617(4) 0.5740(3) 0.19865(18) 0.0502(12) Uani 1 1 d . A . O7 O 0.9971(5) 0.0432(3) 0.3263(2) 0.0577(13) Uani 1 1 d . A . O8 O 1.1664(5) -0.0975(3) 0.3628(2) 0.0715(16) Uani 1 1 d . G . O9 O 1.3708(6) -0.1130(4) 0.2852(3) 0.0853(19) Uani 1 1 d . D . O10 O 1.3823(5) -0.0533(3) 0.1670(3) 0.0694(15) Uani 1 1 d . D . O11 O 1.1793(5) 0.0766(4) 0.1382(3) 0.0747(17) Uani 1 1 d . D . O12 O 0.9885(5) 0.1133(3) 0.2237(2) 0.0582(13) Uani 1 1 d . D . O13 O 0.1377(4) 0.3271(3) 0.20801(18) 0.0495(12) Uani 1 1 d . . . O14 O 0.0748(4) 0.4606(3) 0.12742(19) 0.0532(12) Uani 1 1 d . A . O15 O -0.1674(5) 0.5134(4) 0.1351(2) 0.0693(15) Uani 1 1 d . A . O16 O -0.3273(19) 0.530(2) 0.2394(5) 0.068(7) Uani 0.59(7) 1 d P A 1 O16' O -0.300(2) 0.479(4) 0.2306(16) 0.093(14) Uani 0.41(7) 1 d P A 2 O17 O -0.2196(5) 0.4240(4) 0.3330(2) 0.0683(15) Uani 1 1 d . A . O18 O 0.0031(5) 0.3130(3) 0.2993(2) 0.0556(13) Uani 1 1 d . A . O19 O 0.9510(5) -0.1609(3) 0.29749(19) 0.0559(13) Uani 1 1 d . A . O20 O 1.1833(5) -0.2592(3) 0.2917(2) 0.0655(15) Uani 1 1 d . G . O21 O 1.3086(6) -0.2639(4) 0.1829(3) 0.0859(19) Uani 1 1 d . G . O22 O 1.2351(6) -0.1358(5) 0.0994(3) 0.095(2) Uani 1 1 d . G . O24 O 0.8821(4) -0.0604(3) 0.21255(18) 0.0529(12) Uani 1 1 d . G . C1 C 0.1918(7) 0.4419(5) 0.3498(3) 0.0564(19) Uani 1 1 d D . . H1A H 0.2645 0.4398 0.3607 0.068 Uiso 1 1 calc R A 1 H1B H 0.1916 0.3845 0.3493 0.068 Uiso 1 1 calc R A 1 C2 C 0.0995(9) 0.4864(7) 0.3911(4) 0.044(3) Uani 0.588(13) 1 d PDU A 1 H2A H 0.1134 0.4619 0.4299 0.053 Uiso 0.588(13) 1 calc PR A 1 H2B H 0.0972 0.5447 0.3892 0.053 Uiso 0.588(13) 1 calc PR A 1 O2 O -0.0060(9) 0.4841(9) 0.3811(4) 0.069(4) Uani 0.588(13) 1 d PDU A 1 C3 C -0.1044(14) 0.5103(11) 0.4183(7) 0.096(6) Uani 0.588(13) 1 d PDU A 1 H3A H -0.0837 0.5082 0.4568 0.116 Uiso 0.588(13) 1 calc PR A 1 H3B H -0.1442 0.4694 0.4197 0.116 Uiso 0.588(13) 1 calc PR A 1 O4 O -0.2569(10) 0.6866(8) 0.2405(5) 0.091(5) Uani 0.588(13) 1 d P A 1 C2' C 0.0850(19) 0.4459(17) 0.3792(18) 0.163(17) Uani 0.412(13) 1 d PDU A 2 H2'A H 0.0545 0.4114 0.3602 0.195 Uiso 0.412(13) 1 calc PR A 2 H2'B H 0.0942 0.4211 0.4184 0.195 Uiso 0.412(13) 1 calc PR A 2 O2' O 0.0083(17) 0.5222(12) 0.3824(8) 0.085(6) Uani 0.412(13) 1 d PDU A 2 C3' C -0.0764(12) 0.5506(12) 0.4237(7) 0.050(5) Uani 0.412(13) 1 d PDU A 2 H3'A H -0.0583 0.5907 0.4439 0.060 Uiso 0.412(13) 1 calc PR A 2 H3'B H -0.0800 0.5037 0.4516 0.060 Uiso 0.412(13) 1 calc PR A 2 O4' O -0.2096(11) 0.7155(10) 0.2710(7) 0.070(5) Uani 0.412(13) 1 d P A 2 C4 C -0.1803(12) 0.5878(10) 0.4078(5) 0.149(5) Uani 1 1 d DU . . H4A H -0.2512 0.5903 0.4331 0.178 Uiso 1 1 calc R A 1 H4B H -0.1512 0.6282 0.4209 0.178 Uiso 1 1 calc R A 1 C5 C -0.2861(12) 0.6872(9) 0.3513(6) 0.127(4) Uani 1 1 d U . . H5A H -0.2640 0.7287 0.3678 0.152 Uiso 1 1 calc R A . H5B H -0.3564 0.6832 0.3744 0.152 Uiso 1 1 calc R . . C6 C -0.3079(17) 0.7155(12) 0.2956(8) 0.182(7) Uani 1 1 d U A . H6A H -0.3069 0.7731 0.2925 0.219 Uiso 1 1 calc R B 1 H6B H -0.3878 0.7201 0.2966 0.219 Uiso 1 1 calc R B 1 C7 C -0.2349(11) 0.7282(8) 0.1976(6) 0.133(5) Uani 1 1 d U . . H7A H -0.2971 0.7813 0.2007 0.160 Uiso 1 1 calc R A 1 H7B H -0.2486 0.7013 0.1663 0.160 Uiso 1 1 calc R A 1 C8 C -0.1424(8) 0.7518(5) 0.1744(4) 0.076(3) Uani 1 1 d . A . H8A H -0.1335 0.7918 0.1983 0.092 Uiso 1 1 calc R . . H8B H -0.1527 0.7787 0.1357 0.092 Uiso 1 1 calc R . . C9 C 0.0538(7) 0.7019(5) 0.1575(3) 0.0557(19) Uani 1 1 d . . . H9A H 0.0630 0.7308 0.1890 0.067 Uiso 1 1 calc R A . H9B H 0.0485 0.7399 0.1227 0.067 Uiso 1 1 calc R . . C10 C 0.1518(7) 0.6268(4) 0.1477(3) 0.0543(19) Uani 1 1 d . A . H10A H 0.1424 0.5976 0.1165 0.065 Uiso 1 1 calc R . . H10B H 0.2209 0.6422 0.1363 0.065 Uiso 1 1 calc R . . C11 C 0.2602(6) 0.5092(4) 0.2006(3) 0.0433(15) Uani 1 1 d . . . C12 C 0.3473(6) 0.4906(4) 0.1564(3) 0.0463(16) Uani 1 1 d . A . H12A H 0.3405 0.5223 0.1209 0.056 Uiso 1 1 calc R . . C13 C 0.4444(6) 0.4259(4) 0.1637(3) 0.0498(17) Uani 1 1 d . . . H13A H 0.5042 0.4139 0.1330 0.060 Uiso 1 1 calc R A . C14 C 0.4569(7) 0.3780(4) 0.2148(3) 0.0523(18) Uani 1 1 d . A . C15 C 0.3674(6) 0.3968(4) 0.2587(3) 0.0479(16) Uani 1 1 d . . . H15A H 0.3733 0.3640 0.2938 0.058 Uiso 1 1 calc R A . C16 C 0.2713(7) 0.4614(4) 0.2525(3) 0.0481(17) Uani 1 1 d . A . C17 C 0.5621(7) 0.3113(4) 0.2220(3) 0.0538(18) Uani 1 1 d . . . H17A H 0.6190 0.3014 0.1900 0.065 Uiso 1 1 calc R A . C18 C 0.5856(7) 0.2627(5) 0.2699(3) 0.060(2) Uani 1 1 d . A . H18A H 0.5241 0.2687 0.2995 0.072 Uiso 1 1 calc R . . C19 C 0.8865(6) 0.1323(4) 0.2589(3) 0.0472(17) Uani 1 1 d . . . C20 C 0.7865(6) 0.1839(4) 0.2433(3) 0.0486(17) Uani 1 1 d . A . H20A H 0.7829 0.2068 0.2052 0.058 Uiso 1 1 calc R . . C21 C 0.6905(7) 0.2029(4) 0.2829(3) 0.0555(19) Uani 1 1 d . . . C22 C 0.6968(7) 0.1662(5) 0.3384(3) 0.0589(19) Uani 1 1 d . A . H22A H 0.6314 0.1787 0.3658 0.071 Uiso 1 1 calc R . . C23 C 0.7978(7) 0.1115(4) 0.3539(3) 0.0541(18) Uani 1 1 d . . . H23A H 0.8011 0.0868 0.3916 0.065 Uiso 1 1 calc R A . C24 C 0.8928(7) 0.0935(4) 0.3143(3) 0.0486(17) Uani 1 1 d . A . C25 C 1.0093(8) 0.0170(5) 0.3850(3) 0.066(2) Uani 1 1 d . . . H25A H 0.9679 -0.0226 0.3988 0.079 Uiso 1 1 calc R G . H25B H 0.9780 0.0651 0.4087 0.079 Uiso 1 1 calc R . . C26 C 1.1302(8) -0.0229(5) 0.3896(3) 0.071(2) Uani 1 1 d . G . H26A H 1.1733 0.0136 0.3709 0.085 Uiso 1 1 calc R . . H26B H 1.1420 -0.0337 0.4302 0.085 Uiso 1 1 calc R . . C27 C 1.2771(9) -0.1525(6) 0.3728(4) 0.084(3) Uani 1 1 d . . . H27A H 1.2879 -0.2074 0.3595 0.100 Uiso 1 1 calc R G . H27B H 1.2807 -0.1596 0.4143 0.100 Uiso 1 1 calc R . . C28 C 1.3717(8) -0.1223(7) 0.3434(5) 0.089(3) Uani 1 1 d . D . H28A H 1.3638 -0.0687 0.3577 0.107 Uiso 1 1 calc R . . H28B H 1.4444 -0.1623 0.3522 0.107 Uiso 1 1 calc R . . C29 C 1.4574(8) -0.0891(6) 0.2530(5) 0.091(3) Uani 1 1 d . . . H29A H 1.5151 -0.1393 0.2376 0.109 Uiso 1 1 calc R C 1 H29B H 1.4925 -0.0674 0.2789 0.109 Uiso 1 1 calc R C 1 C30 C 1.4300(12) -0.0282(10) 0.2059(7) 0.081(5) Uani 0.677(17) 1 d P D 1 H30A H 1.3774 0.0242 0.2207 0.097 Uiso 0.677(17) 1 calc PR D 1 H30B H 1.4993 -0.0174 0.1866 0.097 Uiso 0.677(17) 1 calc PR D 1 C31 C 1.3623(11) 0.0060(8) 0.1160(6) 0.068(4) Uani 0.677(17) 1 d P D 1 H31A H 1.4355 0.0134 0.1002 0.082 Uiso 0.677(17) 1 calc PR D 1 H31B H 1.3422 -0.0218 0.0874 0.082 Uiso 0.677(17) 1 calc PR D 1 C30' C 1.489(2) -0.100(2) 0.1944(12) 0.071(9) Uani 0.323(17) 1 d PU D 2 H30C H 1.5141 -0.1595 0.1872 0.085 Uiso 0.323(17) 1 calc PR D 2 H30D H 1.5499 -0.0772 0.1789 0.085 Uiso 0.323(17) 1 calc PR D 2 C31' C 1.383(2) 0.0221(14) 0.1521(11) 0.055(7) Uani 0.323(17) 1 d PU D 2 H31C H 1.4560 0.0189 0.1288 0.066 Uiso 0.323(17) 1 calc PR D 2 H31D H 1.3793 0.0491 0.1872 0.066 Uiso 0.323(17) 1 calc PR D 2 C32 C 1.2900(9) 0.0780(8) 0.1189(5) 0.106(4) Uani 1 1 d U . . H32A H 1.2916 0.1076 0.0807 0.127 Uiso 1 1 calc R D 1 H32B H 1.3110 0.1092 0.1451 0.127 Uiso 1 1 calc R D 1 C33 C 1.1111(9) 0.1578(5) 0.1546(3) 0.072(3) Uani 1 1 d . . . H33A H 1.1152 0.1983 0.1219 0.087 Uiso 1 1 calc R D . H33B H 1.1417 0.1722 0.1861 0.087 Uiso 1 1 calc R . . C34 C 0.9929(7) 0.1642(4) 0.1732(3) 0.057(2) Uani 1 1 d . D . H34A H 0.9475 0.2222 0.1803 0.068 Uiso 1 1 calc R . . H34B H 0.9625 0.1460 0.1434 0.068 Uiso 1 1 calc R . . C35 C 0.2095(6) 0.3326(4) 0.1564(3) 0.0457(16) Uani 1 1 d . A . H35A H 0.2541 0.2767 0.1440 0.055 Uiso 1 1 calc R . . H35B H 0.2619 0.3618 0.1617 0.055 Uiso 1 1 calc R . . C36 C 0.1346(7) 0.3801(4) 0.1126(3) 0.0508(18) Uani 1 1 d . . . H36A H 0.1810 0.3819 0.0752 0.061 Uiso 1 1 calc R A . H36B H 0.0811 0.3512 0.1090 0.061 Uiso 1 1 calc R . . C37 C 0.0083(8) 0.5121(5) 0.0855(3) 0.071(2) Uani 1 1 d . . . H37A H 0.0532 0.5046 0.0473 0.085 Uiso 1 1 calc R A . H37B H -0.0116 0.5708 0.0936 0.085 Uiso 1 1 calc R . . C38 C -0.0948(9) 0.4923(7) 0.0853(4) 0.089(3) Uani 1 1 d . A . H38A H -0.1324 0.5226 0.0523 0.107 Uiso 1 1 calc R . . H38B H -0.0756 0.4324 0.0811 0.107 Uiso 1 1 calc R . . C39 C -0.2693(9) 0.4940(8) 0.1388(5) 0.110(4) Uani 1 1 d . . . H39A H -0.3013 0.5129 0.1025 0.132 Uiso 1 1 calc R A . H39B H -0.2522 0.4333 0.1442 0.132 Uiso 1 1 calc R . . C40 C -0.3500(9) 0.5316(9) 0.1843(4) 0.098(4) Uani 1 1 d . A . H40A H -0.3816 0.5906 0.1716 0.118 Uiso 1 1 calc R E 1 H40B H -0.4116 0.5078 0.1874 0.118 Uiso 1 1 calc R E 1 C41 C -0.3752(9) 0.4813(7) 0.2790(5) 0.092(3) Uani 1 1 d . . . H41A H -0.3679 0.4306 0.2608 0.111 Uiso 1 1 calc R A 1 H41B H -0.4565 0.5117 0.2873 0.111 Uiso 1 1 calc R A 1 C42 C -0.3324(11) 0.4575(10) 0.3308(6) 0.131(5) Uani 1 1 d U A . H42A H -0.3599 0.5068 0.3534 0.157 Uiso 1 1 calc R . . H42B H -0.3677 0.4170 0.3512 0.157 Uiso 1 1 calc R . . C43 C -0.1926(9) 0.3379(6) 0.3299(5) 0.076(4) Uani 0.855(15) 1 d P A 1 H43A H -0.1996 0.3263 0.2912 0.091 Uiso 0.855(15) 1 calc PR A 1 H43B H -0.2459 0.3174 0.3576 0.091 Uiso 0.855(15) 1 calc PR A 1 C43' C -0.173(3) 0.368(2) 0.3742(13) 0.021(9) Uani 0.145(15) 1 d PU A 2 H43C H -0.2300 0.3472 0.3982 0.025 Uiso 0.145(15) 1 calc PR A 2 H43D H -0.1396 0.3935 0.3988 0.025 Uiso 0.145(15) 1 calc PR A 2 C44 C -0.0783(8) 0.2954(5) 0.3422(3) 0.070(2) Uani 1 1 d . . . H44A H -0.0697 0.3120 0.3791 0.084 Uiso 1 1 calc R A 1 H44B H -0.0650 0.2350 0.3460 0.084 Uiso 1 1 calc R A 1 C45 C 0.1109(7) 0.2668(4) 0.3002(3) 0.0480(17) Uani 1 1 d . . . C46 C 0.1536(8) 0.2139(5) 0.3459(3) 0.062(2) Uani 1 1 d . A . H46A H 0.1045 0.2106 0.3801 0.074 Uiso 1 1 calc R . . C47 C 0.2638(8) 0.1669(5) 0.3430(3) 0.062(2) Uani 1 1 d . . . H47A H 0.2896 0.1307 0.3747 0.075 Uiso 1 1 calc R A . C48 C 0.3395(6) 0.1711(4) 0.2943(3) 0.0505(17) Uani 1 1 d . A . C49 C 0.2988(7) 0.2270(4) 0.2487(3) 0.0509(18) Uani 1 1 d . . . H49A H 0.3493 0.2328 0.2157 0.061 Uiso 1 1 calc R A . C50 C 0.1853(6) 0.2740(4) 0.2513(3) 0.0435(16) Uani 1 1 d . A . C51 C 0.4606(7) 0.1171(4) 0.2867(3) 0.0542(18) Uani 1 1 d . . . H51A H 0.5042 0.1243 0.2513 0.065 Uiso 1 1 calc R A . C52 C 0.5137(7) 0.0594(5) 0.3252(3) 0.060(2) Uani 1 1 d . A . H52A H 0.4707 0.0550 0.3613 0.072 Uiso 1 1 calc R . . C53 C 0.8061(7) -0.0530(4) 0.2612(3) 0.0502(18) Uani 1 1 d . . . C54 C 0.6977(7) 0.0012(4) 0.2659(3) 0.0501(17) Uani 1 1 d . A . H54A H 0.6708 0.0366 0.2340 0.060 Uiso 1 1 calc R . . C55 C 0.6272(6) 0.0038(4) 0.3183(3) 0.0497(17) Uani 1 1 d . . . C56 C 0.6677(8) -0.0483(5) 0.3630(3) 0.060(2) Uani 1 1 d . A . H56A H 0.6199 -0.0473 0.3981 0.072 Uiso 1 1 calc R . . C57 C 0.7770(7) -0.1032(5) 0.3588(3) 0.058(2) Uani 1 1 d . . . H57A H 0.8038 -0.1375 0.3911 0.069 Uiso 1 1 calc R A . C58 C 0.8459(7) -0.1073(4) 0.3077(3) 0.0487(17) Uani 1 1 d . A . C59 C 0.9964(8) -0.2164(5) 0.3442(3) 0.067(2) Uani 1 1 d . . . H59A H 0.9382 -0.2385 0.3661 0.080 Uiso 1 1 calc R G . H59B H 1.0193 -0.1861 0.3703 0.080 Uiso 1 1 calc R . . C60 C 1.0968(8) -0.2867(4) 0.3216(3) 0.062(2) Uani 1 1 d . G . H60A H 1.1255 -0.3256 0.3538 0.074 Uiso 1 1 calc R . . H60B H 1.0729 -0.3170 0.2960 0.074 Uiso 1 1 calc R . . C61 C 1.2814(7) -0.3264(5) 0.2757(4) 0.064(2) Uani 1 1 d . . . H61A H 1.2614 -0.3674 0.2576 0.077 Uiso 1 1 calc R G . H61B H 1.3170 -0.3541 0.3099 0.077 Uiso 1 1 calc R . . C62 C 1.3624(8) -0.2926(6) 0.2341(5) 0.093(3) Uani 1 1 d . G . H62A H 1.3752 -0.2464 0.2500 0.112 Uiso 1 1 calc R . . H62B H 1.4356 -0.3363 0.2256 0.112 Uiso 1 1 calc R . . C63 C 1.3828(8) -0.2458(6) 0.1363(4) 0.079(3) Uani 1 1 d U . . H63A H 1.4434 -0.2969 0.1247 0.095 Uiso 1 1 calc R G . H63B H 1.4174 -0.2068 0.1468 0.095 Uiso 1 1 calc R . . C64 C 1.3168(10) -0.2088(6) 0.0899(4) 0.086(3) Uani 1 1 d U G . H64A H 1.3686 -0.2007 0.0556 0.103 Uiso 1 1 calc R . . H64B H 1.2817 -0.2485 0.0812 0.103 Uiso 1 1 calc R . . C65 C 1.1652(10) -0.0961(8) 0.0553(4) 0.095(4) Uani 1 1 d . . . H65A H 1.1230 -0.1323 0.0486 0.114 Uiso 1 1 calc R F 1 H65B H 1.2139 -0.0892 0.0195 0.114 Uiso 1 1 calc R F 1 C66 C 1.0846(13) -0.0145(11) 0.0701(6) 0.059(4) Uani 0.520(11) 1 d P G 1 H66A H 1.1277 0.0221 0.0748 0.071 Uiso 0.520(11) 1 calc PR G 1 H66B H 1.0419 0.0097 0.0376 0.071 Uiso 0.520(11) 1 calc PR G 1 O23 O 1.0080(10) -0.0146(7) 0.1194(4) 0.048(3) Uani 0.520(11) 1 d P G 1 C67 C 0.9155(14) -0.0368(11) 0.1127(7) 0.046(4) Uani 0.520(11) 1 d P G 1 H67A H 0.9392 -0.0971 0.1091 0.055 Uiso 0.520(11) 1 calc PR G 1 H67B H 0.8856 -0.0086 0.0772 0.055 Uiso 0.520(11) 1 calc PR G 1 C68 C 0.8221(16) -0.0132(16) 0.1638(10) 0.039(4) Uani 0.520(11) 1 d P G 1 H68A H 0.7956 0.0471 0.1682 0.046 Uiso 0.520(11) 1 calc PR G 1 H68B H 0.7575 -0.0310 0.1600 0.046 Uiso 0.520(11) 1 calc PR G 1 C66' C 1.0807(19) -0.1118(15) 0.0537(9) 0.092(7) Uani 0.480(11) 1 d PU G 2 H66C H 1.1005 -0.1704 0.0456 0.110 Uiso 0.480(11) 1 calc PR G 2 H66D H 1.0415 -0.0771 0.0224 0.110 Uiso 0.480(11) 1 calc PR G 2 O23' O 1.0085(8) -0.0974(6) 0.1055(4) 0.057(4) Uani 0.480(11) 1 d P G 2 C67' C 0.951(2) -0.0161(14) 0.1180(9) 0.051(5) Uani 0.480(11) 1 d PU G 2 H67C H 1.0018 0.0080 0.1315 0.061 Uiso 0.480(11) 1 calc PR G 2 H67D H 0.9240 0.0166 0.0831 0.061 Uiso 0.480(11) 1 calc PR G 2 C68' C 0.8602(17) -0.0124(16) 0.1596(11) 0.037(5) Uani 0.480(11) 1 d PU G 2 H68C H 0.8058 -0.0300 0.1433 0.044 Uiso 0.480(11) 1 calc PR G 2 H68D H 0.8230 0.0462 0.1683 0.044 Uiso 0.480(11) 1 calc PR G 2 O1P O 0.7876(4) 0.1706(3) 0.0919(2) 0.0583(13) Uani 1 1 d D . . O2P O 0.8863(5) 0.2915(3) 0.0763(2) 0.0696(16) Uani 1 1 d D . . O3P O 0.8703(5) 0.3463(4) -0.0092(2) 0.0770(18) Uani 1 1 d D . . O4P O 0.4845(4) 0.4615(3) -0.0496(2) 0.0548(12) Uani 1 1 d . . . O5P O 0.3566(5) 0.4169(4) 0.0018(3) 0.0717(16) Uani 1 1 d . . . O6P O 0.4734(6) 0.1673(4) 0.1278(3) 0.110(3) Uani 1 1 d . . . O7P O 0.6340(7) 0.0890(5) 0.0984(4) 0.134(3) Uani 1 1 d U . . N1 N 0.8358(5) 0.3123(3) 0.0344(2) 0.0496(14) Uani 1 1 d D . . N2 N 0.4556(5) 0.4143(3) -0.0123(2) 0.0458(13) Uani 1 1 d D . . N3 N 0.5657(6) 0.1580(4) 0.1032(3) 0.0579(16) Uani 1 1 d D . . C1P C 0.7112(6) 0.2270(4) 0.0710(3) 0.0429(15) Uani 1 1 d D . . C2P C 0.7270(5) 0.3009(4) 0.0390(3) 0.0414(14) Uani 1 1 d D . . C3P C 0.6473(6) 0.3593(4) 0.0118(2) 0.0409(15) Uani 1 1 d . . . H3PA H 0.6644 0.4043 -0.0103 0.049 Uiso 1 1 calc R . . C4P C 0.5405(5) 0.3528(4) 0.0166(3) 0.0412(14) Uani 1 1 d D . . C5P C 0.5125(6) 0.2880(4) 0.0492(3) 0.0422(15) Uani 1 1 d . . . H5PA H 0.4380 0.2859 0.0545 0.051 Uiso 1 1 calc R . . C6P C 0.5966(6) 0.2274(4) 0.0734(3) 0.0413(15) Uani 1 1 d D . . C1S C 0.1699(11) 0.2440(8) -0.0143(4) 0.098(3) Uani 1 1 d . . . H1SA H 0.1101 0.2930 -0.0047 0.117 Uiso 1 1 calc R . . C2S C 0.1519(10) 0.1733(8) -0.0107(4) 0.091(3) Uani 1 1 d . . . H2SA H 0.0808 0.1696 0.0066 0.110 Uiso 1 1 calc R . . C3S C 0.2296(15) 0.1073(8) -0.0305(5) 0.118(5) Uani 1 1 d . . . H3SA H 0.2125 0.0579 -0.0318 0.142 Uiso 1 1 calc R . . C4S C 0.3351(14) 0.1102(12) -0.0490(6) 0.151(7) Uani 1 1 d . . . H4SA H 0.3930 0.0612 -0.0607 0.181 Uiso 1 1 calc R . . C5S C 0.3594(15) 0.1802(17) -0.0513(9) 0.181(10) Uani 1 1 d . . . H5SA H 0.4322 0.1826 -0.0660 0.217 Uiso 1 1 calc R . . C6S C 0.2772(18) 0.2463(12) -0.0321(6) 0.147(6) Uani 1 1 d . . . H6SA H 0.2930 0.2962 -0.0307 0.177 Uiso 1 1 calc R . . O8P O 0.2145(17) 0.1476(14) 0.4881(13) 0.221(12) Uiso 0.50 1 d PD H -1 O9P O 0.247(2) 0.2938(16) 0.4751(16) 0.32(2) Uiso 0.50 1 d PD H -1 O10P O 0.420(2) 0.2871(17) 0.4420(14) 0.279(17) Uiso 0.50 1 d PD H -1 O11P O 0.7334(16) 0.0720(10) 0.4881(7) 0.118(5) Uiso 0.50 1 d PD H -1 O12P O 0.7086(19) -0.0468(10) 0.5132(9) 0.148(7) Uiso 0.50 1 d PD H -1 O13P O 0.388(3) -0.1090(17) 0.5022(14) 0.252(14) Uiso 0.50 1 d PD H -1 O14P O 0.232(2) -0.003(2) 0.5119(15) 0.258(16) Uiso 0.50 1 d PD H -1 N4 N 0.352(2) 0.2633(11) 0.4758(11) 0.32(3) Uiso 0.50 1 d PD H -1 N5 N 0.6717(12) 0.0307(10) 0.5015(8) 0.113(6) Uiso 0.50 1 d PD H -1 N6 N 0.336(2) -0.0308(14) 0.4977(12) 0.208 Uiso 0.50 1 d PD H -1 C7P C 0.3233(11) 0.1225(9) 0.4858(6) 0.143(11) Uiso 0.50 1 d PGD H -1 C8P C 0.3823(12) 0.1780(7) 0.4830(6) 0.159(12) Uiso 0.50 1 d PGD H -1 C9P C 0.4963(12) 0.1492(8) 0.4881(5) 0.151(11) Uiso 0.50 1 d PGD H -1 H9PA H 0.5366 0.1871 0.4862 0.181 Uiso 0.50 1 calc PR H -1 C10P C 0.5513(10) 0.0648(8) 0.4958(6) 0.086(6) Uiso 0.50 1 d PGD H -1 C11P C 0.4924(12) 0.0093(7) 0.4986(8) 0.105(5) Uiso 0.50 1 d PGD H -1 H11B H 0.5300 -0.0484 0.5039 0.126 Uiso 0.50 1 calc PR H -1 C12P C 0.3783(12) 0.0381(8) 0.4936(8) 0.149(11) Uiso 0.50 1 d PGD H -1 O15P O 0.6181(12) 0.4779(9) 0.6103(5) 0.073(4) Uiso 0.50 1 d PD I -1 O16P O 0.5440(12) 0.3546(8) 0.6150(6) 0.074(3) Uiso 0.50 1 d PD I -1 O17P O 0.531(2) 0.3119(13) 0.5339(8) 0.176(9) Uiso 0.50 1 d PD I -1 O18P O 0.351(3) 0.543(2) 0.4057(16) 0.248(19) Uiso 0.50 1 d PD I -1 O19P O 0.429(3) 0.6393(19) 0.3842(18) 0.276 Uiso 0.50 1 d PD I -1 O20P O 0.5466(12) 0.6631(9) 0.6040(5) 0.102(4) Uiso 0.50 1 d PD I -1 O21P O 0.6841(13) 0.6497(11) 0.5362(7) 0.138(6) Uiso 0.50 1 d PD I -1 N7 N 0.5321(17) 0.3683(9) 0.5631(7) 0.111(6) Uiso 0.50 1 d PD I -1 N8 N 0.4321(15) 0.5703(12) 0.4082(7) 0.098(5) Uiso 0.50 1 d PD I -1 N9 N 0.5947(13) 0.6428(9) 0.5575(6) 0.094(5) Uiso 0.50 1 d PD I -1 C13P C 0.5794(12) 0.4999(7) 0.5617(5) 0.100(7) Uiso 0.50 1 d PGD I -1 C14P C 0.5467(14) 0.4448(6) 0.5361(6) 0.114(11) Uiso 0.50 1 d PGD I -1 C15P C 0.5000(14) 0.4692(8) 0.4855(6) 0.095(6) Uiso 0.50 1 d PG I -1 H15C H 0.4777 0.4316 0.4680 0.114 Uiso 0.50 1 calc PR I -1 C16P C 0.4860(13) 0.5486(8) 0.4606(5) 0.074(6) Uiso 0.50 1 d PGD I -1 C17P C 0.5187(12) 0.6037(6) 0.4863(5) 0.110(7) Uiso 0.50 1 d PG I -1 H17C H 0.5091 0.6580 0.4693 0.132 Uiso 0.50 1 calc PR I -1 C18P C 0.5654(10) 0.5793(6) 0.5368(5) 0.069(4) Uiso 0.50 1 d PGD I -1 C7S C -0.2061(14) 0.3521(8) 0.4949(8) 0.125(9) Uiso 0.50 1 d PG J -1 H7SA H -0.2616 0.4052 0.4941 0.150 Uiso 0.50 1 calc PR J -1 C8S C -0.2313(11) 0.2833(11) 0.4837(7) 0.115(8) Uiso 0.50 1 d PG J -1 H8SA H -0.3041 0.2894 0.4753 0.138 Uiso 0.50 1 calc PR J -1 C9S C -0.1501(15) 0.2057(9) 0.4849(8) 0.113(8) Uiso 0.50 1 d PG J -1 H9SA H -0.1673 0.1587 0.4773 0.136 Uiso 0.50 1 calc PR J -1 C10S C -0.0437(13) 0.1968(9) 0.4973(8) 0.110(9) Uiso 0.50 1 d PG J -1 H10C H 0.0119 0.1438 0.4981 0.132 Uiso 0.50 1 calc PR J -1 C11S C -0.0184(12) 0.2656(13) 0.5085(8) 0.109(8) Uiso 0.50 1 d PG J -1 H11A H 0.0543 0.2595 0.5169 0.131 Uiso 0.50 1 calc PR J -1 C12S C -0.0997(17) 0.3432(10) 0.5073(9) 0.18(2) Uiso 0.50 1 d PG J -1 H12B H -0.0824 0.3902 0.5149 0.216 Uiso 0.50 1 calc PR J -1 C13S C -0.1362(12) 0.2560(14) 0.5086(8) 0.164(13) Uiso 0.50 1 d PG K -2 H13B H -0.2150 0.2666 0.5112 0.196 Uiso 0.50 1 calc PR K -2 C14S C -0.0628(17) 0.1759(11) 0.5028(9) 0.107(9) Uiso 0.50 1 d PG K -2 H14A H -0.0913 0.1318 0.5015 0.128 Uiso 0.50 1 calc PR K -2 C15S C 0.0524(16) 0.1604(10) 0.4989(8) 0.146(11) Uiso 0.50 1 d PG K -2 H15B H 0.1026 0.1056 0.4949 0.175 Uiso 0.50 1 calc PR K -2 C16S C 0.0942(12) 0.2249(14) 0.5008(8) 0.141(10) Uiso 0.50 1 d PG K -2 H16A H 0.1729 0.2142 0.4981 0.169 Uiso 0.50 1 calc PR K -2 C17S C 0.0207(19) 0.3049(12) 0.5065(10) 0.198(17) Uiso 0.50 1 d PG K -2 H17B H 0.0492 0.3490 0.5078 0.237 Uiso 0.50 1 calc PR K -2 C18S C -0.0945(17) 0.3205(10) 0.5104(9) 0.119(11) Uiso 0.50 1 d PG K -2 H18B H -0.1447 0.3752 0.5144 0.143 Uiso 0.50 1 calc PR K -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cs1 0.0569(3) 0.0407(2) 0.0375(2) -0.00255(16) -0.00748(18) -0.0201(2) Cs2 0.0673(3) 0.0491(3) 0.0463(3) -0.00807(19) -0.0081(2) -0.0315(2) O1 0.072(3) 0.045(3) 0.027(2) 0.0025(19) -0.012(2) -0.018(2) O3 0.106(5) 0.144(6) 0.081(5) -0.037(4) -0.019(4) 0.014(5) O5 0.076(4) 0.033(2) 0.064(3) 0.003(2) -0.017(3) -0.020(2) O6 0.076(3) 0.045(3) 0.037(2) 0.007(2) -0.014(2) -0.030(3) O7 0.072(4) 0.065(3) 0.043(3) -0.001(2) -0.018(2) -0.026(3) O8 0.095(5) 0.058(3) 0.058(3) -0.004(3) -0.030(3) -0.012(3) O9 0.104(5) 0.098(5) 0.072(4) -0.016(4) -0.017(4) -0.049(4) O10 0.065(4) 0.063(4) 0.089(4) -0.007(3) -0.017(3) -0.029(3) O11 0.058(4) 0.083(4) 0.091(4) 0.020(3) -0.016(3) -0.038(3) O12 0.083(4) 0.045(3) 0.050(3) 0.008(2) -0.017(3) -0.026(3) O13 0.064(3) 0.048(3) 0.037(2) 0.000(2) 0.003(2) -0.025(2) O14 0.072(3) 0.051(3) 0.038(2) 0.003(2) -0.004(2) -0.026(3) O15 0.072(4) 0.090(4) 0.058(3) -0.015(3) -0.025(3) -0.029(3) O16 0.065(9) 0.075(16) 0.073(8) -0.024(7) 0.003(6) -0.036(10) O16' 0.076(13) 0.10(3) 0.100(17) 0.013(18) -0.019(12) -0.023(15) O17 0.066(4) 0.067(4) 0.074(4) -0.010(3) 0.006(3) -0.030(3) O18 0.075(4) 0.040(3) 0.049(3) 0.002(2) 0.003(2) -0.022(3) O19 0.084(4) 0.042(3) 0.036(3) 0.004(2) -0.004(2) -0.018(3) O20 0.098(4) 0.043(3) 0.062(3) 0.000(2) -0.017(3) -0.028(3) O21 0.098(5) 0.084(4) 0.074(4) -0.012(3) -0.007(4) -0.027(4) O22 0.072(4) 0.150(7) 0.068(4) -0.045(4) 0.016(3) -0.044(5) O24 0.077(4) 0.042(3) 0.032(2) 0.0033(19) -0.004(2) -0.012(2) C1 0.082(6) 0.059(5) 0.035(4) 0.010(3) -0.016(4) -0.032(4) C2 0.069(7) 0.033(5) 0.022(5) -0.005(4) -0.002(5) -0.006(5) O2 0.079(7) 0.084(7) 0.029(4) 0.012(5) 0.006(4) -0.018(6) C3 0.105(10) 0.113(10) 0.065(8) -0.010(7) -0.004(7) -0.030(8) O4 0.076(8) 0.116(10) 0.060(7) 0.007(7) 0.005(6) -0.015(7) C2' 0.163(19) 0.159(19) 0.161(19) 0.002(10) -0.026(10) -0.048(11) O2' 0.097(10) 0.083(9) 0.066(9) 0.007(7) 0.009(7) -0.031(8) C3' 0.055(8) 0.051(8) 0.036(7) -0.008(6) 0.002(6) -0.009(7) O4' 0.047(8) 0.103(12) 0.077(10) -0.004(8) -0.004(7) -0.048(8) C4 0.130(9) 0.183(10) 0.110(8) -0.022(7) 0.024(7) -0.035(7) C5 0.111(8) 0.119(8) 0.144(8) -0.031(7) 0.031(7) -0.044(7) C6 0.174(11) 0.164(10) 0.183(11) -0.030(8) -0.018(9) -0.015(8) C7 0.111(8) 0.110(7) 0.134(8) 0.022(7) 0.029(6) -0.009(6) C8 0.087(7) 0.036(4) 0.092(7) 0.009(4) -0.013(5) -0.007(4) C9 0.071(5) 0.052(4) 0.056(4) 0.010(3) -0.019(4) -0.036(4) C10 0.071(5) 0.056(4) 0.044(4) 0.021(3) -0.021(4) -0.034(4) C11 0.062(5) 0.037(3) 0.039(3) -0.003(3) -0.010(3) -0.025(3) C12 0.067(5) 0.043(4) 0.043(4) -0.002(3) -0.011(3) -0.035(4) C13 0.062(5) 0.048(4) 0.049(4) -0.006(3) -0.006(3) -0.029(4) C14 0.076(5) 0.039(4) 0.045(4) -0.006(3) -0.011(4) -0.022(4) C15 0.063(5) 0.039(4) 0.048(4) -0.008(3) -0.014(3) -0.020(3) C16 0.084(5) 0.038(4) 0.036(3) 0.000(3) -0.013(3) -0.037(4) C17 0.072(5) 0.047(4) 0.052(4) -0.009(3) -0.013(4) -0.027(4) C18 0.079(6) 0.051(4) 0.061(5) -0.010(4) -0.009(4) -0.033(4) C19 0.065(5) 0.036(3) 0.051(4) -0.011(3) -0.010(4) -0.026(3) C20 0.067(5) 0.036(3) 0.049(4) -0.007(3) -0.017(4) -0.019(3) C21 0.072(5) 0.044(4) 0.059(5) -0.001(3) -0.022(4) -0.023(4) C22 0.079(6) 0.053(4) 0.049(4) -0.009(3) -0.011(4) -0.022(4) C23 0.070(5) 0.053(4) 0.048(4) 0.000(3) -0.018(4) -0.028(4) C24 0.074(5) 0.040(4) 0.039(4) -0.002(3) -0.023(4) -0.021(4) C25 0.089(6) 0.061(5) 0.045(4) -0.009(4) -0.023(4) -0.012(5) C26 0.096(7) 0.070(5) 0.051(5) -0.016(4) -0.033(4) -0.015(5) C27 0.102(8) 0.071(6) 0.063(6) -0.001(5) -0.017(5) -0.008(6) C28 0.068(6) 0.086(7) 0.105(8) -0.019(6) -0.030(6) 0.001(6) C29 0.063(6) 0.071(6) 0.149(11) 0.000(7) -0.038(7) -0.024(5) C30 0.069(9) 0.081(11) 0.110(12) -0.001(9) -0.032(8) -0.040(8) C31 0.068(9) 0.071(9) 0.069(9) 0.001(7) 0.001(7) -0.034(7) C30' 0.059(11) 0.084(12) 0.069(12) 0.003(8) -0.015(8) -0.023(9) C31' 0.061(10) 0.050(10) 0.055(10) -0.011(7) -0.005(8) -0.020(8) C32 0.069(6) 0.131(8) 0.113(7) 0.036(6) -0.018(5) -0.038(6) C33 0.124(8) 0.064(5) 0.054(5) -0.002(4) -0.013(5) -0.063(6) C34 0.090(6) 0.040(4) 0.045(4) 0.002(3) -0.006(4) -0.032(4) C35 0.068(5) 0.044(4) 0.035(3) -0.001(3) -0.005(3) -0.032(4) C36 0.077(5) 0.051(4) 0.037(4) -0.010(3) 0.002(3) -0.040(4) C37 0.093(7) 0.073(6) 0.047(4) 0.014(4) -0.018(4) -0.032(5) C38 0.104(8) 0.121(9) 0.052(5) -0.013(5) -0.023(5) -0.040(7) C39 0.092(8) 0.134(10) 0.124(10) -0.016(8) -0.059(8) -0.041(8) C40 0.075(7) 0.158(11) 0.077(7) -0.031(7) -0.013(6) -0.050(7) C41 0.068(7) 0.092(8) 0.108(9) -0.006(7) -0.006(6) -0.015(6) C42 0.102(7) 0.158(9) 0.112(8) 0.004(7) 0.003(6) -0.028(7) C43 0.087(8) 0.063(6) 0.093(8) -0.025(6) 0.008(6) -0.046(6) C43' 0.025(13) 0.023(12) 0.017(12) -0.001(8) -0.007(8) -0.008(9) C44 0.107(8) 0.057(5) 0.053(5) 0.001(4) 0.004(5) -0.045(5) C45 0.074(5) 0.035(3) 0.040(4) -0.006(3) -0.007(3) -0.023(4) C46 0.084(6) 0.055(5) 0.046(4) -0.005(3) 0.002(4) -0.026(5) C47 0.091(7) 0.061(5) 0.038(4) 0.003(3) -0.006(4) -0.030(5) C48 0.062(5) 0.042(4) 0.056(4) 0.000(3) -0.018(4) -0.024(4) C49 0.079(5) 0.038(3) 0.046(4) -0.004(3) -0.008(4) -0.031(4) C50 0.065(5) 0.029(3) 0.040(3) -0.003(3) -0.004(3) -0.021(3) C51 0.080(6) 0.048(4) 0.044(4) -0.002(3) -0.013(4) -0.031(4) C52 0.084(6) 0.063(5) 0.040(4) -0.004(3) -0.002(4) -0.036(5) C53 0.080(6) 0.041(4) 0.039(4) -0.008(3) -0.005(3) -0.032(4) C54 0.073(5) 0.044(4) 0.042(4) -0.001(3) -0.011(3) -0.030(4) C55 0.060(5) 0.046(4) 0.047(4) -0.009(3) -0.006(3) -0.020(4) C56 0.089(6) 0.054(4) 0.044(4) 0.005(3) -0.010(4) -0.035(5) C57 0.082(6) 0.048(4) 0.038(4) 0.003(3) -0.002(4) -0.020(4) C58 0.069(5) 0.040(4) 0.039(4) 0.003(3) -0.005(3) -0.023(4) C59 0.094(7) 0.064(5) 0.043(4) 0.016(4) -0.024(4) -0.026(5) C60 0.098(7) 0.040(4) 0.048(4) 0.010(3) -0.025(4) -0.021(4) C61 0.065(5) 0.043(4) 0.084(6) -0.005(4) -0.036(5) -0.006(4) C62 0.067(6) 0.080(7) 0.134(10) -0.047(7) -0.006(6) -0.017(5) C63 0.064(5) 0.097(6) 0.084(6) -0.019(5) 0.004(4) -0.037(5) C64 0.124(7) 0.069(5) 0.073(5) -0.022(4) 0.012(5) -0.046(5) C65 0.129(9) 0.153(11) 0.041(5) -0.007(6) -0.008(5) -0.098(9) C66 0.057(9) 0.088(12) 0.038(7) -0.011(7) 0.003(6) -0.034(9) O23 0.055(7) 0.065(7) 0.033(5) 0.005(4) -0.009(5) -0.031(6) C67 0.050(11) 0.051(9) 0.038(8) 0.009(6) -0.008(7) -0.022(8) C68 0.034(10) 0.049(9) 0.034(8) 0.006(6) 0.005(8) -0.022(9) C66' 0.092(10) 0.090(10) 0.089(10) -0.006(8) -0.009(8) -0.026(8) O23' 0.049(7) 0.056(7) 0.032(5) 0.014(4) 0.007(4) 0.016(5) C67' 0.050(10) 0.052(9) 0.053(8) 0.009(7) -0.017(8) -0.020(8) C68' 0.042(10) 0.033(7) 0.035(8) 0.001(6) -0.006(8) -0.011(7) O1P 0.057(3) 0.049(3) 0.070(3) 0.013(2) -0.021(3) -0.018(3) O2P 0.071(4) 0.072(4) 0.076(4) 0.028(3) -0.034(3) -0.036(3) O3P 0.068(4) 0.113(5) 0.062(3) 0.032(3) -0.017(3) -0.053(4) O4P 0.068(3) 0.050(3) 0.052(3) 0.015(2) -0.022(2) -0.027(3) O5P 0.051(3) 0.079(4) 0.083(4) 0.024(3) -0.018(3) -0.024(3) O6P 0.101(6) 0.083(5) 0.141(7) -0.002(4) 0.040(5) -0.051(4) O7P 0.095(5) 0.072(5) 0.223(9) 0.055(5) -0.015(6) -0.035(4) N1 0.052(4) 0.050(3) 0.050(3) 0.006(3) -0.012(3) -0.022(3) N2 0.056(4) 0.037(3) 0.048(3) 0.006(2) -0.014(3) -0.019(3) N3 0.062(4) 0.053(4) 0.059(4) 0.021(3) -0.012(3) -0.026(3) C1P 0.050(4) 0.042(4) 0.043(4) 0.003(3) -0.012(3) -0.022(3) C2P 0.051(4) 0.035(3) 0.042(3) 0.001(3) -0.008(3) -0.020(3) C3P 0.057(4) 0.030(3) 0.034(3) 0.002(2) -0.001(3) -0.016(3) C4P 0.053(4) 0.039(3) 0.035(3) 0.003(3) -0.010(3) -0.019(3) C5P 0.052(4) 0.041(3) 0.033(3) -0.002(3) -0.003(3) -0.015(3) C6P 0.051(4) 0.031(3) 0.039(3) 0.005(3) 0.001(3) -0.015(3) C1S 0.107(9) 0.114(9) 0.079(7) -0.027(6) -0.030(6) -0.030(8) C2S 0.095(8) 0.109(9) 0.084(7) -0.006(6) -0.017(6) -0.049(8) C3S 0.174(15) 0.091(9) 0.072(7) -0.003(6) -0.013(8) -0.020(10) C4S 0.101(12) 0.180(18) 0.100(10) -0.016(11) 0.025(9) 0.031(12) C5S 0.090(11) 0.25(3) 0.20(2) 0.007(19) 0.028(11) -0.072(16) C6S 0.197(18) 0.195(18) 0.116(11) -0.009(11) -0.037(12) -0.144(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 Cs1 O14 3.195(5) . ? Cs1 O17 3.205(5) . ? Cs1 O3 3.217(7) . ? Cs1 O4 3.228(12) . ? Cs1 O1 3.245(5) . ? Cs1 O15 3.249(5) . ? Cs1 O2 3.255(11) . ? Cs1 O5 3.318(5) . ? Cs1 O18 3.342(5) . ? Cs1 O16 3.357(17) . ? Cs1 O6 3.357(5) . ? Cs1 O16' 3.39(3) . ? Cs2 O20 3.154(5) . ? Cs2 O8 3.221(5) . ? Cs2 O22 3.241(6) . ? Cs2 O9 3.243(7) . ? Cs2 O7 3.252(5) . ? Cs2 O23 3.256(11) . ? Cs2 O12 3.280(5) . ? Cs2 O19 3.310(5) . ? Cs2 O10 3.313(6) . ? Cs2 O24 3.317(5) . ? Cs2 O21 3.327(6) . ? Cs2 O11 3.379(5) . ? O1 C16 1.391(9) . ? O1 C1 1.445(7) . ? O3 C5 1.305(14) . ? O3 C4 1.337(11) . ? O5 C9 1.407(9) . ? O5 C8 1.422(9) . ? O6 C11 1.375(8) . ? O6 C10 1.425(7) . ? O7 C24 1.377(9) . ? O7 C25 1.435(8) . ? O8 C26 1.404(9) . ? O8 C27 1.451(11) . ? O9 C28 1.377(11) . ? O9 C29 1.387(12) . ? O10 C31' 1.31(2) . ? O10 C30 1.368(14) . ? O10 C31 1.490(14) . ? O10 C30' 1.53(3) . ? O11 C32 1.417(11) . ? O11 C33 1.437(10) . ? O12 C19 1.386(9) . ? O12 C34 1.406(8) . ? O13 C50 1.372(8) . ? O13 C35 1.421(7) . ? O14 C36 1.394(8) . ? O14 C37 1.439(9) . ? O15 C38 1.383(11) . ? O15 C39 1.432(12) . ? O16 C40 1.386(16) . ? O16 C41 1.39(2) . ? O16' C41 1.37(3) . ? O16' C40 1.43(2) . ? O17 C43' 1.35(3) . ? O17 C42 1.366(13) . ? O17 C43 1.413(11) . ? O18 C45 1.339(9) . ? O18 C44 1.415(9) . ? O19 C58 1.349(9) . ? O19 C59 1.442(8) . ? O20 C60 1.399(10) . ? O20 C61 1.422(9) . ? O21 C63 1.412(11) . ? O21 C62 1.452(12) . ? O22 C64 1.353(11) . ? O22 C65 1.448(12) . ? O24 C53 1.371(8) . ? O24 C68' 1.44(3) . ? O24 C68 1.50(3) . ? C1 C2' 1.408(18) . ? C1 C2 1.459(11) . ? C2 O2 1.417(13) . ? O2 C3 1.382(13) . ? C3 C4 1.384(15) . ? O4 C7 1.225(15) . ? O4 C6 1.43(2) . ? C2' O2' 1.351(16) . ? O2' C3' 1.336(14) . ? C3' C4 1.358(15) . ? O4' C6 1.29(2) . ? O4' C7 1.81(2) . ? C5 C6 1.40(2) . ? C7 C8 1.383(15) . ? C9 C10 1.476(11) . ? C11 C12 1.379(9) . ? C11 C16 1.402(9) . ? C12 C13 1.380(10) . ? C13 C14 1.388(9) . ? C14 C15 1.393(10) . ? C14 C17 1.464(10) . ? C15 C16 1.366(10) . ? C17 C18 1.346(10) . ? C18 C21 1.443(11) . ? C19 C20 1.368(10) . ? C19 C24 1.407(9) . ? C20 C21 1.385(11) . ? C21 C22 1.398(10) . ? C22 C23 1.394(11) . ? C23 C24 1.376(10) . ? C25 C26 1.478(12) . ? C27 C28 1.506(14) . ? C29 C30' 1.40(3) . ? C29 C30 1.444(17) . ? C31 C32 1.275(16) . ? C31' C32 1.52(3) . ? C33 C34 1.468(12) . ? C35 C36 1.507(10) . ? C37 C38 1.464(13) . ? C39 C40 1.415(14) . ? C41 C42 1.395(15) . ? C43 C44 1.457(14) . ? C43' C44 1.58(3) . ? C45 C46 1.394(10) . ? C45 C50 1.396(9) . ? C46 C47 1.361(11) . ? C47 C48 1.392(10) . ? C48 C49 1.406(9) . ? C48 C51 1.505(11) . ? C49 C50 1.396(10) . ? C51 C52 1.352(10) . ? C52 C55 1.439(11) . ? C53 C54 1.379(10) . ? C53 C58 1.407(10) . ? C54 C55 1.409(10) . ? C55 C56 1.360(10) . ? C56 C57 1.391(11) . ? C57 C58 1.372(10) . ? C59 C60 1.512(11) . ? C61 C62 1.523(13) . ? C63 C64 1.454(13) . ? C65 C66' 1.20(2) . ? C65 C66 1.477(19) . ? C66 O23 1.397(17) . ? O23 C67 1.393(19) . ? C67 C68 1.54(3) . ? C66' O23' 1.41(2) . ? O23' C67' 1.39(2) . ? C67' C68' 1.38(3) . ? O1P C1P 1.245(7) . ? O2P N1 1.231(6) . ? O3P N1 1.221(6) . ? O4P N2 1.228(7) . ? O5P N2 1.237(7) . ? O6P N3 1.192(8) . ? O7P N3 1.220(9) . ? N1 C2P 1.449(8) . ? N2 C4P 1.439(7) . ? N3 C6P 1.451(7) . ? C1P C6P 1.450(9) . ? C1P C2P 1.460(8) . ? C2P C3P 1.356(9) . ? C3P C4P 1.388(9) . ? C4P C5P 1.395(8) . ? C5P C6P 1.372(9) . ? C1S C2S 1.302(15) . ? C1S C6S 1.376(19) . ? C2S C3S 1.309(16) . ? C3S C4S 1.36(2) . ? C4S C5S 1.33(3) . ? C5S C6S 1.33(2) . ? O8P C7P 1.300(17) . ? O9P N4 1.258(15) . ? O10P N4 1.223(14) . ? O11P N5 1.211(12) . ? O12P N5 1.270(13) . ? O13P N6 1.288(14) . ? O14P N6 1.247(14) . ? N4 C8P 1.385(13) . ? N5 C10P 1.470(13) . ? N6 C12P 1.448(13) . ? C7P C8P 1.3900 . ? C7P C12P 1.3900 . ? C8P C9P 1.3900 . ? C9P C10P 1.3900 . ? C10P C11P 1.3900 . ? C11P C12P 1.3900 . ? O15P C13P 1.298(13) . ? O16P N7 1.256(13) . ? O17P N7 1.265(13) . ? O18P N8 1.284(14) . ? O19P N8 1.246(15) . ? O20P N9 1.204(12) . ? O21P N9 1.207(12) . ? N7 C14P 1.452(12) . ? N8 C16P 1.474(13) . ? N9 C18P 1.426(11) . ? C13P C14P 1.3900 . ? C13P C18P 1.3900 . ? C14P C15P 1.3900 . ? C15P C16P 1.3900 . ? C16P C17P 1.3900 . ? C17P C18P 1.3900 . ? C7S C8S 1.3900 . ? C7S C12S 1.3900 . ? C8S C9S 1.3900 . ? C9S C10S 1.3900 . ? C10S C11S 1.3900 . ? C11S C12S 1.3900 . ? C13S C14S 1.3900 . ? C13S C18S 1.3900 . ? C14S C15S 1.3900 . ? C15S C16S 1.3900 . ? C16S C17S 1.3900 . ? C17S C18S 1.3900 . ? 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 O14 Cs1 O17 128.59(13) . . ? O14 Cs1 O3 163.0(2) . . ? O17 Cs1 O3 65.2(2) . . ? O14 Cs1 O4 110.8(2) . . ? O17 Cs1 O4 93.8(2) . . ? O3 Cs1 O4 54.4(3) . . ? O14 Cs1 O1 88.33(12) . . ? O17 Cs1 O1 114.20(13) . . ? O3 Cs1 O1 94.18(17) . . ? O4 Cs1 O1 124.6(3) . . ? O14 Cs1 O15 53.30(14) . . ? O17 Cs1 O15 95.96(15) . . ? O3 Cs1 O15 121.10(18) . . ? O4 Cs1 O15 73.6(3) . . ? O1 Cs1 O15 141.39(13) . . ? O14 Cs1 O2 137.1(2) . . ? O17 Cs1 O2 67.8(2) . . ? O3 Cs1 O2 53.2(2) . . ? O4 Cs1 O2 106.3(3) . . ? O1 Cs1 O2 52.27(19) . . ? O15 Cs1 O2 163.8(2) . . ? O14 Cs1 O5 70.92(12) . . ? O17 Cs1 O5 146.15(14) . . ? O3 Cs1 O5 92.2(2) . . ? O4 Cs1 O5 52.5(2) . . ? O1 Cs1 O5 91.24(12) . . ? O15 Cs1 O5 73.61(14) . . ? O2 Cs1 O5 119.7(3) . . ? O14 Cs1 O18 91.47(12) . . ? O17 Cs1 O18 52.26(14) . . ? O3 Cs1 O18 105.52(19) . . ? O4 Cs1 O18 145.8(2) . . ? O1 Cs1 O18 79.85(12) . . ? O15 Cs1 O18 102.78(14) . . ? O2 Cs1 O18 67.8(3) . . ? O5 Cs1 O18 160.60(13) . . ? O14 Cs1 O16 104.7(3) . . ? O17 Cs1 O16 52.9(4) . . ? O3 Cs1 O16 75.1(4) . . ? O4 Cs1 O16 56.5(6) . . ? O1 Cs1 O16 165.7(2) . . ? O15 Cs1 O16 52.4(2) . . ? O2 Cs1 O16 113.4(3) . . ? O5 Cs1 O16 98.5(5) . . ? O18 Cs1 O16 93.7(6) . . ? O14 Cs1 O6 60.05(12) . . ? O17 Cs1 O6 160.37(14) . . ? O3 Cs1 O6 110.6(2) . . ? O4 Cs1 O6 98.7(3) . . ? O1 Cs1 O6 46.18(11) . . ? O15 Cs1 O6 102.02(13) . . ? O2 Cs1 O6 94.1(2) . . ? O5 Cs1 O6 49.35(12) . . ? O18 Cs1 O6 115.05(13) . . ? O16 Cs1 O6 146.4(4) . . ? O14 Cs1 O16' 96.7(9) . . ? O17 Cs1 O16' 49.1(4) . . ? O3 Cs1 O16' 86.4(11) . . ? O4 Cs1 O16' 70.7(11) . . ? O1 Cs1 O16' 160.9(6) . . ? O15 Cs1 O16' 48.5(6) . . ? O2 Cs1 O16' 115.6(5) . . ? O5 Cs1 O16' 107.9(6) . . ? O18 Cs1 O16' 81.5(8) . . ? O16 Cs1 O16' 14.8(6) . . ? O6 Cs1 O16' 150.1(4) . . ? O20 Cs2 O8 63.51(14) . . ? O20 Cs2 O22 98.79(18) . . ? O8 Cs2 O22 152.29(18) . . ? O20 Cs2 O9 77.08(16) . . ? O8 Cs2 O9 53.03(16) . . ? O22 Cs2 O9 104.14(17) . . ? O20 Cs2 O7 104.05(13) . . ? O8 Cs2 O7 51.46(13) . . ? O22 Cs2 O7 155.06(18) . . ? O9 Cs2 O7 90.75(15) . . ? O20 Cs2 O23 124.6(2) . . ? O8 Cs2 O23 153.5(2) . . ? O22 Cs2 O23 54.0(2) . . ? O9 Cs2 O23 148.3(2) . . ? O7 Cs2 O23 103.7(2) . . ? O20 Cs2 O12 147.31(14) . . ? O8 Cs2 O12 96.24(13) . . ? O22 Cs2 O12 108.29(18) . . ? O9 Cs2 O12 112.36(15) . . ? O7 Cs2 O12 46.90(12) . . ? O23 Cs2 O12 63.5(2) . . ? O20 Cs2 O19 52.56(14) . . ? O8 Cs2 O19 72.62(14) . . ? O22 Cs2 O19 114.89(15) . . ? O9 Cs2 O19 118.65(15) . . ? O7 Cs2 O19 73.01(12) . . ? O23 Cs2 O19 92.7(2) . . ? O12 Cs2 O19 98.34(13) . . ? O20 Cs2 O10 112.27(15) . . ? O8 Cs2 O10 103.19(16) . . ? O22 Cs2 O10 62.14(15) . . ? O9 Cs2 O10 52.10(16) . . ? O7 Cs2 O10 116.40(13) . . ? O23 Cs2 O10 96.3(2) . . ? O12 Cs2 O10 96.70(14) . . ? O19 Cs2 O10 164.74(13) . . ? O20 Cs2 O24 93.05(13) . . ? O8 Cs2 O24 109.61(14) . . ? O22 Cs2 O24 91.58(14) . . ? O9 Cs2 O24 162.45(14) . . ? O7 Cs2 O24 77.45(12) . . ? O23 Cs2 O24 48.8(2) . . ? O12 Cs2 O24 68.75(12) . . ? O19 Cs2 O24 45.62(11) . . ? O10 Cs2 O24 145.15(13) . . ? O20 Cs2 O21 51.21(15) . . ? O8 Cs2 O21 104.26(15) . . ? O22 Cs2 O21 50.62(19) . . ? O9 Cs2 O21 77.33(17) . . ? O7 Cs2 O21 154.15(15) . . ? O23 Cs2 O21 98.2(2) . . ? O12 Cs2 O21 158.91(15) . . ? O19 Cs2 O21 92.50(15) . . ? O10 Cs2 O21 74.08(15) . . ? O24 Cs2 O21 107.93(15) . . ? O20 Cs2 O11 162.07(16) . . ? O8 Cs2 O11 123.76(15) . . ? O22 Cs2 O11 67.57(19) . . ? O9 Cs2 O11 94.54(15) . . ? O7 Cs2 O11 91.74(14) . . ? O23 Cs2 O11 57.6(2) . . ? O12 Cs2 O11 50.57(14) . . ? O19 Cs2 O11 142.90(13) . . ? O10 Cs2 O11 51.68(14) . . ? O24 Cs2 O11 98.72(12) . . ? O21 Cs2 O11 111.79(16) . . ? C16 O1 C1 116.0(5) . . ? C16 O1 Cs1 114.7(4) . . ? C1 O1 Cs1 115.6(4) . . ? C5 O3 C4 116.9(10) . . ? C5 O3 Cs1 125.2(8) . . ? C4 O3 Cs1 117.7(8) . . ? C9 O5 C8 111.3(6) . . ? C9 O5 Cs1 123.9(4) . . ? C8 O5 Cs1 118.1(5) . . ? C11 O6 C10 117.0(5) . . ? C11 O6 Cs1 110.6(3) . . ? C10 O6 Cs1 116.1(4) . . ? C24 O7 C25 117.4(6) . . ? C24 O7 Cs2 115.5(4) . . ? C25 O7 Cs2 118.6(4) . . ? C26 O8 C27 115.1(7) . . ? C26 O8 Cs2 115.9(4) . . ? C27 O8 Cs2 109.9(5) . . ? C28 O9 C29 116.2(8) . . ? C28 O9 Cs2 122.1(6) . . ? C29 O9 Cs2 118.2(6) . . ? C31' O10 C30 70.6(13) . . ? C31' O10 C31 42.7(11) . . ? C30 O10 C31 112.4(9) . . ? C31' O10 C30' 108.2(17) . . ? C30 O10 C30' 50.6(13) . . ? C31 O10 C30' 132.2(12) . . ? C31' O10 Cs2 118.7(11) . . ? C30 O10 Cs2 109.7(7) . . ? C31 O10 Cs2 110.4(6) . . ? C30' O10 Cs2 117.4(11) . . ? C32 O11 C33 108.2(8) . . ? C32 O11 Cs2 118.6(5) . . ? C33 O11 Cs2 115.6(4) . . ? C19 O12 C34 116.4(6) . . ? C19 O12 Cs2 115.7(4) . . ? C34 O12 Cs2 120.8(4) . . ? C50 O13 C35 117.0(5) . . ? C50 O13 Cs1 115.2(3) . . ? C35 O13 Cs1 115.8(4) . . ? C36 O14 C37 115.1(6) . . ? C36 O14 Cs1 125.3(4) . . ? C37 O14 Cs1 107.4(4) . . ? C38 O15 C39 114.4(7) . . ? C38 O15 Cs1 118.2(5) . . ? C39 O15 Cs1 120.0(6) . . ? C40 O16 C41 114.2(12) . . ? C40 O16 Cs1 115.0(9) . . ? C41 O16 Cs1 115.5(14) . . ? C41 O16' C40 112(3) . . ? C41 O16' Cs1 114(3) . . ? C40 O16' Cs1 111.5(18) . . ? C43' O17 C42 124.6(16) . . ? C43' O17 C43 57.2(14) . . ? C42 O17 C43 106.4(9) . . ? C43' O17 Cs1 117.3(15) . . ? C42 O17 Cs1 116.8(7) . . ? C43 O17 Cs1 116.4(5) . . ? C45 O18 C44 118.1(6) . . ? C45 O18 Cs1 119.6(4) . . ? C44 O18 Cs1 114.7(4) . . ? C58 O19 C59 117.8(6) . . ? C58 O19 Cs2 116.1(4) . . ? C59 O19 Cs2 109.1(5) . . ? C60 O20 C61 111.6(6) . . ? C60 O20 Cs2 123.8(4) . . ? C61 O20 Cs2 121.2(5) . . ? C63 O21 C62 112.1(8) . . ? C63 O21 Cs2 105.6(5) . . ? C62 O21 Cs2 95.8(5) . . ? C64 O22 C65 118.8(8) . . ? C64 O22 Cs2 119.7(6) . . ? C65 O22 Cs2 118.5(6) . . ? C53 O24 C68' 124.8(10) . . ? C53 O24 C68 109.0(9) . . ? C68' O24 C68 18.8(9) . . ? C53 O24 Cs2 116.5(4) . . ? C68' O24 Cs2 106.9(8) . . ? C68 O24 Cs2 125.7(7) . . ? C2' C1 O1 108.6(18) . . ? C2' C1 C2 35.2(16) . . ? O1 C1 C2 108.8(7) . . ? O2 C2 C1 112.5(9) . . ? C3 O2 C2 124.4(13) . . ? C3 O2 Cs1 110.3(10) . . ? C2 O2 Cs1 118.1(7) . . ? O2 C3 C4 118.8(14) . . ? C7 O4 C6 127.0(16) . . ? C7 O4 Cs1 110.8(9) . . ? C6 O4 Cs1 111.5(9) . . ? O2' C2' C1 116(2) . . ? O2' C2' Cs1 68(2) . . ? C1 C2' Cs1 95(2) . . ? C3' O2' C2' 129(2) . . ? C3' O2' Cs1 117.3(14) . . ? C2' O2' Cs1 90(2) . . ? O2' C3' C4 117.0(16) . . ? C6 O4' C7 99.1(13) . . ? C6 O4' Cs1 105.0(12) . . ? C7 O4' Cs1 88.1(7) . . ? O3 C4 C3' 128.6(13) . . ? O3 C4 C3 122.0(14) . . ? C3' C4 C3 38.8(11) . . ? O3 C5 C6 114.7(13) . . ? O4' C6 C5 101.2(17) . . ? O4' C6 O4 54.5(10) . . ? C5 C6 O4 134.1(16) . . ? O4 C7 C8 134.5(15) . . ? O4 C7 O4' 43.9(9) . . ? C8 C7 O4' 97.2(11) . . ? O4 C7 Cs1 51.8(7) . . ? C8 C7 Cs1 94.5(7) . . ? O4' C7 Cs1 63.8(6) . . ? C7 C8 O5 108.8(8) . . ? O5 C9 C10 109.8(6) . . ? O6 C10 C9 109.4(6) . . ? O6 C11 C12 124.7(6) . . ? O6 C11 C16 116.0(6) . . ? C12 C11 C16 119.4(7) . . ? C11 C12 C13 119.8(6) . . ? C12 C13 C14 121.6(7) . . ? C13 C14 C15 117.8(7) . . ? C13 C14 C17 120.4(7) . . ? C15 C14 C17 121.7(7) . . ? C16 C15 C14 121.4(7) . . ? C15 C16 O1 125.0(6) . . ? C15 C16 C11 120.0(7) . . ? O1 C16 C11 114.9(6) . . ? C18 C17 C14 125.9(7) . . ? C17 C18 C21 129.5(8) . . ? C20 C19 O12 124.9(6) . . ? C20 C19 C24 121.0(7) . . ? O12 C19 C24 114.2(6) . . ? C19 C20 C21 120.3(7) . . ? C20 C21 C22 118.9(7) . . ? C20 C21 C18 122.3(7) . . ? C22 C21 C18 118.7(8) . . ? C23 C22 C21 120.9(8) . . ? C24 C23 C22 119.7(7) . . ? C23 C24 O7 123.7(6) . . ? C23 C24 C19 119.2(7) . . ? O7 C24 C19 117.0(7) . . ? O7 C25 C26 108.5(7) . . ? O8 C26 C25 107.8(7) . . ? O8 C27 C28 113.8(8) . . ? O9 C28 C27 110.6(8) . . ? O9 C29 C30' 123.1(14) . . ? O9 C29 C30 117.9(9) . . ? C30' C29 C30 51.9(14) . . ? O10 C30 C29 112.1(11) . . ? C32 C31 O10 122.1(12) . . ? C29 C30' O10 105(2) . . ? O10 C31' C32 117.3(19) . . ? C31 C32 O11 112.9(11) . . ? C31 C32 C31' 42.1(10) . . ? O11 C32 C31' 117.2(12) . . ? O11 C33 C34 112.8(6) . . ? O12 C34 C33 107.7(7) . . ? O13 C35 C36 106.6(6) . . ? O14 C36 C35 111.8(5) . . ? O14 C37 C38 111.8(7) . . ? O14 C37 Cs1 51.9(3) . . ? C38 C37 Cs1 87.7(5) . . ? O15 C38 C37 111.0(7) . . ? C40 C39 O15 112.2(9) . . ? O16 C40 C39 124.4(15) . . ? O16 C40 O16' 35.8(16) . . ? C39 C40 O16' 98(2) . . ? O16' C41 O16 36.7(17) . . ? O16' C41 C42 117.6(13) . . ? O16 C41 C42 117.7(12) . . ? O17 C42 C41 121.4(11) . . ? O17 C43 C44 110.2(8) . . ? O17 C43' C44 106(2) . . ? O18 C44 C43 112.3(7) . . ? O18 C44 C43' 120.1(13) . . ? C43 C44 C43' 51.4(13) . . ? O18 C45 C46 125.2(7) . . ? O18 C45 C50 116.4(6) . . ? C46 C45 C50 118.4(7) . . ? C47 C46 C45 121.7(7) . . ? C46 C47 C48 121.2(7) . . ? C47 C48 C49 117.8(7) . . ? C47 C48 C51 123.9(7) . . ? C49 C48 C51 118.3(7) . . ? C50 C49 C48 121.0(7) . . ? O13 C50 C49 124.9(6) . . ? O13 C50 C45 115.3(6) . . ? C49 C50 C45 119.8(6) . . ? C52 C51 C48 126.5(7) . . ? C51 C52 C55 127.9(7) . . ? O24 C53 C54 124.4(6) . . ? O24 C53 C58 114.8(7) . . ? C54 C53 C58 120.8(6) . . ? C53 C54 C55 119.5(7) . . ? C56 C55 C54 118.9(7) . . ? C56 C55 C52 119.6(7) . . ? C54 C55 C52 121.5(7) . . ? C55 C56 C57 122.1(7) . . ? C58 C57 C56 119.6(7) . . ? O19 C58 C57 125.1(7) . . ? O19 C58 C53 115.8(6) . . ? C57 C58 C53 119.1(7) . . ? O19 C59 C60 109.7(6) . . ? O20 C60 C59 112.3(6) . . ? O20 C61 C62 108.2(7) . . ? O21 C62 C61 105.5(7) . . ? O21 C62 Cs2 61.6(4) . . ? C61 C62 Cs2 90.7(5) . . ? O21 C63 C64 107.1(8) . . ? O22 C64 C63 115.9(8) . . ? C66' C65 O22 120.1(14) . . ? C66' C65 C66 82.7(15) . . ? O22 C65 C66 112.8(9) . . ? O23 C66 C65 115.6(13) . . ? C67 O23 C66 115.4(12) . . ? C67 O23 Cs2 122.4(9) . . ? C66 O23 Cs2 109.3(9) . . ? O23 C67 C68 111.2(15) . . ? O24 C68 C67 101.7(14) . . ? C65 C66' O23' 111.3(19) . . ? C67' O23' C66' 118.1(15) . . ? C67' O23' Cs2 79.5(11) . . ? C66' O23' Cs2 114.9(11) . . ? C68' C67' O23' 110.5(19) . . ? C68' C67' Cs2 90.2(14) . . ? O23' C67' Cs2 79.1(10) . . ? C67' C68' O24 117.6(19) . . ? O3P N1 O2P 122.9(6) . . ? O3P N1 C2P 119.1(5) . . ? O2P N1 C2P 117.9(5) . . ? O4P N2 O5P 123.1(6) . . ? O4P N2 C4P 118.7(6) . . ? O5P N2 C4P 118.2(5) . . ? O6P N3 O7P 120.7(7) . . ? O6P N3 C6P 121.1(7) . . ? O7P N3 C6P 118.0(7) . . ? O1P C1P C6P 125.1(6) . . ? O1P C1P C2P 123.9(6) . . ? C6P C1P C2P 110.9(5) . . ? C3P C2P N1 117.2(5) . . ? C3P C2P C1P 124.5(6) . . ? N1 C2P C1P 118.3(5) . . ? C2P C3P C4P 119.4(6) . . ? C3P C4P C5P 121.6(6) . . ? C3P C4P N2 119.7(5) . . ? C5P C4P N2 118.7(6) . . ? C6P C5P C4P 117.6(6) . . ? C5P C6P C1P 125.7(6) . . ? C5P C6P N3 115.6(6) . . ? C1P C6P N3 118.7(6) . . ? C2S C1S C6S 118.8(14) . . ? C1S C2S C3S 121.4(13) . . ? C2S C3S C4S 119.2(15) . . ? C5S C4S C3S 121.6(16) . . ? C6S C5S C4S 117.2(17) . . ? C5S C6S C1S 121.2(16) . . ? O10P N4 O9P 123(2) . . ? O10P N4 C8P 112.7(16) . . ? O9P N4 C8P 109.9(15) . . ? O11P N5 O12P 122.3(16) . . ? O11P N5 C10P 121.3(14) . . ? O12P N5 C10P 115.5(15) . . ? O14P N6 O13P 120.7(19) . . ? O14P N6 C12P 107(2) . . ? O13P N6 C12P 130(3) . . ? O8P C7P C8P 121.5(8) . . ? O8P C7P C12P 118.0(8) . . ? C8P C7P C12P 120.0 . . ? N4 C8P C7P 133.3(11) . . ? N4 C8P C9P 106.7(11) . . ? C7P C8P C9P 120.0 . . ? C10P C9P C8P 120.0 . . ? C9P C10P C11P 120.0 . . ? C9P C10P N5 122.5(7) . . ? C11P C10P N5 117.5(7) . . ? C12P C11P C10P 120.0 . . ? C11P C12P C7P 120.0 . . ? C11P C12P N6 109.9(12) . . ? C7P C12P N6 130.1(13) . . ? O16P N7 O17P 121.3(15) . . ? O16P N7 C14P 115.9(12) . . ? O17P N7 C14P 121.2(17) . . ? O19P N8 O18P 118.4(18) . . ? O19P N8 C16P 115(2) . . ? O18P N8 C16P 118(2) . . ? O20P N9 O21P 126.0(15) . . ? O20P N9 C18P 114.1(11) . . ? O21P N9 C18P 115.5(12) . . ? O15P C13P C14P 119.6(10) . . ? O15P C13P C18P 120.4(10) . . ? C14P C13P C18P 120.0 . . ? C15P C14P C13P 120.0 . . ? C15P C14P N7 113.0(9) . . ? C13P C14P N7 125.5(9) . . ? C16P C15P C14P 120.0 . . ? C15P C16P C17P 120.0 . . ? C15P C16P N8 116.4(11) . . ? C17P C16P N8 123.6(11) . . ? C18P C17P C16P 120.0 . . ? C17P C18P C13P 120.0 . . ? C17P C18P N9 113.0(9) . . ? C13P C18P N9 127.0(9) . . ? C8S C7S C12S 120.0 . . ? C7S C8S C9S 120.0 . . ? C10S C9S C8S 120.0 . . ? C11S C10S C9S 120.0 . . ? C10S C11S C12S 120.0 . . ? C11S C12S C7S 120.0 . . ? C14S C13S C18S 120.0 . . ? C13S C14S C15S 120.0 . . ? C16S C15S C14S 120.0 . . ? C15S C16S C17S 120.0 . . ? C16S C17S C18S 120.0 . . ? C17S C18S C13S 120.0 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.093 _refine_diff_density_min -0.985 _refine_diff_density_rms 0.128 #===END data_4b+Ca _database_code_depnum_ccdc_archive 'CCDC 780040' #TrackingRef 'all-CIFs-revised.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H116 Ca2 Cl4 O45' _chemical_formula_weight 1995.67 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.4368(8) _cell_length_b 17.9290(11) _cell_length_c 18.9170(11) _cell_angle_alpha 78.740(3) _cell_angle_beta 84.002(3) _cell_angle_gamma 87.880(3) _cell_volume 4775.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120.0(2) _cell_measurement_reflns_used 1332 _cell_measurement_theta_min 2.562 _cell_measurement_theta_max 18.958 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 0.324 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8980 _exptl_absorpt_correction_T_max 0.9936 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120.0(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-6K' _diffrn_measurement_method /W _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46792 _diffrn_reflns_av_R_equivalents 0.2700 _diffrn_reflns_av_sigmaI/netI 0.5067 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 29.00 _reflns_number_total 25054 _reflns_number_gt 5685 _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 ; Perchlorate anion Cl(3)O4- is disordered over two positions with occupancies 0.77:0.23. Anions Cl(4)O4- and Cl(5)O4- have incomplete occupancies, 0.61 and 0.39, respectively. The occupancies of solvate water molecules, O(10W) and O(11W), are 0.31 and 0.19. Water molecule O(9W) has occupancy of 0.5 and disordered about symmetry center. The SADI commands were applied to constrain the disordered anions Cl(3)O4-, Cl(4)O4-, and Cl(5)O4-. The ISOR command was applied for the atoms of disordered perchlorate anions, for atoms O(1), C(5), C(10), C(18), C(24), C(31), C(38), and C(56) of cyclobutane molecule, for carbon atoms of two of three independent solvate benzene molecules, and for atoms O(8W), O(9W), and O(11W) of solvate water molecules. It was done in order to avoid N.P.D. for thermal anisotropic displacement parameters of the above-said atoms. 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^)+(0.0892P)^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 25054 _refine_ls_number_parameters 1254 _refine_ls_number_restraints 591 _refine_ls_R_factor_all 0.3780 _refine_ls_R_factor_gt 0.1145 _refine_ls_wR_factor_ref 0.2961 _refine_ls_wR_factor_gt 0.2320 _refine_ls_goodness_of_fit_ref 0.877 _refine_ls_restrained_S_all 0.909 _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 Cl1 Cl 0.70692(18) 0.35971(15) 0.14617(13) 0.0329(6) Uani 1 1 d . . . O11' O 0.6613(6) 0.4320(4) 0.1209(4) 0.056(2) Uani 1 1 d . . . O12' O 0.7497(5) 0.3300(4) 0.0855(3) 0.0423(19) Uani 1 1 d . . . O13' O 0.6372(5) 0.3058(5) 0.1873(4) 0.063(2) Uani 1 1 d . . . O14' O 0.7753(5) 0.3719(4) 0.1932(4) 0.049(2) Uani 1 1 d . . . Cl2 Cl 0.58557(18) 0.83784(15) 0.36860(17) 0.0427(7) Uani 1 1 d . . . O21 O 0.6267(5) 0.9108(4) 0.3627(4) 0.052(2) Uani 1 1 d . . . O22 O 0.4993(5) 0.8296(4) 0.4171(5) 0.064(3) Uani 1 1 d . . . O23 O 0.5669(5) 0.8278(4) 0.2971(4) 0.055(2) Uani 1 1 d . . . O24 O 0.6489(5) 0.7783(4) 0.3971(4) 0.047(2) Uani 1 1 d . . . Cl3 Cl 0.08587(19) 0.35948(17) 0.33896(16) 0.0484(8) Uani 1 1 d D . . O31 O -0.0049(4) 0.3464(4) 0.3745(4) 0.054(2) Uani 1 1 d D A . O32 O 0.0841(7) 0.3911(9) 0.2646(5) 0.057(4) Uani 0.77(3) 1 d PDU A 1 O33 O 0.1399(11) 0.2923(8) 0.3504(11) 0.128(8) Uani 0.77(3) 1 d PDU A 1 O34 O 0.1268(10) 0.4162(12) 0.3712(8) 0.099(6) Uani 0.77(3) 1 d PDU A 1 O35 O 0.1125(17) 0.2927(15) 0.309(2) 0.063(15) Uani 0.23(3) 1 d PDU A 2 O36 O 0.1495(13) 0.371(2) 0.3855(11) 0.032(11) Uani 0.23(3) 1 d PDU A 2 O37 O 0.0836(18) 0.4216(19) 0.2795(17) 0.13(3) Uani 0.23(3) 1 d PDU A 2 Cl4 Cl 0.7845(4) 0.7399(4) 0.1241(3) 0.078(2) Uani 0.612(3) 1 d PDU B -1 O41 O 0.8799(6) 0.7297(8) 0.1231(7) 0.084(5) Uani 0.612(3) 1 d PDU B -1 O42 O 0.7559(9) 0.8084(7) 0.0798(7) 0.097(6) Uani 0.612(3) 1 d PDU B -1 O43 O 0.7575(10) 0.6788(8) 0.0869(9) 0.132(8) Uani 0.612(3) 1 d PDU B -1 O44 O 0.7435(11) 0.7305(10) 0.1924(6) 0.156(9) Uani 0.612(3) 1 d PDU B -1 O10W O 0.545(2) 0.9823(17) 0.073(2) 0.086(10) Uani 0.3062(16) 1 d PU B -1 Cl5 Cl 0.4784(8) 1.0060(6) 0.0286(5) 0.086(3) Uani 0.388(3) 1 d PDU B -2 O51 O 0.3962(12) 1.0303(15) -0.0003(11) 0.080(8) Uani 0.388(3) 1 d PDU B -2 O52 O 0.5496(19) 1.0599(18) -0.0042(13) 0.143(15) Uani 0.388(3) 1 d PDU B -2 O53 O 0.513(2) 0.9374(11) 0.0060(12) 0.102(10) Uani 0.388(3) 1 d PDU B -2 O54 O 0.4737(15) 0.9987(11) 0.1035(8) 0.088(8) Uani 0.388(3) 1 d PDU B -2 O11W O 0.877(3) 0.541(2) 0.088(2) 0.073(13) Uani 0.1938(16) 1 d PU B -2 Ca1 Ca 0.45080(12) 0.48840(10) 0.30941(10) 0.0184(4) Uani 1 1 d . . . Ca2 Ca 0.12509(13) 0.88235(11) 0.85456(10) 0.0232(5) Uani 1 1 d . . . O1W O 0.3953(4) 0.5975(3) 0.2312(3) 0.0258(15) Uani 1 1 d . . . O2W O 0.4826(4) 0.4532(3) 0.1946(3) 0.0288(16) Uani 1 1 d . . . O3W O 0.2941(4) 0.4624(4) 0.3008(4) 0.0412(19) Uani 1 1 d . . . O4W O 0.0251(4) 0.9384(3) 0.7663(3) 0.0229(14) Uani 1 1 d . . . O5W O 0.0171(4) 0.9510(3) 0.9233(3) 0.0310(16) Uani 1 1 d . . . O6W O 0.1802(4) 1.0103(4) 0.8193(4) 0.0373(18) Uani 1 1 d . . . O1 O 0.3810(4) 0.4624(3) 0.4403(3) 0.0238(15) Uani 1 1 d U . . O2 O 0.4477(4) 0.3524(3) 0.3737(3) 0.0221(14) Uani 1 1 d . . . O3 O 0.6045(4) 0.4278(3) 0.3157(3) 0.0246(15) Uani 1 1 d . . . O4 O 0.5810(4) 0.5801(3) 0.2741(3) 0.0252(15) Uani 1 1 d . . . O5 O 0.4568(4) 0.5877(3) 0.3870(3) 0.0199(14) Uani 1 1 d . . . O6 O 0.2744(4) 0.8618(4) 0.7869(3) 0.0295(16) Uani 1 1 d . . . O7 O 0.2677(4) 0.8912(4) 0.9189(3) 0.0281(16) Uani 1 1 d . . . O8 O 0.1185(4) 0.8029(4) 0.9781(3) 0.0268(15) Uani 1 1 d . . . O9 O 0.0032(4) 0.7829(3) 0.8779(3) 0.0244(15) Uani 1 1 d . . . O10 O 0.1375(4) 0.7910(3) 0.7677(3) 0.0210(14) Uani 1 1 d . . . O11 O -0.0997(4) 0.9678(3) 0.6524(3) 0.0235(15) Uani 1 1 d . . . O12 O -0.1661(4) 0.9573(3) 0.7997(3) 0.0245(15) Uani 1 1 d . . . O13 O -0.0579(4) 1.0774(4) 0.8402(4) 0.0322(16) Uani 1 1 d . . . O14 O 0.0946(4) 1.1149(3) 0.7216(3) 0.0285(16) Uani 1 1 d . . . O15 O 0.0586(4) 1.0284(3) 0.6236(3) 0.0240(15) Uani 1 1 d . . . O16 O 0.2129(4) 0.6826(3) 0.2012(3) 0.0264(15) Uani 1 1 d . . . O17 O 0.2311(5) 0.5368(4) 0.1737(4) 0.0436(19) Uani 1 1 d . . . O18 O 0.4036(5) 0.5461(4) 0.0791(4) 0.0416(19) Uani 1 1 d . . . O19 O 0.5099(4) 0.6671(4) 0.1120(3) 0.0309(16) Uani 1 1 d . . . O20 O 0.3606(4) 0.7619(3) 0.1574(3) 0.0233(15) Uani 1 1 d . . . C1 C 0.1946(6) 0.7320(5) 0.4925(5) 0.021(2) Uani 1 1 d . . . H1A H 0.1416 0.7193 0.5311 0.026 Uiso 1 1 calc R . . C2 C 0.2459(6) 0.8020(5) 0.5072(4) 0.022(2) Uani 1 1 d . . . H2A H 0.3086 0.8056 0.4787 0.027 Uiso 1 1 calc R . . C3 C 0.1746(6) 0.8552(5) 0.4615(5) 0.023(2) Uani 1 1 d . . . H3A H 0.2068 0.8976 0.4263 0.028 Uiso 1 1 calc R . . C4 C 0.1562(6) 0.7880(5) 0.4251(4) 0.021(2) Uani 1 1 d . . . H4A H 0.0882 0.7813 0.4227 0.026 Uiso 1 1 calc R . . C5 C 0.2450(6) 0.6600(5) 0.4832(4) 0.0168(19) Uani 1 1 d U . . C6 C 0.2043(6) 0.5907(5) 0.5130(4) 0.022(2) Uani 1 1 d . . . H6A H 0.1469 0.5897 0.5427 0.027 Uiso 1 1 calc R . . C7 C 0.2461(6) 0.5217(5) 0.5001(4) 0.021(2) Uani 1 1 d . . . H7A H 0.2166 0.4746 0.5195 0.026 Uiso 1 1 calc R . . C8 C 0.3308(6) 0.5243(5) 0.4588(5) 0.024(2) Uani 1 1 d . . . C9 C 0.3728(6) 0.5934(5) 0.4300(4) 0.019(2) Uani 1 1 d . . . C10 C 0.3326(6) 0.6604(5) 0.4418(4) 0.018(2) Uani 1 1 d U . . H10A H 0.3632 0.7071 0.4223 0.022 Uiso 1 1 calc R . . C11 C 0.3492(6) 0.3874(5) 0.4690(5) 0.025(2) Uani 1 1 d . . . H11A H 0.2931 0.3773 0.4466 0.030 Uiso 1 1 calc R . . H11B H 0.3337 0.3802 0.5221 0.030 Uiso 1 1 calc R . . C12 C 0.4283(6) 0.3360(5) 0.4507(4) 0.024(2) Uani 1 1 d . . . H12A H 0.4837 0.3456 0.4741 0.029 Uiso 1 1 calc R . . H12B H 0.4109 0.2821 0.4677 0.029 Uiso 1 1 calc R . . C13 C 0.5284(6) 0.3106(5) 0.3507(5) 0.027(2) Uani 1 1 d . . . H13A H 0.5246 0.3038 0.3004 0.033 Uiso 1 1 calc R . . H13B H 0.5298 0.2595 0.3821 0.033 Uiso 1 1 calc R . . C14 C 0.6168(6) 0.3518(5) 0.3544(5) 0.029(2) Uani 1 1 d . . . H14A H 0.6268 0.3518 0.4054 0.035 Uiso 1 1 calc R . . H14B H 0.6712 0.3268 0.3317 0.035 Uiso 1 1 calc R . . C15 C 0.6862(6) 0.4746(5) 0.3065(5) 0.029(2) Uani 1 1 d . . . H15A H 0.7421 0.4466 0.2898 0.035 Uiso 1 1 calc R . . H15B H 0.6968 0.4891 0.3529 0.035 Uiso 1 1 calc R . . C16 C 0.6673(6) 0.5438(5) 0.2509(5) 0.031(2) Uani 1 1 d . . . H16A H 0.7193 0.5797 0.2449 0.037 Uiso 1 1 calc R . . H16B H 0.6624 0.5290 0.2037 0.037 Uiso 1 1 calc R . . C17 C 0.5942(6) 0.6340(5) 0.3196(5) 0.028(2) Uani 1 1 d . . . H17A H 0.6271 0.6791 0.2906 0.034 Uiso 1 1 calc R . . H17B H 0.6325 0.6106 0.3589 0.034 Uiso 1 1 calc R . . C18 C 0.5011(6) 0.6573(5) 0.3510(5) 0.023(2) Uani 1 1 d U . . H18A H 0.5079 0.6909 0.3858 0.028 Uiso 1 1 calc R . . H18B H 0.4643 0.6846 0.3123 0.028 Uiso 1 1 calc R . . C19 C 0.2565(6) 0.8137(5) 0.5816(5) 0.021(2) Uani 1 1 d . . . C20 C 0.3325(6) 0.8530(5) 0.5934(5) 0.022(2) Uani 1 1 d . . . H20A H 0.3793 0.8684 0.5546 0.026 Uiso 1 1 calc R . . C21 C 0.3422(6) 0.8704(5) 0.6611(5) 0.023(2) Uani 1 1 d . . . H21A H 0.3951 0.8973 0.6678 0.028 Uiso 1 1 calc R . . C22 C 0.2763(6) 0.8491(6) 0.7170(5) 0.027(2) Uani 1 1 d . . . C23 C 0.2000(6) 0.8092(5) 0.7062(4) 0.019(2) Uani 1 1 d . . . C24 C 0.1894(6) 0.7916(5) 0.6395(5) 0.019(2) Uani 1 1 d U . . H24A H 0.1365 0.7644 0.6333 0.023 Uiso 1 1 calc R . . C25 C 0.3593(6) 0.8813(6) 0.8109(5) 0.033(3) Uani 1 1 d . . . H25A H 0.3689 0.9369 0.7972 0.040 Uiso 1 1 calc R . . H25B H 0.4128 0.8551 0.7885 0.040 Uiso 1 1 calc R . . C26 C 0.3509(6) 0.8566(6) 0.8915(5) 0.035(3) Uani 1 1 d . . . H26A H 0.3474 0.8005 0.9051 0.042 Uiso 1 1 calc R . . H26B H 0.4056 0.8732 0.9116 0.042 Uiso 1 1 calc R . . C27 C 0.2471(7) 0.8705(6) 0.9962(5) 0.033(3) Uani 1 1 d . . . H27A H 0.2063 0.9102 1.0136 0.040 Uiso 1 1 calc R . . H27B H 0.3057 0.8680 1.0196 0.040 Uiso 1 1 calc R . . C28 C 0.1995(7) 0.7947(6) 1.0182(5) 0.035(3) Uani 1 1 d . . . H28A H 0.2412 0.7533 1.0053 0.042 Uiso 1 1 calc R . . H28B H 0.1809 0.7833 1.0710 0.042 Uiso 1 1 calc R . . C29 C 0.0580(7) 0.7374(6) 0.9976(5) 0.035(3) Uani 1 1 d . . . H29A H 0.0383 0.7270 1.0502 0.041 Uiso 1 1 calc R . . H29B H 0.0903 0.6916 0.9845 0.041 Uiso 1 1 calc R . . C30 C -0.0254(6) 0.7593(6) 0.9545(5) 0.034(3) Uani 1 1 d . . . H30A H -0.0671 0.7152 0.9619 0.040 Uiso 1 1 calc R . . H30B H -0.0607 0.8013 0.9725 0.040 Uiso 1 1 calc R . . C31 C 0.0183(6) 0.7181(5) 0.8416(5) 0.027(2) Uani 1 1 d U . . H31A H -0.0408 0.6911 0.8437 0.032 Uiso 1 1 calc R . . H31B H 0.0642 0.6820 0.8655 0.032 Uiso 1 1 calc R . . C32 C 0.0541(6) 0.7483(5) 0.7643(5) 0.027(2) Uani 1 1 d . . . H32A H 0.0697 0.7061 0.7381 0.032 Uiso 1 1 calc R . . H32B H 0.0068 0.7819 0.7392 0.032 Uiso 1 1 calc R . . C33 C 0.0955(6) 0.8841(5) 0.5079(5) 0.023(2) Uani 1 1 d . . . C34 C 0.0103(6) 0.8491(5) 0.5262(5) 0.021(2) Uani 1 1 d . . . H34A H -0.0029 0.8073 0.5050 0.025 Uiso 1 1 calc R . . C35 C -0.0572(6) 0.8744(5) 0.5759(5) 0.025(2) Uani 1 1 d . . . H35A H -0.1146 0.8487 0.5894 0.030 Uiso 1 1 calc R . . C36 C -0.0394(6) 0.9360(5) 0.6046(4) 0.024(2) Uani 1 1 d . . . C37 C 0.0469(6) 0.9706(5) 0.5873(5) 0.021(2) Uani 1 1 d . . . C38 C 0.1127(6) 0.9445(5) 0.5401(4) 0.0159(19) Uani 1 1 d U . . H38A H 0.1716 0.9683 0.5292 0.019 Uiso 1 1 calc R . . C39 C -0.1789(6) 0.9229(6) 0.6855(5) 0.029(2) Uani 1 1 d . . . H39A H -0.1588 0.8709 0.7073 0.035 Uiso 1 1 calc R . . H39B H -0.2222 0.9194 0.6490 0.035 Uiso 1 1 calc R . . C40 C -0.2250(6) 0.9625(6) 0.7423(5) 0.031(2) Uani 1 1 d . . . H40A H -0.2368 1.0166 0.7211 0.037 Uiso 1 1 calc R . . H40B H -0.2856 0.9388 0.7617 0.037 Uiso 1 1 calc R . . C41 C -0.1956(6) 1.0072(5) 0.8484(5) 0.026(2) Uani 1 1 d . . . H41A H -0.1777 0.9848 0.8972 0.031 Uiso 1 1 calc R . . H41B H -0.2643 1.0129 0.8518 0.031 Uiso 1 1 calc R . . C42 C -0.1522(6) 1.0849(5) 0.8231(5) 0.025(2) Uani 1 1 d . . . H42A H -0.1544 1.1019 0.7703 0.030 Uiso 1 1 calc R . . H42B H -0.1863 1.1228 0.8482 0.030 Uiso 1 1 calc R . . C43 C -0.0056(7) 1.1469(5) 0.8205(5) 0.039(3) Uani 1 1 d . . . H43A H 0.0502 1.1414 0.8475 0.047 Uiso 1 1 calc R . . H43B H -0.0445 1.1892 0.8348 0.047 Uiso 1 1 calc R . . C44 C 0.0246(7) 1.1664(6) 0.7404(6) 0.045(3) Uani 1 1 d . . . H44A H -0.0294 1.1641 0.7128 0.054 Uiso 1 1 calc R . . H44B H 0.0487 1.2188 0.7278 0.054 Uiso 1 1 calc R . . C45 C 0.1321(6) 1.1335(6) 0.6472(5) 0.032(2) Uani 1 1 d . . . H45A H 0.1922 1.1595 0.6435 0.038 Uiso 1 1 calc R . . H45B H 0.0886 1.1686 0.6191 0.038 Uiso 1 1 calc R . . C46 C 0.1463(6) 1.0627(5) 0.6167(5) 0.030(2) Uani 1 1 d . . . H46A H 0.1714 1.0752 0.5651 0.036 Uiso 1 1 calc R . . H46B H 0.1909 1.0279 0.6437 0.036 Uiso 1 1 calc R . . C47 C 0.2121(6) 0.7863(5) 0.3541(4) 0.018(2) Uani 1 1 d . . . C48 C 0.2898(5) 0.8283(5) 0.3282(4) 0.020(2) Uani 1 1 d . . . H48A H 0.3094 0.8626 0.3559 0.023 Uiso 1 1 calc R . . C49 C 0.3414(6) 0.8228(5) 0.2629(4) 0.019(2) Uani 1 1 d . . . H49A H 0.3944 0.8537 0.2465 0.022 Uiso 1 1 calc R . . C50 C 0.3155(6) 0.7724(5) 0.2218(5) 0.025(2) Uani 1 1 d . . . C51 C 0.2356(6) 0.7287(5) 0.2466(5) 0.022(2) Uani 1 1 d . . . C52 C 0.1857(6) 0.7363(5) 0.3117(5) 0.023(2) Uani 1 1 d . . . H52A H 0.1318 0.7065 0.3280 0.028 Uiso 1 1 calc R . . C53 C 0.1433(7) 0.6269(6) 0.2290(5) 0.036(3) Uani 1 1 d . . . H53A H 0.0815 0.6518 0.2355 0.043 Uiso 1 1 calc R . . H53B H 0.1580 0.5970 0.2764 0.043 Uiso 1 1 calc R . . C54 C 0.1432(7) 0.5759(6) 0.1741(6) 0.037(3) Uani 1 1 d . . . H54A H 0.0918 0.5393 0.1880 0.045 Uiso 1 1 calc R . . H54B H 0.1351 0.6065 0.1255 0.045 Uiso 1 1 calc R . . C55 C 0.2554(10) 0.4913(8) 0.1222(8) 0.079(4) Uani 1 1 d . . . H55A H 0.1981 0.4738 0.1064 0.094 Uiso 1 1 calc R . . H55B H 0.2906 0.4459 0.1445 0.094 Uiso 1 1 calc R . . C56 C 0.3121(9) 0.5327(7) 0.0593(6) 0.061(4) Uani 1 1 d U . . H56A H 0.3184 0.5028 0.0202 0.074 Uiso 1 1 calc R . . H56B H 0.2812 0.5819 0.0410 0.074 Uiso 1 1 calc R . . C57 C 0.4584(8) 0.5989(6) 0.0252(5) 0.046(3) Uani 1 1 d . . . H57A H 0.4198 0.6438 0.0067 0.056 Uiso 1 1 calc R . . H57B H 0.4819 0.5744 -0.0159 0.056 Uiso 1 1 calc R . . C58 C 0.5386(8) 0.6231(6) 0.0594(5) 0.043(3) Uani 1 1 d . . . H58A H 0.5728 0.5773 0.0822 0.051 Uiso 1 1 calc R . . H58B H 0.5819 0.6531 0.0212 0.051 Uiso 1 1 calc R . . C59 C 0.5004(7) 0.7464(6) 0.0833(5) 0.039(3) Uani 1 1 d . . . H59A H 0.4613 0.7543 0.0424 0.047 Uiso 1 1 calc R . . H59B H 0.5624 0.7681 0.0652 0.047 Uiso 1 1 calc R . . C60 C 0.4554(6) 0.7857(6) 0.1429(5) 0.032(3) Uani 1 1 d . . . H60A H 0.4883 0.7710 0.1870 0.039 Uiso 1 1 calc R . . H60B H 0.4581 0.8416 0.1270 0.039 Uiso 1 1 calc R . . C1S C 0.3639(7) 0.1654(6) 0.3727(6) 0.043(3) Uani 1 1 d . . . H1SA H 0.3482 0.2176 0.3579 0.052 Uiso 1 1 calc R . . C2S C 0.4028(7) 0.1244(7) 0.3208(6) 0.039(3) Uani 1 1 d . . . H2SA H 0.4118 0.1478 0.2710 0.047 Uiso 1 1 calc R . . C3S C 0.4280(7) 0.0490(6) 0.3435(7) 0.048(3) Uani 1 1 d . . . H3SA H 0.4568 0.0208 0.3093 0.057 Uiso 1 1 calc R . . C4S C 0.4117(7) 0.0138(7) 0.4163(7) 0.048(3) Uani 1 1 d . . . H4SA H 0.4280 -0.0383 0.4313 0.058 Uiso 1 1 calc R . . C5S C 0.3723(7) 0.0547(7) 0.4657(6) 0.044(3) Uani 1 1 d . . . H5SA H 0.3616 0.0302 0.5150 0.053 Uiso 1 1 calc R . . C6S C 0.3473(8) 0.1311(6) 0.4461(7) 0.047(3) Uani 1 1 d . . . H6SA H 0.3202 0.1591 0.4811 0.056 Uiso 1 1 calc R . . C7S C 0.1125(8) 0.3353(6) 0.5689(7) 0.053(3) Uani 1 1 d U . . H7SA H 0.1357 0.2987 0.5410 0.063 Uiso 1 1 calc R . . C8S C 0.0395(8) 0.3821(7) 0.5485(7) 0.058(4) Uani 1 1 d U . . H8SA H 0.0109 0.3780 0.5065 0.069 Uiso 1 1 calc R . . C9S C 0.0084(9) 0.4338(8) 0.5879(7) 0.061(4) Uani 1 1 d . . . H9SA H -0.0419 0.4669 0.5731 0.073 Uiso 1 1 calc R . . C10S C 0.0486(9) 0.4402(7) 0.6506(8) 0.063(4) Uani 1 1 d . . . H10B H 0.0261 0.4780 0.6772 0.075 Uiso 1 1 calc R . . C11S C 0.1189(10) 0.3934(8) 0.6734(8) 0.074(4) Uani 1 1 d U . . H11C H 0.1443 0.3960 0.7172 0.088 Uiso 1 1 calc R . . C12S C 0.1530(8) 0.3419(7) 0.6320(7) 0.059(4) Uani 1 1 d U . . H12C H 0.2046 0.3101 0.6460 0.071 Uiso 1 1 calc R . . C13S C 0.3989(9) 0.2087(8) 0.1042(7) 0.067(4) Uani 1 1 d U . . H13C H 0.4469 0.1852 0.0775 0.080 Uiso 1 1 calc R . . C14S C 0.3077(9) 0.1883(7) 0.1058(6) 0.053(3) Uani 1 1 d . . . H14C H 0.2918 0.1515 0.0793 0.063 Uiso 1 1 calc R . . C15S C 0.2404(8) 0.2219(6) 0.1461(7) 0.048(3) Uani 1 1 d . . . H15C H 0.1768 0.2093 0.1471 0.058 Uiso 1 1 calc R . . C16S C 0.2652(9) 0.2740(7) 0.1853(7) 0.061(4) Uani 1 1 d . . . H16C H 0.2183 0.2953 0.2148 0.073 Uiso 1 1 calc R . . C17S C 0.3555(10) 0.2960(7) 0.1828(8) 0.069(4) Uani 1 1 d U . . H17C H 0.3715 0.3329 0.2092 0.083 Uiso 1 1 calc R . . C18S C 0.4205(9) 0.2637(8) 0.1420(7) 0.066(4) Uani 1 1 d U . . H18C H 0.4834 0.2790 0.1388 0.079 Uiso 1 1 calc R . . O7W O -0.1302(5) 0.9295(4) 1.0305(4) 0.054(2) Uani 1 1 d . . . O8W O 0.3430(7) 1.0814(6) 0.8282(5) 0.100(4) Uani 1 1 d U . . O9W O -0.0157(18) 0.5202(13) 0.9629(12) 0.135(9) Uani 0.50 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0373(15) 0.0353(15) 0.0289(14) -0.0147(12) -0.0034(12) 0.0084(12) O11' 0.091(6) 0.043(5) 0.037(5) -0.013(4) -0.028(4) 0.042(5) O12' 0.053(5) 0.051(5) 0.027(4) -0.023(4) 0.002(3) 0.018(4) O13' 0.055(5) 0.071(6) 0.062(6) -0.021(5) 0.012(4) -0.009(5) O14' 0.035(4) 0.066(6) 0.055(5) -0.035(4) -0.005(4) 0.013(4) Cl2 0.0347(16) 0.0279(15) 0.068(2) -0.0131(14) -0.0049(15) -0.0042(13) O21 0.041(5) 0.032(4) 0.085(6) -0.016(4) -0.007(4) -0.015(4) O22 0.033(5) 0.055(5) 0.104(7) -0.036(5) 0.026(5) -0.005(4) O23 0.048(5) 0.061(6) 0.056(5) -0.004(5) -0.025(4) -0.002(4) O24 0.034(4) 0.034(4) 0.069(5) -0.003(4) -0.007(4) 0.001(4) Cl3 0.0383(17) 0.052(2) 0.057(2) -0.0192(17) 0.0092(15) -0.0176(15) O31 0.031(4) 0.070(6) 0.061(5) -0.024(5) 0.017(4) -0.022(4) O32 0.055(8) 0.061(9) 0.051(7) -0.007(7) 0.008(5) -0.008(6) O33 0.110(12) 0.112(12) 0.125(14) 0.029(10) 0.046(10) 0.050(10) O34 0.075(9) 0.105(13) 0.133(12) -0.073(10) 0.030(8) -0.047(9) O35 0.018(17) 0.08(2) 0.08(2) 0.005(16) 0.008(15) -0.021(14) O36 0.028(13) 0.038(15) 0.030(14) 0.006(9) -0.021(9) -0.014(9) O37 0.14(3) 0.12(4) 0.12(3) -0.011(19) -0.017(19) 0.012(19) Cl4 0.073(4) 0.087(4) 0.061(4) 0.024(3) 0.003(3) -0.045(3) O41 0.038(8) 0.144(13) 0.089(10) -0.072(10) 0.003(7) -0.006(8) O42 0.075(10) 0.137(13) 0.070(10) 0.010(10) -0.009(8) -0.042(10) O43 0.092(12) 0.144(14) 0.171(15) -0.016(12) -0.074(11) -0.055(11) O44 0.125(14) 0.163(16) 0.142(14) 0.032(13) 0.029(12) 0.068(13) O10W 0.096(17) 0.045(15) 0.120(19) 0.002(14) -0.045(15) -0.044(14) Cl5 0.114(8) 0.058(6) 0.080(7) 0.007(6) -0.013(6) -0.032(6) O51 0.088(15) 0.088(15) 0.083(14) -0.054(12) -0.027(13) 0.003(13) O52 0.15(2) 0.14(2) 0.14(2) 0.000(16) -0.064(16) -0.080(17) O53 0.16(2) 0.064(15) 0.073(15) 0.011(13) -0.014(15) -0.004(15) O54 0.073(14) 0.050(13) 0.145(18) -0.038(13) 0.024(13) -0.031(12) O11W 0.076(16) 0.062(15) 0.082(16) -0.008(10) -0.006(10) -0.033(10) Ca1 0.0168(10) 0.0145(9) 0.0242(10) -0.0043(8) -0.0024(8) 0.0011(8) Ca2 0.0206(10) 0.0256(11) 0.0236(11) -0.0034(9) -0.0071(8) 0.0034(9) O1W 0.024(4) 0.019(3) 0.035(4) -0.005(3) -0.008(3) 0.003(3) O2W 0.038(4) 0.024(4) 0.029(4) -0.013(3) -0.008(3) 0.005(3) O3W 0.028(4) 0.031(4) 0.060(5) 0.006(4) -0.011(4) -0.007(3) O4W 0.020(3) 0.019(3) 0.030(4) -0.001(3) -0.011(3) 0.005(3) O5W 0.044(4) 0.019(4) 0.030(4) -0.009(3) 0.000(3) 0.011(3) O6W 0.026(4) 0.025(4) 0.059(5) -0.003(4) -0.009(3) -0.001(3) O1 0.026(3) 0.009(3) 0.033(4) -0.002(3) 0.011(3) 0.000(3) O2 0.022(3) 0.011(3) 0.030(4) 0.000(3) 0.003(3) 0.002(3) O3 0.018(3) 0.020(3) 0.036(4) -0.006(3) -0.008(3) 0.006(3) O4 0.027(4) 0.016(3) 0.032(4) -0.003(3) -0.005(3) -0.003(3) O5 0.019(3) 0.013(3) 0.028(4) -0.008(3) 0.002(3) -0.002(3) O6 0.020(3) 0.048(4) 0.027(4) -0.020(3) 0.000(3) -0.009(3) O7 0.027(4) 0.032(4) 0.025(4) -0.005(3) -0.004(3) 0.007(3) O8 0.019(3) 0.031(4) 0.031(4) -0.006(3) -0.004(3) 0.000(3) O9 0.020(3) 0.030(4) 0.023(4) -0.006(3) 0.004(3) 0.003(3) O10 0.021(3) 0.018(3) 0.025(3) -0.006(3) 0.000(3) -0.003(3) O11 0.019(3) 0.028(4) 0.026(4) -0.010(3) 0.001(3) 0.002(3) O12 0.021(3) 0.022(4) 0.033(4) -0.012(3) -0.005(3) 0.005(3) O13 0.025(4) 0.024(4) 0.050(4) -0.011(3) -0.006(3) 0.006(3) O14 0.028(4) 0.027(4) 0.033(4) -0.012(3) -0.008(3) 0.012(3) O15 0.017(3) 0.023(4) 0.032(4) -0.007(3) -0.006(3) 0.001(3) O16 0.028(4) 0.027(4) 0.025(4) -0.007(3) -0.001(3) 0.000(3) O17 0.042(5) 0.026(4) 0.068(5) -0.023(4) -0.005(4) 0.005(4) O18 0.058(5) 0.035(4) 0.033(4) -0.005(4) -0.012(4) -0.001(4) O19 0.039(4) 0.023(4) 0.028(4) -0.004(3) 0.005(3) 0.009(3) O20 0.022(3) 0.026(4) 0.022(3) -0.002(3) -0.003(3) 0.002(3) C1 0.022(5) 0.018(5) 0.022(5) -0.001(4) 0.004(4) -0.006(4) C2 0.023(5) 0.030(6) 0.014(5) -0.006(4) 0.000(4) 0.003(4) C3 0.025(5) 0.014(5) 0.026(5) 0.005(4) 0.002(4) -0.001(4) C4 0.015(5) 0.030(6) 0.019(5) -0.003(4) -0.003(4) -0.002(4) C5 0.019(4) 0.021(4) 0.013(4) -0.007(4) -0.007(4) 0.000(4) C6 0.017(5) 0.032(6) 0.012(5) 0.006(4) 0.005(4) -0.006(4) C7 0.027(5) 0.015(5) 0.018(5) 0.004(4) 0.003(4) -0.002(4) C8 0.017(5) 0.025(5) 0.032(6) -0.014(5) 0.000(4) 0.005(4) C9 0.016(5) 0.027(5) 0.012(5) -0.004(4) -0.003(4) 0.007(4) C10 0.028(5) 0.016(4) 0.015(4) -0.012(4) -0.004(4) -0.003(4) C11 0.030(5) 0.013(5) 0.033(6) -0.011(4) 0.003(4) -0.001(4) C12 0.039(6) 0.014(5) 0.020(5) -0.002(4) 0.000(4) 0.003(4) C13 0.027(5) 0.018(5) 0.035(6) -0.007(5) 0.008(5) -0.008(4) C14 0.032(6) 0.028(6) 0.025(5) -0.003(5) -0.004(4) 0.020(5) C15 0.021(5) 0.023(5) 0.049(7) -0.020(5) -0.009(5) 0.003(4) C16 0.019(5) 0.032(6) 0.043(6) -0.019(5) 0.009(5) 0.001(4) C17 0.023(5) 0.028(6) 0.033(6) -0.007(5) 0.005(4) -0.008(4) C18 0.025(5) 0.014(4) 0.030(5) -0.003(4) 0.003(4) -0.009(4) C19 0.017(5) 0.016(5) 0.029(5) 0.000(4) -0.004(4) 0.007(4) C20 0.019(5) 0.027(5) 0.016(5) 0.006(4) -0.002(4) 0.000(4) C21 0.017(5) 0.018(5) 0.033(6) -0.001(4) -0.004(4) -0.003(4) C22 0.021(5) 0.037(6) 0.025(5) -0.009(5) -0.002(4) -0.004(5) C23 0.024(5) 0.018(5) 0.014(5) 0.002(4) -0.008(4) 0.005(4) C24 0.022(4) 0.013(4) 0.026(5) -0.005(4) -0.013(4) 0.007(4) C25 0.025(6) 0.040(7) 0.038(6) -0.015(5) -0.009(5) -0.001(5) C26 0.020(5) 0.051(7) 0.035(6) -0.007(6) -0.009(5) -0.004(5) C27 0.045(7) 0.037(6) 0.023(6) -0.014(5) -0.009(5) 0.007(5) C28 0.035(6) 0.042(7) 0.030(6) -0.012(5) -0.005(5) 0.010(5) C29 0.039(6) 0.030(6) 0.027(6) 0.010(5) 0.002(5) 0.000(5) C30 0.024(5) 0.054(7) 0.022(5) -0.008(5) 0.003(4) 0.006(5) C31 0.029(5) 0.032(5) 0.020(5) -0.011(4) 0.006(4) 0.000(4) C32 0.026(5) 0.026(5) 0.030(6) -0.010(5) -0.001(4) -0.008(4) C33 0.021(5) 0.025(5) 0.024(5) -0.007(4) -0.007(4) 0.001(4) C34 0.017(5) 0.022(5) 0.027(5) -0.012(4) -0.006(4) -0.001(4) C35 0.019(5) 0.023(5) 0.035(6) -0.006(5) -0.006(4) 0.000(4) C36 0.026(5) 0.034(6) 0.012(5) -0.002(4) -0.006(4) 0.001(5) C37 0.015(5) 0.017(5) 0.032(6) -0.005(4) -0.001(4) -0.005(4) C38 0.017(4) 0.013(4) 0.017(4) -0.005(4) 0.005(4) -0.003(3) C39 0.015(5) 0.045(7) 0.029(6) -0.016(5) 0.005(4) -0.004(5) C40 0.021(5) 0.034(6) 0.037(6) -0.004(5) -0.005(5) 0.007(5) C41 0.027(5) 0.026(5) 0.027(5) -0.014(5) 0.003(4) -0.003(4) C42 0.026(5) 0.026(5) 0.025(5) -0.013(4) 0.000(4) 0.010(4) C43 0.051(7) 0.017(5) 0.049(7) -0.015(5) 0.013(6) 0.000(5) C44 0.043(7) 0.034(6) 0.052(7) -0.002(6) 0.009(6) 0.019(5) C45 0.023(5) 0.035(6) 0.038(6) -0.006(5) -0.005(5) -0.006(5) C46 0.020(5) 0.036(6) 0.032(6) -0.004(5) -0.001(4) 0.001(5) C47 0.020(5) 0.020(5) 0.012(4) -0.001(4) -0.004(4) 0.006(4) C48 0.015(5) 0.026(5) 0.018(5) -0.003(4) 0.000(4) -0.004(4) C49 0.025(5) 0.012(5) 0.018(5) -0.003(4) 0.001(4) 0.003(4) C50 0.031(6) 0.016(5) 0.023(5) 0.003(4) 0.005(4) 0.006(4) C51 0.020(5) 0.024(5) 0.024(5) -0.010(4) -0.004(4) 0.006(4) C52 0.020(5) 0.023(5) 0.027(5) -0.005(4) -0.002(4) 0.009(4) C53 0.032(6) 0.036(6) 0.037(6) -0.005(5) 0.002(5) -0.001(5) C54 0.036(6) 0.029(6) 0.052(7) -0.019(6) -0.009(5) 0.001(5) C55 0.073(10) 0.076(11) 0.097(12) -0.039(10) -0.013(9) 0.008(9) C56 0.074(7) 0.067(7) 0.043(6) -0.001(6) -0.021(6) -0.014(6) C57 0.069(8) 0.039(7) 0.025(6) -0.002(5) 0.015(6) 0.011(6) C58 0.052(7) 0.037(7) 0.035(6) -0.009(6) 0.014(6) 0.005(6) C59 0.042(7) 0.046(7) 0.030(6) -0.015(6) 0.010(5) 0.001(6) C60 0.024(5) 0.043(7) 0.028(6) -0.009(5) 0.006(4) -0.007(5) C1S 0.043(7) 0.030(6) 0.056(8) 0.001(6) -0.018(6) -0.012(5) C2S 0.027(6) 0.056(8) 0.035(6) -0.006(6) -0.008(5) -0.009(6) C3S 0.041(7) 0.036(7) 0.065(9) -0.008(7) -0.008(6) 0.003(6) C4S 0.038(7) 0.045(7) 0.062(9) -0.002(7) -0.017(6) 0.001(6) C5S 0.048(7) 0.050(8) 0.037(7) -0.010(6) -0.006(6) -0.011(6) C6S 0.050(7) 0.031(7) 0.062(8) -0.013(6) -0.006(6) -0.006(6) C7S 0.044(6) 0.036(6) 0.069(7) 0.007(6) 0.010(6) -0.016(5) C8S 0.044(6) 0.058(7) 0.064(7) 0.010(6) -0.008(6) -0.012(6) C9S 0.044(8) 0.060(9) 0.062(9) 0.024(8) 0.003(7) 0.005(7) C10S 0.060(9) 0.040(8) 0.085(11) -0.008(8) 0.000(8) -0.002(7) C11S 0.069(8) 0.059(7) 0.095(8) -0.009(7) -0.025(7) -0.014(6) C12S 0.029(6) 0.059(7) 0.079(7) 0.022(6) -0.018(6) -0.011(5) C13S 0.058(7) 0.074(8) 0.055(7) 0.005(6) 0.007(6) 0.028(6) C14S 0.064(9) 0.058(8) 0.034(7) 0.000(6) -0.012(6) 0.014(7) C15S 0.045(7) 0.031(7) 0.068(9) 0.001(6) -0.020(7) -0.012(6) C16S 0.060(9) 0.058(9) 0.060(9) -0.014(7) 0.006(7) 0.027(7) C17S 0.081(8) 0.047(7) 0.084(8) -0.011(6) -0.033(7) 0.000(6) C18S 0.046(6) 0.061(7) 0.077(8) 0.031(6) -0.022(6) -0.018(6) O7W 0.056(5) 0.067(6) 0.048(5) -0.034(4) -0.005(4) 0.009(4) O8W 0.093(7) 0.117(8) 0.095(7) -0.026(7) -0.002(6) -0.052(7) O9W 0.156(12) 0.108(12) 0.156(13) -0.036(9) -0.041(9) -0.062(9) _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 Cl1 O12' 1.432(6) . ? Cl1 O14' 1.445(7) . ? Cl1 O11' 1.451(7) . ? Cl1 O13' 1.472(8) . ? Cl2 O21 1.437(7) . ? Cl2 O24 1.439(7) . ? Cl2 O23 1.452(8) . ? Cl2 O22 1.462(7) . ? Cl3 O36 1.385(12) . ? Cl3 O33 1.403(9) . ? Cl3 O32 1.413(8) . ? Cl3 O31 1.415(6) . ? Cl3 O37 1.422(12) . ? Cl3 O35 1.445(12) . ? Cl3 O34 1.456(9) . ? Cl4 O44 1.344(10) . ? Cl4 O41 1.382(9) . ? Cl4 O42 1.420(10) . ? Cl4 O43 1.496(10) . ? Cl5 O51 1.380(12) . ? Cl5 O54 1.391(12) . ? Cl5 O53 1.437(13) . ? Cl5 O52 1.443(13) . ? Ca1 O3W 2.354(6) . ? Ca1 O2W 2.374(6) . ? Ca1 O1W 2.379(6) . ? Ca1 O3 2.438(6) . ? Ca1 O4 2.494(6) . ? Ca1 O2 2.504(6) . ? Ca1 O5 2.528(6) . ? Ca1 O1 2.535(6) . ? Ca2 O4W 2.371(6) . ? Ca2 O5W 2.387(6) . ? Ca2 O6W 2.402(6) . ? Ca2 O6 2.443(6) . ? Ca2 O8 2.482(6) . ? Ca2 O9 2.497(6) . ? Ca2 O7 2.523(6) . ? Ca2 O10 2.526(6) . ? O1 C8 1.387(10) . ? O1 C11 1.421(9) . ? O2 C12 1.429(10) . ? O2 C13 1.437(10) . ? O3 C14 1.430(10) . ? O3 C15 1.449(10) . ? O4 C17 1.444(10) . ? O4 C16 1.451(10) . ? O5 C9 1.400(9) . ? O5 C18 1.438(9) . ? O6 C22 1.383(10) . ? O6 C25 1.427(10) . ? O7 C26 1.427(11) . ? O7 C27 1.440(10) . ? O8 C28 1.447(11) . ? O8 C29 1.454(10) . ? O9 C30 1.449(10) . ? O9 C31 1.458(10) . ? O10 C23 1.389(10) . ? O10 C32 1.465(9) . ? O11 C36 1.379(10) . ? O11 C39 1.439(10) . ? O12 C41 1.428(10) . ? O12 C40 1.434(10) . ? O13 C42 1.427(10) . ? O13 C43 1.446(10) . ? O14 C44 1.409(11) . ? O14 C45 1.434(10) . ? O15 C37 1.373(10) . ? O15 C46 1.411(10) . ? O16 C51 1.374(10) . ? O16 C53 1.428(10) . ? O17 C55 1.398(14) . ? O17 C54 1.427(11) . ? O18 C57 1.439(11) . ? O18 C56 1.452(13) . ? O19 C58 1.406(11) . ? O19 C59 1.426(11) . ? O20 C50 1.362(10) . ? O20 C60 1.431(10) . ? C1 C5 1.490(12) . ? C1 C2 1.565(12) . ? C1 C4 1.596(12) . ? C2 C19 1.487(12) . ? C2 C3 1.583(12) . ? C3 C33 1.507(12) . ? C3 C4 1.543(12) . ? C4 C47 1.497(11) . ? C5 C6 1.385(11) . ? C5 C10 1.417(11) . ? C6 C7 1.408(12) . ? C7 C8 1.377(11) . ? C8 C9 1.386(12) . ? C9 C10 1.363(11) . ? C11 C12 1.496(12) . ? C13 C14 1.512(12) . ? C15 C16 1.498(13) . ? C17 C18 1.490(12) . ? C19 C20 1.386(11) . ? C19 C24 1.390(11) . ? C20 C21 1.397(12) . ? C21 C22 1.352(12) . ? C22 C23 1.389(12) . ? C23 C24 1.384(11) . ? C25 C26 1.497(12) . ? C27 C28 1.511(13) . ? C29 C30 1.521(12) . ? C31 C32 1.500(11) . ? C33 C34 1.381(11) . ? C33 C38 1.384(11) . ? C34 C35 1.408(12) . ? C35 C36 1.366(12) . ? C36 C37 1.393(11) . ? C37 C38 1.369(11) . ? C39 C40 1.489(12) . ? C41 C42 1.519(12) . ? C43 C44 1.508(13) . ? C45 C46 1.493(13) . ? C47 C48 1.367(11) . ? C47 C52 1.402(12) . ? C48 C49 1.393(11) . ? C49 C50 1.386(12) . ? C50 C51 1.405(12) . ? C51 C52 1.388(12) . ? C53 C54 1.511(13) . ? C55 C56 1.460(16) . ? C57 C58 1.499(14) . ? C59 C60 1.521(13) . ? C1S C2S 1.398(14) . ? C1S C6S 1.405(14) . ? C2S C3S 1.384(15) . ? C3S C4S 1.398(15) . ? C4S C5S 1.364(15) . ? C5S C6S 1.392(15) . ? C7S C8S 1.363(16) . ? C7S C12S 1.409(16) . ? C8S C9S 1.337(17) . ? C9S C10S 1.399(17) . ? C10S C11S 1.344(17) . ? C11S C12S 1.371(18) . ? C13S C14S 1.375(16) . ? C13S C18S 1.387(18) . ? C14S C15S 1.368(16) . ? C15S C16S 1.380(16) . ? C16S C17S 1.370(16) . ? C17S C18S 1.340(18) . ? O9W O9W 1.55(4) 2_567 ? 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 O12' Cl1 O14' 111.1(4) . . ? O12' Cl1 O11' 109.7(4) . . ? O14' Cl1 O11' 108.3(5) . . ? O12' Cl1 O13' 109.3(5) . . ? O14' Cl1 O13' 109.4(5) . . ? O11' Cl1 O13' 109.2(5) . . ? O21 Cl2 O24 110.1(4) . . ? O21 Cl2 O23 109.1(5) . . ? O24 Cl2 O23 108.4(5) . . ? O21 Cl2 O22 112.1(5) . . ? O24 Cl2 O22 107.4(5) . . ? O23 Cl2 O22 109.6(5) . . ? O36 Cl3 O33 74.7(12) . . ? O36 Cl3 O32 128.6(12) . . ? O33 Cl3 O32 112.2(7) . . ? O36 Cl3 O31 112.5(9) . . ? O33 Cl3 O31 110.2(6) . . ? O32 Cl3 O31 111.8(5) . . ? O36 Cl3 O37 111.2(11) . . ? O33 Cl3 O37 132.9(14) . . ? O32 Cl3 O37 27.0(18) . . ? O31 Cl3 O37 109.7(10) . . ? O36 Cl3 O35 110.0(10) . . ? O33 Cl3 O35 37.3(13) . . ? O32 Cl3 O35 80.7(17) . . ? O31 Cl3 O35 106.3(9) . . ? O37 Cl3 O35 106.8(10) . . ? O36 Cl3 O34 35.2(12) . . ? O33 Cl3 O34 109.0(7) . . ? O32 Cl3 O34 106.6(7) . . ? O31 Cl3 O34 106.8(6) . . ? O37 Cl3 O34 82.0(16) . . ? O35 Cl3 O34 140.1(11) . . ? O44 Cl4 O41 111.2(8) . . ? O44 Cl4 O42 112.7(9) . . ? O41 Cl4 O42 114.3(8) . . ? O44 Cl4 O43 111.2(9) . . ? O41 Cl4 O43 102.5(8) . . ? O42 Cl4 O43 104.2(8) . . ? O51 Cl5 O54 114.1(11) . . ? O51 Cl5 O53 111.2(11) . . ? O54 Cl5 O53 111.4(11) . . ? O51 Cl5 O52 108.2(11) . . ? O54 Cl5 O52 108.8(10) . . ? O53 Cl5 O52 102.3(10) . . ? O3W Ca1 O2W 86.1(2) . . ? O3W Ca1 O1W 75.2(2) . . ? O2W Ca1 O1W 78.5(2) . . ? O3W Ca1 O3 142.0(2) . . ? O2W Ca1 O3 76.8(2) . . ? O1W Ca1 O3 132.0(2) . . ? O3W Ca1 O4 147.4(2) . . ? O2W Ca1 O4 88.2(2) . . ? O1W Ca1 O4 72.1(2) . . ? O3 Ca1 O4 66.6(2) . . ? O3W Ca1 O2 81.0(2) . . ? O2W Ca1 O2 92.0(2) . . ? O1W Ca1 O2 154.8(2) . . ? O3 Ca1 O2 66.20(19) . . ? O4 Ca1 O2 131.4(2) . . ? O3W Ca1 O5 109.2(2) . . ? O2W Ca1 O5 148.8(2) . . ? O1W Ca1 O5 79.4(2) . . ? O3 Ca1 O5 102.7(2) . . ? O4 Ca1 O5 64.05(19) . . ? O2 Ca1 O5 116.7(2) . . ? O3W Ca1 O1 76.7(2) . . ? O2W Ca1 O1 151.6(2) . . ? O1W Ca1 O1 117.7(2) . . ? O3 Ca1 O1 103.1(2) . . ? O4 Ca1 O1 118.3(2) . . ? O2 Ca1 O1 63.25(19) . . ? O5 Ca1 O1 59.59(18) . . ? O4W Ca2 O5W 78.5(2) . . ? O4W Ca2 O6W 77.2(2) . . ? O5W Ca2 O6W 77.3(2) . . ? O4W Ca2 O6 105.6(2) . . ? O5W Ca2 O6 154.4(2) . . ? O6W Ca2 O6 79.0(2) . . ? O4W Ca2 O8 140.4(2) . . ? O5W Ca2 O8 77.2(2) . . ? O6W Ca2 O8 126.2(2) . . ? O6 Ca2 O8 109.8(2) . . ? O4W Ca2 O9 80.8(2) . . ? O5W Ca2 O9 85.3(2) . . ? O6W Ca2 O9 154.2(2) . . ? O6 Ca2 O9 120.2(2) . . ? O8 Ca2 O9 66.5(2) . . ? O4W Ca2 O7 149.1(2) . . ? O5W Ca2 O7 98.9(2) . . ? O6W Ca2 O7 72.2(2) . . ? O6 Ca2 O7 64.2(2) . . ? O8 Ca2 O7 66.1(2) . . ? O9 Ca2 O7 130.1(2) . . ? O4W Ca2 O10 76.9(2) . . ? O5W Ca2 O10 143.5(2) . . ? O6W Ca2 O10 122.1(2) . . ? O6 Ca2 O10 59.95(19) . . ? O8 Ca2 O10 106.2(2) . . ? O9 Ca2 O10 64.47(19) . . ? O7 Ca2 O10 115.9(2) . . ? C8 O1 C11 120.0(6) . . ? C8 O1 Ca1 112.2(5) . . ? C11 O1 Ca1 116.7(5) . . ? C12 O2 C13 111.2(7) . . ? C12 O2 Ca1 118.7(5) . . ? C13 O2 Ca1 111.6(4) . . ? C14 O3 C15 114.6(6) . . ? C14 O3 Ca1 121.6(5) . . ? C15 O3 Ca1 119.5(5) . . ? C17 O4 C16 113.0(7) . . ? C17 O4 Ca1 119.2(5) . . ? C16 O4 Ca1 112.2(5) . . ? C9 O5 C18 117.6(6) . . ? C9 O5 Ca1 112.0(5) . . ? C18 O5 Ca1 115.0(5) . . ? C22 O6 C25 118.2(7) . . ? C22 O6 Ca2 119.5(5) . . ? C25 O6 Ca2 120.4(5) . . ? C26 O7 C27 114.0(7) . . ? C26 O7 Ca2 116.1(5) . . ? C27 O7 Ca2 111.2(5) . . ? C28 O8 C29 113.0(7) . . ? C28 O8 Ca2 120.2(5) . . ? C29 O8 Ca2 120.2(5) . . ? C30 O9 C31 111.9(7) . . ? C30 O9 Ca2 111.9(5) . . ? C31 O9 Ca2 118.2(5) . . ? C23 O10 C32 119.1(7) . . ? C23 O10 Ca2 116.7(5) . . ? C32 O10 Ca2 117.1(5) . . ? C36 O11 C39 115.9(7) . . ? C41 O12 C40 112.7(7) . . ? C42 O13 C43 114.6(7) . . ? C44 O14 C45 113.2(7) . . ? C37 O15 C46 119.6(7) . . ? C51 O16 C53 117.3(7) . . ? C55 O17 C54 119.6(9) . . ? C57 O18 C56 114.2(8) . . ? C58 O19 C59 113.9(7) . . ? C50 O20 C60 116.2(7) . . ? C5 C1 C2 122.0(7) . . ? C5 C1 C4 120.9(7) . . ? C2 C1 C4 87.2(6) . . ? C19 C2 C1 122.5(7) . . ? C19 C2 C3 118.3(8) . . ? C1 C2 C3 88.0(6) . . ? C33 C3 C4 118.1(7) . . ? C33 C3 C2 113.1(7) . . ? C4 C3 C2 88.4(7) . . ? C47 C4 C3 115.9(7) . . ? C47 C4 C1 114.2(7) . . ? C3 C4 C1 88.3(6) . . ? C6 C5 C10 118.6(8) . . ? C6 C5 C1 119.8(8) . . ? C10 C5 C1 121.5(8) . . ? C5 C6 C7 121.5(8) . . ? C8 C7 C6 118.3(8) . . ? C7 C8 C9 120.5(8) . . ? C7 C8 O1 126.0(8) . . ? C9 C8 O1 113.5(7) . . ? C10 C9 C8 121.6(8) . . ? C10 C9 O5 124.0(8) . . ? C8 C9 O5 114.3(8) . . ? C9 C10 C5 119.4(8) . . ? O1 C11 C12 105.2(7) . . ? O2 C12 C11 106.7(7) . . ? O2 C13 C14 111.0(7) . . ? O3 C14 C13 106.2(7) . . ? O3 C15 C16 106.2(7) . . ? O4 C16 C15 109.3(7) . . ? O4 C17 C18 108.6(7) . . ? O5 C18 C17 105.5(7) . . ? C20 C19 C24 117.9(8) . . ? C20 C19 C2 119.4(8) . . ? C24 C19 C2 122.6(8) . . ? C19 C20 C21 121.7(8) . . ? C22 C21 C20 120.0(8) . . ? C21 C22 O6 127.7(8) . . ? C21 C22 C23 119.1(9) . . ? O6 C22 C23 113.2(8) . . ? C24 C23 O10 125.2(8) . . ? C24 C23 C22 121.5(8) . . ? O10 C23 C22 113.3(7) . . ? C23 C24 C19 119.8(8) . . ? O6 C25 C26 106.9(7) . . ? O7 C26 C25 106.8(8) . . ? O7 C27 C28 111.7(8) . . ? O8 C28 C27 104.9(8) . . ? O8 C29 C30 105.0(7) . . ? O9 C30 C29 111.5(7) . . ? O9 C31 C32 107.5(7) . . ? O10 C32 C31 105.5(7) . . ? C34 C33 C38 118.1(8) . . ? C34 C33 C3 123.9(8) . . ? C38 C33 C3 117.6(8) . . ? C33 C34 C35 120.9(8) . . ? C36 C35 C34 119.5(8) . . ? C35 C36 O11 125.7(8) . . ? C35 C36 C37 119.7(9) . . ? O11 C36 C37 114.5(8) . . ? C38 C37 O15 125.7(7) . . ? C38 C37 C36 120.1(8) . . ? O15 C37 C36 114.1(8) . . ? C37 C38 C33 121.5(8) . . ? O11 C39 C40 106.2(7) . . ? O12 C40 C39 109.4(7) . . ? O12 C41 C42 111.2(7) . . ? O13 C42 C41 107.0(7) . . ? O13 C43 C44 112.4(8) . . ? O14 C44 C43 110.0(8) . . ? O14 C45 C46 109.8(8) . . ? O15 C46 C45 107.0(7) . . ? C48 C47 C52 116.8(8) . . ? C48 C47 C4 124.8(8) . . ? C52 C47 C4 118.4(8) . . ? C47 C48 C49 122.7(8) . . ? C50 C49 C48 120.1(8) . . ? O20 C50 C49 125.4(8) . . ? O20 C50 C51 116.0(8) . . ? C49 C50 C51 118.7(8) . . ? O16 C51 C52 125.6(8) . . ? O16 C51 C50 114.9(8) . . ? C52 C51 C50 119.5(8) . . ? C51 C52 C47 122.2(8) . . ? O16 C53 C54 106.6(8) . . ? O17 C54 C53 106.5(8) . . ? O17 C55 C56 111.5(11) . . ? O18 C56 C55 109.9(10) . . ? O18 C57 C58 108.5(8) . . ? O19 C58 C57 112.5(9) . . ? O19 C59 C60 108.9(8) . . ? O20 C60 C59 107.1(8) . . ? C2S C1S C6S 121.6(11) . . ? C3S C2S C1S 118.5(11) . . ? C2S C3S C4S 120.7(12) . . ? C5S C4S C3S 119.7(11) . . ? C4S C5S C6S 122.1(11) . . ? C5S C6S C1S 117.4(11) . . ? C8S C7S C12S 119.0(13) . . ? C9S C8S C7S 119.7(13) . . ? C8S C9S C10S 121.2(13) . . ? C11S C10S C9S 120.6(14) . . ? C10S C11S C12S 118.4(14) . . ? C11S C12S C7S 121.0(13) . . ? C14S C13S C18S 119.7(13) . . ? C15S C14S C13S 118.8(13) . . ? C14S C15S C16S 119.7(12) . . ? C17S C16S C15S 121.9(13) . . ? C18S C17S C16S 117.7(13) . . ? C17S C18S C13S 122.1(13) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.085 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.120 #===END data_4b+K _database_code_depnum_ccdc_archive 'CCDC 780041' #TrackingRef 'all-CIFs-revised.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H100 Cl2 K2 O32' _chemical_formula_weight 1626.62 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' 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' K K 0.2009 0.2494 '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 13.9879(9) _cell_length_b 26.9584(19) _cell_length_c 21.0031(15) _cell_angle_alpha 90.00 _cell_angle_beta 103.011(4) _cell_angle_gamma 90.00 _cell_volume 7716.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 120.0(2) _cell_measurement_reflns_used 2348 _cell_measurement_theta_min 2.329 _cell_measurement_theta_max 27.142 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3440 _exptl_absorpt_coefficient_mu 0.279 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120.0(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-6K' _diffrn_measurement_method /W _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43634 _diffrn_reflns_av_R_equivalents 0.1790 _diffrn_reflns_av_sigmaI/netI 0.1732 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 29.00 _reflns_number_total 10251 _reflns_number_gt 4619 _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 ; The oxygen atoms of three solvate water molecules, O(2W), O(3W), and O(4W), have position occupancies of 0.25, 0.50, and 0.25, respectively. The ISOR command was applied to atom O(12) of perchlorate anion, to atoms C(10), C(11), C(12), C(13) of one of two independent crown-ether fragments, and to atom O(4W) of solvate water molecule to avoid N.P.D. for their thermal anisotropic displacement parameters. 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^)+(0.1360P)^2^+11.4871P] 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 10251 _refine_ls_number_parameters 501 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.2154 _refine_ls_R_factor_gt 0.1020 _refine_ls_wR_factor_ref 0.3110 _refine_ls_wR_factor_gt 0.2778 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.078 _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 K1 K 0.65655(9) 0.61971(4) 0.59476(6) 0.0237(3) Uani 1 1 d . . . Cl1 Cl 0.20202(12) 0.66262(7) 0.32461(9) 0.0437(5) Uani 1 1 d . . . O11 O 0.2210(4) 0.6750(2) 0.2627(3) 0.0596(15) Uani 1 1 d . . . O12 O 0.1050(5) 0.6446(4) 0.3181(4) 0.099(3) Uani 1 1 d U . . O13 O 0.2719(5) 0.6279(2) 0.3563(3) 0.0727(19) Uani 1 1 d . . . O14 O 0.2126(5) 0.7077(2) 0.3620(3) 0.0727(18) Uani 1 1 d . . . O1 O 0.7073(3) 0.53664(15) 0.51143(18) 0.0272(9) Uani 1 1 d . . . O2 O 0.7838(4) 0.5287(2) 0.6409(2) 0.0455(13) Uani 1 1 d . . . O3 O 0.6222(4) 0.55971(19) 0.6930(2) 0.0502(14) Uani 1 1 d . . . O4 O 0.4544(3) 0.59665(17) 0.5900(2) 0.0362(11) Uani 1 1 d . . . O5 O 0.5325(3) 0.56751(15) 0.48615(18) 0.0253(9) Uani 1 1 d . . . O6 O 0.5686(3) 0.71273(15) 0.54513(17) 0.0247(9) Uani 1 1 d . . . O7 O 0.5653(3) 0.68938(15) 0.67206(18) 0.0248(9) Uani 1 1 d . . . O8 O 0.7741(3) 0.66586(14) 0.70203(18) 0.0246(9) Uani 1 1 d . . . O9 O 0.8552(3) 0.63490(14) 0.59249(18) 0.0248(9) Uani 1 1 d . . . O10 O 0.7217(3) 0.69151(14) 0.50684(17) 0.0219(8) Uani 1 1 d . . . C1 C 0.5547(4) 0.6261(2) 0.2669(2) 0.0225(12) Uani 1 1 d . . . H1A H 0.5939 0.6184 0.2337 0.027 Uiso 1 1 calc R . . C2 C 0.5930(4) 0.5957(2) 0.3266(3) 0.0216(12) Uani 1 1 d . . . C3 C 0.6882(4) 0.5775(2) 0.3408(3) 0.0250(12) Uani 1 1 d . . . H3A H 0.7260 0.5793 0.3085 0.030 Uiso 1 1 calc R . . C4 C 0.7297(5) 0.5566(2) 0.4016(3) 0.0263(13) Uani 1 1 d . . . H4A H 0.7948 0.5440 0.4103 0.032 Uiso 1 1 calc R . . C5 C 0.6754(4) 0.55439(19) 0.4488(3) 0.0233(12) Uani 1 1 d . . . C6 C 0.5780(4) 0.57150(19) 0.4350(3) 0.0202(11) Uani 1 1 d . . . C7 C 0.5372(4) 0.5908(2) 0.3744(3) 0.0211(11) Uani 1 1 d . . . H7A H 0.4704 0.6008 0.3645 0.025 Uiso 1 1 calc R . . C8 C 0.8078(5) 0.5217(2) 0.5329(3) 0.0282(13) Uani 1 1 d . . . H8A H 0.8518 0.5509 0.5389 0.034 Uiso 1 1 calc R . . H8B H 0.8268 0.4990 0.5008 0.034 Uiso 1 1 calc R . . C9 C 0.8128(5) 0.4956(3) 0.5972(3) 0.0355(15) Uani 1 1 d . . . H9A H 0.7689 0.4663 0.5904 0.043 Uiso 1 1 calc R . . H9B H 0.8806 0.4840 0.6154 0.043 Uiso 1 1 calc R . . C10 C 0.7545(7) 0.5015(4) 0.6919(4) 0.067(3) Uani 1 1 d U . . H10A H 0.7087 0.4747 0.6725 0.080 Uiso 1 1 calc R . . H10B H 0.8129 0.4859 0.7204 0.080 Uiso 1 1 calc R . . C11 C 0.7089(8) 0.5327(4) 0.7291(5) 0.074(3) Uani 1 1 d U . . H11A H 0.7577 0.5573 0.7514 0.089 Uiso 1 1 calc R . . H11B H 0.6891 0.5125 0.7634 0.089 Uiso 1 1 calc R . . C12 C 0.5347(8) 0.5346(3) 0.6700(4) 0.064(2) Uani 1 1 d U . . H12A H 0.5210 0.5124 0.7045 0.077 Uiso 1 1 calc R . . H12B H 0.5392 0.5141 0.6317 0.077 Uiso 1 1 calc R . . C13 C 0.4530(6) 0.5727(4) 0.6509(3) 0.056(2) Uani 1 1 d U . . H13A H 0.3889 0.5561 0.6473 0.067 Uiso 1 1 calc R . . H13B H 0.4599 0.5981 0.6857 0.067 Uiso 1 1 calc R . . C14 C 0.3989(5) 0.5698(3) 0.5357(3) 0.0350(15) Uani 1 1 d . . . H14A H 0.3283 0.5777 0.5298 0.042 Uiso 1 1 calc R . . H14B H 0.4076 0.5337 0.5438 0.042 Uiso 1 1 calc R . . C15 C 0.4330(4) 0.5836(2) 0.4757(3) 0.0274(13) Uani 1 1 d . . . H15A H 0.3922 0.5671 0.4369 0.033 Uiso 1 1 calc R . . H15B H 0.4286 0.6200 0.4689 0.033 Uiso 1 1 calc R . . C16 C 0.5505(4) 0.6850(2) 0.2756(2) 0.0209(12) Uani 1 1 d . . . H16A H 0.6030 0.7025 0.2590 0.025 Uiso 1 1 calc R . . C17 C 0.5491(4) 0.69977(19) 0.3455(2) 0.0188(11) Uani 1 1 d . . . C18 C 0.4646(4) 0.7122(2) 0.3669(3) 0.0217(12) Uani 1 1 d . . . H18A H 0.4044 0.7169 0.3359 0.026 Uiso 1 1 calc R . . C19 C 0.4679(4) 0.7177(2) 0.4335(3) 0.0205(11) Uani 1 1 d . . . H19A H 0.4104 0.7266 0.4477 0.025 Uiso 1 1 calc R . . C20 C 0.5546(4) 0.71009(19) 0.4782(2) 0.0181(11) Uani 1 1 d . . . C21 C 0.6406(4) 0.69865(19) 0.4574(3) 0.0203(11) Uani 1 1 d . . . C22 C 0.6376(4) 0.6945(2) 0.3914(3) 0.0210(11) Uani 1 1 d . . . H22A H 0.6962 0.6881 0.3771 0.025 Uiso 1 1 calc R . . C23 C 0.4874(4) 0.7280(2) 0.5728(3) 0.0239(12) Uani 1 1 d . . . H23A H 0.4363 0.7020 0.5665 0.029 Uiso 1 1 calc R . . H23B H 0.4578 0.7590 0.5521 0.029 Uiso 1 1 calc R . . C24 C 0.5306(5) 0.7360(2) 0.6441(3) 0.0292(13) Uani 1 1 d . . . H24A H 0.5855 0.7600 0.6499 0.035 Uiso 1 1 calc R . . H24B H 0.4802 0.7494 0.6658 0.035 Uiso 1 1 calc R . . C25 C 0.6297(5) 0.6945(3) 0.7347(3) 0.0324(15) Uani 1 1 d . . . H25A H 0.6297 0.6631 0.7592 0.039 Uiso 1 1 calc R . . H25B H 0.6044 0.7210 0.7592 0.039 Uiso 1 1 calc R . . C26 C 0.7325(5) 0.7067(2) 0.7319(3) 0.0293(13) Uani 1 1 d . . . H26A H 0.7334 0.7373 0.7059 0.035 Uiso 1 1 calc R . . H26B H 0.7722 0.7127 0.7765 0.035 Uiso 1 1 calc R . . C27 C 0.8716(4) 0.6763(2) 0.6977(3) 0.0281(13) Uani 1 1 d . . . H27A H 0.9147 0.6779 0.7421 0.034 Uiso 1 1 calc R . . H27B H 0.8743 0.7087 0.6761 0.034 Uiso 1 1 calc R . . C28 C 0.9061(4) 0.6363(2) 0.6593(3) 0.0278(13) Uani 1 1 d . . . H28A H 0.9769 0.6411 0.6615 0.033 Uiso 1 1 calc R . . H28B H 0.8981 0.6039 0.6797 0.033 Uiso 1 1 calc R . . C29 C 0.8864(4) 0.6731(2) 0.5536(3) 0.0236(12) Uani 1 1 d . . . H29A H 0.9514 0.6646 0.5455 0.028 Uiso 1 1 calc R . . H29B H 0.8920 0.7051 0.5772 0.028 Uiso 1 1 calc R . . C30 C 0.8127(4) 0.6772(2) 0.4905(3) 0.0214(11) Uani 1 1 d . . . H30A H 0.8334 0.7025 0.4621 0.026 Uiso 1 1 calc R . . H30B H 0.8052 0.6450 0.4672 0.026 Uiso 1 1 calc R . . C1S C 0.1791(7) 0.6241(3) 0.6220(4) 0.060(2) Uani 1 1 d . . . H1SA H 0.2009 0.6246 0.6683 0.072 Uiso 1 1 calc R . . C2S C 0.2092(8) 0.6590(4) 0.5852(5) 0.071(3) Uani 1 1 d . . . H2SA H 0.2513 0.6844 0.6067 0.085 Uiso 1 1 calc R . . C3S C 0.1825(8) 0.6597(4) 0.5185(5) 0.074(3) Uani 1 1 d . . . H3SA H 0.2078 0.6837 0.4936 0.089 Uiso 1 1 calc R . . C4S C 0.1166(8) 0.6238(5) 0.4892(5) 0.080(3) Uani 1 1 d . . . H4SA H 0.0944 0.6239 0.4430 0.096 Uiso 1 1 calc R . . C5S C 0.0819(8) 0.5876(4) 0.5252(6) 0.077(3) Uani 1 1 d . . . H5SA H 0.0359 0.5634 0.5044 0.092 Uiso 1 1 calc R . . C6S C 0.1164(7) 0.5878(4) 0.5918(5) 0.063(2) Uani 1 1 d . . . H6SA H 0.0964 0.5624 0.6174 0.076 Uiso 1 1 calc R . . O1W O -0.0791(8) 0.6336(5) 0.3456(6) 0.168(5) Uani 1 1 d . . . O2W O 1.0000 0.5146(8) 0.7500 0.120(9) Uani 0.50 2 d SP . . O3W O -0.0626(8) 0.5316(6) 0.3455(8) 0.088(5) Uani 0.50 1 d P A 1 O4W O -0.0243(17) 0.5677(8) 0.2876(12) 0.068(6) Uani 0.25 1 d PU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0263(7) 0.0219(6) 0.0215(6) 0.0001(5) 0.0020(5) -0.0030(5) Cl1 0.0272(9) 0.0486(11) 0.0535(11) 0.0179(9) 0.0051(7) -0.0019(8) O11 0.064(4) 0.062(4) 0.056(3) 0.016(3) 0.020(3) 0.004(3) O12 0.042(4) 0.164(7) 0.086(5) 0.018(5) 0.007(3) -0.037(4) O13 0.064(4) 0.049(4) 0.091(5) 0.025(3) -0.015(3) 0.011(3) O14 0.077(5) 0.064(4) 0.082(5) 0.000(3) 0.026(4) 0.016(3) O1 0.033(2) 0.024(2) 0.021(2) 0.0055(16) -0.0017(17) 0.0039(18) O2 0.048(3) 0.062(3) 0.027(2) 0.011(2) 0.010(2) -0.001(3) O3 0.070(4) 0.044(3) 0.042(3) 0.023(2) 0.025(3) 0.020(3) O4 0.039(3) 0.045(3) 0.026(2) -0.010(2) 0.0123(19) -0.013(2) O5 0.028(2) 0.025(2) 0.022(2) 0.0049(16) 0.0043(16) 0.0016(17) O6 0.025(2) 0.034(2) 0.0152(18) 0.0009(16) 0.0047(15) 0.0033(18) O7 0.025(2) 0.030(2) 0.0179(19) 0.0003(16) 0.0007(16) -0.0023(17) O8 0.024(2) 0.025(2) 0.025(2) -0.0038(16) 0.0039(16) -0.0035(17) O9 0.026(2) 0.024(2) 0.023(2) 0.0003(16) 0.0012(16) -0.0016(17) O10 0.019(2) 0.031(2) 0.0157(18) -0.0006(15) 0.0031(15) 0.0034(17) C1 0.028(3) 0.026(3) 0.014(2) 0.002(2) 0.005(2) 0.001(2) C2 0.024(3) 0.020(3) 0.022(3) -0.001(2) 0.007(2) 0.000(2) C3 0.026(3) 0.024(3) 0.024(3) -0.002(2) 0.004(2) 0.000(2) C4 0.028(3) 0.023(3) 0.027(3) -0.002(2) 0.005(2) 0.007(2) C5 0.029(3) 0.013(3) 0.023(3) 0.000(2) -0.004(2) -0.001(2) C6 0.025(3) 0.016(3) 0.019(3) 0.000(2) 0.005(2) -0.001(2) C7 0.021(3) 0.021(3) 0.020(3) 0.001(2) 0.001(2) 0.003(2) C8 0.030(3) 0.025(3) 0.023(3) -0.002(2) -0.006(2) 0.007(3) C9 0.024(3) 0.040(4) 0.036(4) 0.012(3) -0.005(3) 0.000(3) C10 0.056(5) 0.099(6) 0.050(4) 0.036(4) 0.023(4) 0.024(5) C11 0.097(7) 0.066(5) 0.057(5) 0.020(4) 0.012(5) 0.019(5) C12 0.110(7) 0.048(4) 0.036(4) 0.004(3) 0.019(4) -0.027(5) C13 0.047(4) 0.099(6) 0.027(3) -0.013(4) 0.018(3) -0.030(4) C14 0.035(4) 0.044(4) 0.028(3) -0.007(3) 0.013(3) -0.017(3) C15 0.024(3) 0.034(3) 0.023(3) 0.000(2) 0.002(2) -0.005(3) C16 0.026(3) 0.021(3) 0.015(3) 0.002(2) 0.002(2) -0.002(2) C17 0.026(3) 0.016(3) 0.015(2) 0.003(2) 0.006(2) -0.003(2) C18 0.019(3) 0.019(3) 0.024(3) 0.003(2) -0.004(2) -0.001(2) C19 0.022(3) 0.019(3) 0.021(3) -0.001(2) 0.004(2) 0.001(2) C20 0.021(3) 0.018(3) 0.015(2) 0.002(2) 0.005(2) -0.001(2) C21 0.026(3) 0.014(2) 0.019(3) 0.002(2) 0.001(2) -0.002(2) C22 0.023(3) 0.020(3) 0.020(3) 0.000(2) 0.004(2) 0.000(2) C23 0.020(3) 0.028(3) 0.026(3) 0.004(2) 0.010(2) 0.006(2) C24 0.039(4) 0.024(3) 0.025(3) 0.003(2) 0.008(3) 0.003(3) C25 0.038(4) 0.045(4) 0.014(3) -0.002(3) 0.006(2) 0.002(3) C26 0.030(3) 0.031(3) 0.026(3) -0.005(2) 0.002(2) -0.006(3) C27 0.028(3) 0.028(3) 0.026(3) -0.003(2) 0.001(2) -0.002(3) C28 0.021(3) 0.031(3) 0.029(3) 0.006(3) 0.001(2) 0.001(3) C29 0.024(3) 0.022(3) 0.026(3) 0.001(2) 0.008(2) 0.001(2) C30 0.022(3) 0.019(3) 0.023(3) 0.001(2) 0.006(2) 0.000(2) C1S 0.068(6) 0.065(6) 0.045(5) 0.006(4) 0.011(4) 0.010(5) C2S 0.080(7) 0.071(6) 0.057(6) -0.004(5) 0.010(5) 0.012(5) C3S 0.075(7) 0.096(8) 0.053(6) 0.006(5) 0.017(5) 0.035(6) C4S 0.063(7) 0.113(9) 0.060(6) -0.019(6) 0.003(5) 0.055(7) C5S 0.059(6) 0.079(7) 0.086(8) -0.034(6) 0.005(5) 0.029(6) C6S 0.059(6) 0.059(6) 0.076(7) 0.002(5) 0.027(5) 0.014(5) O1W 0.108(8) 0.220(13) 0.169(11) 0.041(9) 0.015(7) -0.052(8) O2W 0.095(18) 0.047(12) 0.22(3) 0.000 0.046(19) 0.000 O3W 0.025(7) 0.101(11) 0.133(13) 0.012(9) 0.006(7) 0.008(7) O4W 0.054(9) 0.040(8) 0.090(10) 0.020(8) -0.025(8) -0.026(7) _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 K1 O3 2.748(5) . ? K1 O8 2.768(4) . ? K1 O9 2.820(4) . ? K1 O4 2.875(5) . ? K1 O6 2.883(4) . ? K1 O5 2.900(4) . ? K1 O7 2.954(4) . ? K1 O10 2.957(4) . ? K1 O1 3.024(4) . ? K1 O2 3.058(5) . ? K1 C12 3.447(8) . ? K1 C28 3.477(6) . ? Cl1 O13 1.408(6) . ? Cl1 O12 1.419(6) . ? Cl1 O11 1.425(6) . ? Cl1 O14 1.437(7) . ? O1 C5 1.376(6) . ? O1 C8 1.434(7) . ? O2 C9 1.404(8) . ? O2 C10 1.432(9) . ? O3 C12 1.386(10) . ? O3 C11 1.471(11) . ? O4 C14 1.424(7) . ? O4 C13 1.437(8) . ? O5 C6 1.369(6) . ? O5 C15 1.428(7) . ? O6 C20 1.378(6) . ? O6 C23 1.447(6) . ? O7 C25 1.425(7) . ? O7 C24 1.425(7) . ? O8 C27 1.416(7) . ? O8 C26 1.452(7) . ? O9 C28 1.424(7) . ? O9 C29 1.440(7) . ? O10 C21 1.368(6) . ? O10 C30 1.444(7) . ? C1 C2 1.492(7) . ? C1 C1 1.535(11) 2_655 ? C1 C16 1.601(8) . ? C2 C3 1.388(8) . ? C2 C7 1.410(7) . ? C3 C4 1.397(8) . ? C4 C5 1.381(8) . ? C5 C6 1.405(8) . ? C6 C7 1.376(7) . ? C8 C9 1.512(8) . ? C10 C11 1.398(12) . ? C12 C13 1.523(13) . ? C14 C15 1.492(8) . ? C16 C17 1.526(7) . ? C16 C16 1.571(11) 2_655 ? C17 C22 1.393(8) . ? C17 C18 1.397(8) . ? C18 C19 1.396(7) . ? C19 C20 1.372(8) . ? C20 C21 1.403(8) . ? C21 C22 1.383(7) . ? C23 C24 1.499(8) . ? C25 C26 1.490(9) . ? C27 C28 1.489(8) . ? C29 C30 1.490(8) . ? C1S C2S 1.344(13) . ? C1S C6S 1.370(13) . ? C2S C3S 1.366(13) . ? C3S C4S 1.382(16) . ? C4S C5S 1.387(16) . ? C5S C6S 1.374(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 K1 O8 79.97(16) . . ? O3 K1 O9 115.97(15) . . ? O8 K1 O9 62.70(11) . . ? O3 K1 O4 64.01(16) . . ? O8 K1 O4 121.66(12) . . ? O9 K1 O4 174.96(13) . . ? O3 K1 O6 130.62(13) . . ? O8 K1 O6 91.73(12) . . ? O9 K1 O6 102.09(12) . . ? O4 K1 O6 80.75(13) . . ? O3 K1 O5 97.47(15) . . ? O8 K1 O5 177.38(12) . . ? O9 K1 O5 118.32(12) . . ? O4 K1 O5 57.20(11) . . ? O6 K1 O5 90.39(11) . . ? O3 K1 O7 77.96(13) . . ? O8 K1 O7 61.17(11) . . ? O9 K1 O7 117.80(11) . . ? O4 K1 O7 67.24(12) . . ? O6 K1 O7 56.20(10) . . ? O5 K1 O7 119.00(12) . . ? O3 K1 O10 169.98(16) . . ? O8 K1 O10 90.22(11) . . ? O9 K1 O10 56.69(11) . . ? O4 K1 O10 123.98(13) . . ? O6 K1 O10 51.04(10) . . ? O5 K1 O10 92.31(11) . . ? O7 K1 O10 99.16(11) . . ? O3 K1 O1 95.86(13) . . ? O8 K1 O1 129.07(12) . . ? O9 K1 O1 74.76(11) . . ? O4 K1 O1 100.19(12) . . ? O6 K1 O1 124.87(11) . . ? O5 K1 O1 50.36(11) . . ? O7 K1 O1 167.39(12) . . ? O10 K1 O1 88.73(11) . . ? O3 K1 O2 58.50(14) . . ? O8 K1 O2 84.62(13) . . ? O9 K1 O2 67.44(12) . . ? O4 K1 O2 109.59(14) . . ? O6 K1 O2 169.45(13) . . ? O5 K1 O2 93.56(13) . . ? O7 K1 O2 128.96(12) . . ? O10 K1 O2 118.93(12) . . ? O1 K1 O2 52.64(11) . . ? O3 K1 C12 22.42(19) . . ? O8 K1 C12 100.97(17) . . ? O9 K1 C12 134.0(2) . . ? O4 K1 C12 44.6(2) . . ? O6 K1 C12 122.0(2) . . ? O5 K1 C12 76.58(17) . . ? O7 K1 C12 81.47(18) . . ? O10 K1 C12 167.38(18) . . ? O1 K1 C12 88.69(17) . . ? O2 K1 C12 68.5(2) . . ? O3 K1 C28 96.49(16) . . ? O8 K1 C28 42.65(13) . . ? O9 K1 C28 23.27(12) . . ? O4 K1 C28 159.15(14) . . ? O6 K1 C28 109.76(13) . . ? O5 K1 C28 137.67(13) . . ? O7 K1 C28 102.94(13) . . ? O10 K1 C28 74.67(13) . . ? O1 K1 C28 88.58(13) . . ? O2 K1 C28 61.20(14) . . ? C12 K1 C28 117.6(2) . . ? O13 Cl1 O12 111.3(5) . . ? O13 Cl1 O11 109.6(4) . . ? O12 Cl1 O11 111.3(4) . . ? O13 Cl1 O14 109.3(4) . . ? O12 Cl1 O14 108.8(5) . . ? O11 Cl1 O14 106.4(4) . . ? C5 O1 C8 118.8(4) . . ? C5 O1 K1 103.2(3) . . ? C8 O1 K1 111.6(3) . . ? C9 O2 C10 109.6(6) . . ? C9 O2 K1 122.5(3) . . ? C10 O2 K1 113.8(4) . . ? C12 O3 C11 119.9(7) . . ? C12 O3 K1 108.5(4) . . ? C11 O3 K1 114.6(5) . . ? C14 O4 C13 111.7(5) . . ? C14 O4 K1 119.5(3) . . ? C13 O4 K1 106.1(4) . . ? C6 O5 C15 117.7(4) . . ? C6 O5 K1 106.1(3) . . ? C15 O5 K1 111.3(3) . . ? C20 O6 C23 118.7(4) . . ? C20 O6 K1 106.0(3) . . ? C23 O6 K1 114.3(3) . . ? C25 O7 C24 112.4(5) . . ? C25 O7 K1 107.9(3) . . ? C24 O7 K1 118.9(3) . . ? C27 O8 C26 111.3(4) . . ? C27 O8 K1 116.2(3) . . ? C26 O8 K1 118.0(3) . . ? C28 O9 C29 113.1(4) . . ? C28 O9 K1 105.2(3) . . ? C29 O9 K1 122.6(3) . . ? C21 O10 C30 118.8(4) . . ? C21 O10 K1 104.3(3) . . ? C30 O10 K1 112.7(3) . . ? C2 C1 C1 121.3(5) . 2_655 ? C2 C1 C16 117.6(4) . . ? C1 C1 C16 89.7(3) 2_655 . ? C3 C2 C7 118.2(5) . . ? C3 C2 C1 121.4(5) . . ? C7 C2 C1 119.9(5) . . ? C2 C3 C4 121.3(5) . . ? C5 C4 C3 119.5(6) . . ? O1 C5 C4 126.1(5) . . ? O1 C5 C6 113.7(5) . . ? C4 C5 C6 120.2(5) . . ? O5 C6 C7 125.9(5) . . ? O5 C6 C5 114.4(5) . . ? C7 C6 C5 119.7(5) . . ? O5 C6 K1 52.0(3) . . ? C7 C6 K1 135.7(4) . . ? C5 C6 K1 81.1(3) . . ? C6 C7 C2 121.0(5) . . ? O1 C8 C9 104.8(5) . . ? O2 C9 C8 109.0(5) . . ? C11 C10 O2 110.7(8) . . ? C10 C11 O3 115.9(8) . . ? O3 C12 C13 108.3(7) . . ? O3 C12 K1 49.1(3) . . ? C13 C12 K1 81.3(4) . . ? O4 C13 C12 112.2(6) . . ? O4 C14 C15 109.2(5) . . ? O5 C15 C14 106.3(5) . . ? C17 C16 C16 117.0(6) . 2_655 ? C17 C16 C1 112.2(4) . . ? C16 C16 C1 88.4(3) 2_655 . ? C22 C17 C18 119.1(5) . . ? C22 C17 C16 115.9(5) . . ? C18 C17 C16 124.5(5) . . ? C19 C18 C17 120.5(5) . . ? C20 C19 C18 119.6(5) . . ? C19 C20 O6 126.3(5) . . ? C19 C20 C21 120.6(5) . . ? O6 C20 C21 113.2(5) . . ? C19 C20 K1 137.4(4) . . ? O6 C20 K1 51.9(2) . . ? C21 C20 K1 79.8(3) . . ? O10 C21 C22 125.6(5) . . ? O10 C21 C20 114.7(4) . . ? C22 C21 C20 119.6(5) . . ? C21 C22 C17 120.4(5) . . ? O6 C23 C24 105.4(5) . . ? O7 C24 C23 107.9(5) . . ? O7 C25 C26 113.6(5) . . ? O8 C26 C25 109.5(5) . . ? O8 C27 C28 109.0(5) . . ? O9 C28 C27 113.8(5) . . ? O9 C28 K1 51.5(3) . . ? C27 C28 K1 83.4(3) . . ? O9 C29 C30 108.8(5) . . ? O10 C30 C29 106.1(4) . . ? C2S C1S C6S 118.9(9) . . ? C1S C2S C3S 123.5(11) . . ? C2S C3S C4S 116.6(11) . . ? C3S C4S C5S 122.1(10) . . ? C6S C5S C4S 117.8(10) . . ? C1S C6S C5S 121.1(10) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.388 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.108