# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Philip Coppens' 'Marc Messerschmidt' 'Shao-Liang Zheng.' _publ_contact_author_name 'Philip Coppens' _publ_contact_author_address ; Department of Chemistry State University of New York at Buffalo Buffalo New York 14260-3000 UNITED STATES OF AMERICA ; _publ_contact_author_email 'COPPENS@ACSU.BUFFALO.EDU' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Single-crystal-to-single-crystal E->Z and Z->E isomerizations of 3-Chloro-acrylic acid within the nanocavities of a supramolecular framework ; #============================================================ data_CECR-E-HClA-2MeOH-1.5H2O@90k _database_code_depnum_ccdc_archive 'CCDC 629568' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CECR-E-HClA-2MeOH-1.5H2O@90k _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C41 H54 Cl O13.50' _chemical_formula_weight 798.29 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3821(5) _cell_length_b 13.2720(5) _cell_length_c 14.5631(6) _cell_angle_alpha 99.0020(12) _cell_angle_beta 108.7610(11) _cell_angle_gamma 95.1928(12) _cell_volume 2033.94(14) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 865 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.9749 _exptl_absorpt_correction_T_max 0.9842 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26025 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7170 _reflns_number_gt 6141 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+2.3738P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7170 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1422 _refine_ls_wR_factor_gt 0.1351 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 O1 O 0.79560(14) 0.60415(13) 0.57907(11) 0.0159(3) Uani 1 1 d . . . O2 O 0.42052(14) 0.60361(12) 0.31379(12) 0.0166(3) Uani 1 1 d . . . O3 O 0.32007(14) 0.65539(13) 0.13221(12) 0.0169(3) Uani 1 1 d . . . O4 O 0.54788(15) 0.61421(12) -0.09572(11) 0.0184(3) Uani 1 1 d . . . O5 O 0.77449(15) 0.54168(12) -0.03640(11) 0.0179(3) Uani 1 1 d . . . O6 O 1.14278(14) 0.54125(13) 0.23520(12) 0.0189(3) Uani 1 1 d . . . O7 O 1.28799(14) 0.59634(11) 0.44273(12) 0.0165(3) Uani 1 1 d . . . O8 O 1.05166(16) 0.63134(12) 0.65330(11) 0.0185(3) Uani 1 1 d . . . C1 C 0.78239(19) 0.74386(16) 0.49450(15) 0.0130(4) Uani 1 1 d . . . C2 C 0.72656(19) 0.65010(16) 0.50524(15) 0.0132(4) Uani 1 1 d . . . C3 C 0.60648(19) 0.60522(16) 0.44414(15) 0.0140(4) Uani 1 1 d . . . H3A H 0.5702 0.5416 0.4526 0.017 Uiso 1 1 calc R . . C4 C 0.53927(19) 0.65388(16) 0.37018(15) 0.0135(4) Uani 1 1 d . . . C5 C 0.59005(19) 0.74834(15) 0.35695(15) 0.0129(4) Uani 1 1 d . . . C6 C 0.71172(19) 0.79031(15) 0.42037(15) 0.0131(4) Uani 1 1 d . . . H6A H 0.7481 0.8542 0.4123 0.016 Uiso 1 1 calc R . . C7 C 0.51642(19) 0.80077(15) 0.27493(15) 0.0135(4) Uani 1 1 d . . . H7A H 0.4264 0.7881 0.2699 0.016 Uiso 1 1 calc R . . C8 C 0.52309(19) 0.75080(15) 0.17504(15) 0.0132(4) Uani 1 1 d . . . C9 C 0.42365(19) 0.67978(16) 0.10600(15) 0.0145(4) Uani 1 1 d . . . C10 C 0.4298(2) 0.63466(16) 0.01521(15) 0.0159(4) Uani 1 1 d . . . H10A H 0.3608 0.5875 -0.0312 0.019 Uiso 1 1 calc R . . C11 C 0.5373(2) 0.65879(16) -0.00739(15) 0.0148(4) Uani 1 1 d . . . C12 C 0.63960(19) 0.72893(15) 0.05953(15) 0.0139(4) Uani 1 1 d . . . C13 C 0.62943(19) 0.77234(15) 0.14950(15) 0.0135(4) Uani 1 1 d . . . H13A H 0.6986 0.8192 0.1960 0.016 Uiso 1 1 calc R . . C14 C 0.75795(19) 0.75642(16) 0.03496(15) 0.0146(4) Uani 1 1 d . . . H14A H 0.7362 0.7296 -0.0375 0.017 Uiso 1 1 calc R . . C15 C 0.86256(19) 0.69983(16) 0.08778(15) 0.0134(4) Uani 1 1 d . . . C16 C 0.86353(19) 0.59626(16) 0.05024(15) 0.0144(4) Uani 1 1 d . . . C17 C 0.9561(2) 0.54235(16) 0.09815(15) 0.0156(4) Uani 1 1 d . . . H17A H 0.9548 0.4721 0.0713 0.019 Uiso 1 1 calc R . . C18 C 1.05042(19) 0.59138(16) 0.18538(15) 0.0146(4) Uani 1 1 d . . . C19 C 1.05408(19) 0.69506(16) 0.22602(15) 0.0127(4) Uani 1 1 d . . . C20 C 0.95931(19) 0.74630(16) 0.17564(15) 0.0132(4) Uani 1 1 d . . . H20A H 0.9606 0.8166 0.2025 0.016 Uiso 1 1 calc R . . C21 C 1.15903(19) 0.74461(15) 0.32214(15) 0.0130(4) Uani 1 1 d . . . H21A H 1.2359 0.7151 0.3195 0.016 Uiso 1 1 calc R . . C22 C 1.13103(19) 0.71386(15) 0.41089(15) 0.0133(4) Uani 1 1 d . . . C23 C 1.19416(19) 0.64409(16) 0.46388(15) 0.0141(4) Uani 1 1 d . . . C24 C 1.1655(2) 0.61762(16) 0.54334(16) 0.0162(4) Uani 1 1 d . . . H24A H 1.2087 0.5694 0.5778 0.019 Uiso 1 1 calc R . . C25 C 1.07409(19) 0.66129(16) 0.57267(15) 0.0147(4) Uani 1 1 d . . . C26 C 1.01093(19) 0.73354(15) 0.52462(15) 0.0131(4) Uani 1 1 d . . . C27 C 1.03965(19) 0.75589(15) 0.44313(15) 0.0127(4) Uani 1 1 d . . . H27A H 0.9944 0.8024 0.4075 0.015 Uiso 1 1 calc R . . C28 C 0.91619(19) 0.78782(16) 0.56086(15) 0.0138(4) Uani 1 1 d . . . H28A H 0.9256 0.7715 0.6274 0.017 Uiso 1 1 calc R . . C29 C 0.5556(2) 0.91870(16) 0.29748(16) 0.0155(4) Uani 1 1 d . . . H29A H 0.5543 0.9473 0.3641 0.019 Uiso 1 1 calc R . . H29B H 0.6427 0.9342 0.2983 0.019 Uiso 1 1 calc R . . C30 C 0.4698(2) 0.97113(17) 0.22197(17) 0.0224(5) Uani 1 1 d . . . H30A H 0.4974 1.0459 0.2400 0.034 Uiso 1 1 calc R . . H30B H 0.3834 0.9562 0.2210 0.034 Uiso 1 1 calc R . . H30C H 0.4733 0.9451 0.1563 0.034 Uiso 1 1 calc R . . C31 C 0.7940(2) 0.87383(16) 0.05164(16) 0.0175(4) Uani 1 1 d . . . H31A H 0.8116 0.9044 0.1221 0.021 Uiso 1 1 calc R . . H31B H 0.8716 0.8893 0.0362 0.021 Uiso 1 1 calc R . . C32 C 0.6893(2) 0.92270(18) -0.01319(18) 0.0254(5) Uani 1 1 d . . . H32A H 0.7157 0.9973 -0.0017 0.038 Uiso 1 1 calc R . . H32B H 0.6133 0.9095 0.0036 0.038 Uiso 1 1 calc R . . H32C H 0.6718 0.8926 -0.0830 0.038 Uiso 1 1 calc R . . C33 C 1.1911(2) 0.86220(16) 0.33538(15) 0.0156(4) Uani 1 1 d . . . H33A H 1.2071 0.8784 0.2760 0.019 Uiso 1 1 calc R . . H33B H 1.1181 0.8947 0.3410 0.019 Uiso 1 1 calc R . . C34 C 1.3058(2) 0.90814(17) 0.42674(17) 0.0207(5) Uani 1 1 d . . . H34A H 1.3222 0.9830 0.4321 0.031 Uiso 1 1 calc R . . H34B H 1.3788 0.8775 0.4209 0.031 Uiso 1 1 calc R . . H34C H 1.2899 0.8934 0.4859 0.031 Uiso 1 1 calc R . . C35 C 0.9453(2) 0.90541(16) 0.57599(16) 0.0168(4) Uani 1 1 d . . . H35A H 0.9439 0.9245 0.5126 0.020 Uiso 1 1 calc R . . H35B H 0.8791 0.9368 0.5955 0.020 Uiso 1 1 calc R . . C36 C 1.0729(2) 0.94899(18) 0.65504(17) 0.0232(5) Uani 1 1 d . . . H36A H 1.0877 1.0241 0.6619 0.035 Uiso 1 1 calc R . . H36B H 1.1389 0.9188 0.6356 0.035 Uiso 1 1 calc R . . H36C H 1.0739 0.9320 0.7184 0.035 Uiso 1 1 calc R . . O1S O 0.88786(17) 0.14575(15) 0.06741(14) 0.0353(4) Uani 1 1 d . . . H1S H 0.8482 0.1884 0.1034 0.053 Uiso 1 1 d R . . C1S C 0.8676(3) 0.1737(2) -0.0268(2) 0.0389(7) Uani 1 1 d . . . H1S1 H 0.7865 0.1984 -0.0487 0.058 Uiso 1 1 calc R . . H1S2 H 0.8678 0.1133 -0.0751 0.058 Uiso 1 1 calc R . . H1S3 H 0.9347 0.2285 -0.0213 0.058 Uiso 1 1 calc R . . O2S O 0.77954(18) 0.26965(16) 0.16595(14) 0.0407(5) Uani 1 1 d . . . H2S H 0.8289 0.2908 0.2193 0.061 Uiso 1 1 d R . . C2S C 0.6778(3) 0.2172(3) 0.1852(2) 0.0456(7) Uani 1 1 d . . . H2S1 H 0.7107 0.1851 0.2426 0.068 Uiso 1 1 calc R . . H2S2 H 0.6292 0.1638 0.1274 0.068 Uiso 1 1 calc R . . H2S3 H 0.6237 0.2666 0.1989 0.068 Uiso 1 1 calc R . . O1W O 0.3331(9) 0.5301(8) 0.7666(7) 0.0453(14) Uani 0.30 1 d P A 1 H1WA H 0.2673 0.4808 0.7163 0.131 Uiso 0.30 1 d PR A 1 H1WB H 0.3207 0.5637 0.8269 0.131 Uiso 0.30 1 d PR A 1 O2W O 0.2347(2) 0.44834(18) 0.74184(17) 0.0143(5) Uani 0.60 1 d P B 2 H2WA H 0.1878 0.3893 0.7219 0.021 Uiso 0.60 1 d PR B 2 H2WB H 0.2391 0.4666 0.6882 0.021 Uiso 0.60 1 d PR B 2 O3W O 0.3580(2) 0.46328(17) 0.81085(17) 0.0116(5) Uani 0.60 1 d P C 3 H3WA H 0.2789 0.4525 0.8145 0.017 Uiso 0.60 1 d PR C 3 H3WB H 0.3591 0.4891 0.7611 0.017 Uiso 0.60 1 d PR C 3 H1O H 0.759(3) 0.552(3) 0.576(2) 0.039(9) Uiso 1 1 d . . . H2O H 0.393(3) 0.627(2) 0.263(2) 0.027(7) Uiso 1 1 d . . . H3O H 0.283(3) 0.609(2) 0.100(2) 0.021(8) Uiso 1 1 d . . . H40 H 0.484(3) 0.574(3) -0.128(2) 0.040(9) Uiso 1 1 d . . . H5O H 0.716(3) 0.572(2) -0.052(2) 0.037(9) Uiso 1 1 d . . . H6O H 1.133(3) 0.485(2) 0.211(2) 0.030(8) Uiso 1 1 d . . . H7O H 1.292(3) 0.604(2) 0.392(2) 0.024(7) Uiso 1 1 d . . . H8O H 0.979(3) 0.625(2) 0.643(2) 0.029(8) Uiso 1 1 d . . . O9 O 1.11774(18) 0.17061(14) 0.17454(15) 0.0354(4) Uani 1 1 d . . . H9O H 1.025(3) 0.161(2) 0.129(2) 0.029(7) Uiso 1 1 d . . . O10 O 1.10022(17) 0.33491(13) 0.16707(13) 0.0308(4) Uani 1 1 d . . . C41 C 1.1633(2) 0.26892(19) 0.19581(17) 0.0261(5) Uani 1 1 d . . . C42 C 1.2981(2) 0.2950(2) 0.25784(19) 0.0328(6) Uani 1 1 d . . . H42A H 1.3401 0.3632 0.2687 0.039 Uiso 1 1 calc R . . C43 C 1.3597(3) 0.2251(3) 0.2978(2) 0.0437(8) Uani 1 1 d . . . H43A H 1.3178 0.1563 0.2841 0.052 Uiso 1 1 calc R . . Cl1 Cl 1.51378(7) 0.25368(8) 0.37414(6) 0.0639(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0164(8) 0.0160(8) 0.0154(8) 0.0064(6) 0.0037(6) 0.0040(7) O2 0.0123(7) 0.0184(8) 0.0165(8) 0.0060(6) 0.0008(6) 0.0000(6) O3 0.0132(8) 0.0175(8) 0.0165(8) -0.0015(7) 0.0036(6) -0.0022(7) O4 0.0175(8) 0.0225(8) 0.0111(7) -0.0015(6) 0.0028(6) -0.0011(7) O5 0.0153(8) 0.0180(8) 0.0145(8) -0.0029(6) 0.0002(6) 0.0010(7) O6 0.0183(8) 0.0135(8) 0.0200(8) -0.0010(7) 0.0009(6) 0.0061(6) O7 0.0177(8) 0.0188(8) 0.0176(8) 0.0069(6) 0.0094(7) 0.0077(6) O8 0.0168(9) 0.0267(9) 0.0164(8) 0.0098(6) 0.0075(7) 0.0084(7) C1 0.0142(10) 0.0136(10) 0.0116(10) -0.0006(8) 0.0056(8) 0.0042(8) C2 0.0153(10) 0.0153(10) 0.0115(10) 0.0025(8) 0.0068(8) 0.0074(8) C3 0.0158(10) 0.0126(10) 0.0165(10) 0.0034(8) 0.0088(9) 0.0029(8) C4 0.0123(10) 0.0150(10) 0.0135(10) 0.0000(8) 0.0058(8) 0.0030(8) C5 0.0149(10) 0.0134(10) 0.0113(10) 0.0008(8) 0.0055(8) 0.0054(8) C6 0.0153(10) 0.0111(10) 0.0137(10) 0.0013(8) 0.0062(8) 0.0031(8) C7 0.0129(10) 0.0129(10) 0.0142(10) 0.0027(8) 0.0037(8) 0.0032(8) C8 0.0142(10) 0.0116(10) 0.0129(10) 0.0040(8) 0.0020(8) 0.0044(8) C9 0.0133(10) 0.0151(10) 0.0152(10) 0.0051(8) 0.0037(8) 0.0043(8) C10 0.0147(10) 0.0164(10) 0.0130(10) 0.0021(8) 0.0004(8) 0.0007(8) C11 0.0177(11) 0.0153(10) 0.0103(10) 0.0034(8) 0.0023(8) 0.0049(8) C12 0.0157(10) 0.0131(10) 0.0134(10) 0.0060(8) 0.0036(8) 0.0037(8) C13 0.0146(10) 0.0113(10) 0.0122(10) 0.0036(8) 0.0007(8) 0.0023(8) C14 0.0146(10) 0.0168(11) 0.0119(10) 0.0037(8) 0.0036(8) 0.0024(8) C15 0.0148(10) 0.0155(10) 0.0114(10) 0.0045(8) 0.0061(8) 0.0011(8) C16 0.0137(10) 0.0171(10) 0.0110(10) 0.0006(8) 0.0044(8) -0.0016(8) C17 0.0169(11) 0.0135(10) 0.0160(10) -0.0004(8) 0.0068(9) 0.0010(8) C18 0.0132(10) 0.0166(10) 0.0152(10) 0.0034(8) 0.0061(8) 0.0032(8) C19 0.0130(10) 0.0150(10) 0.0107(10) 0.0026(8) 0.0052(8) 0.0006(8) C20 0.0156(10) 0.0125(10) 0.0127(10) 0.0018(8) 0.0070(8) 0.0015(8) C21 0.0120(10) 0.0131(10) 0.0131(10) 0.0023(8) 0.0033(8) 0.0022(8) C22 0.0136(10) 0.0111(10) 0.0119(10) -0.0003(8) 0.0018(8) -0.0009(8) C23 0.0124(10) 0.0131(10) 0.0153(10) 0.0004(8) 0.0039(8) 0.0021(8) C24 0.0157(10) 0.0155(10) 0.0169(11) 0.0051(8) 0.0033(9) 0.0053(8) C25 0.0154(10) 0.0163(10) 0.0113(10) 0.0024(8) 0.0036(8) 0.0012(8) C26 0.0121(10) 0.0121(10) 0.0119(10) -0.0004(8) 0.0014(8) 0.0003(8) C27 0.0130(10) 0.0101(9) 0.0115(10) 0.0008(8) 0.0005(8) 0.0009(8) C28 0.0149(10) 0.0146(10) 0.0111(10) 0.0020(8) 0.0033(8) 0.0038(8) C29 0.0169(10) 0.0121(10) 0.0161(10) 0.0016(8) 0.0037(8) 0.0040(8) C30 0.0244(12) 0.0170(11) 0.0243(12) 0.0065(9) 0.0041(10) 0.0067(9) C31 0.0182(11) 0.0174(11) 0.0161(10) 0.0062(9) 0.0039(9) 0.0006(9) C32 0.0271(13) 0.0204(12) 0.0255(12) 0.0101(10) 0.0020(10) 0.0035(10) C33 0.0170(11) 0.0142(10) 0.0151(10) 0.0031(8) 0.0048(9) 0.0022(8) C34 0.0186(11) 0.0174(11) 0.0221(12) 0.0009(9) 0.0040(9) -0.0015(9) C35 0.0174(11) 0.0141(10) 0.0166(11) -0.0001(8) 0.0039(9) 0.0036(8) C36 0.0231(12) 0.0176(11) 0.0223(12) -0.0007(9) 0.0015(10) 0.0011(9) O1S 0.0327(10) 0.0372(10) 0.0322(10) 0.0045(8) 0.0089(8) -0.0022(8) C1S 0.0318(15) 0.0510(18) 0.0299(14) 0.0088(13) 0.0068(12) -0.0008(13) O2S 0.0326(10) 0.0561(13) 0.0259(10) 0.0024(9) 0.0044(8) -0.0010(9) C2S 0.0288(15) 0.066(2) 0.0423(17) 0.0160(15) 0.0092(13) 0.0073(14) O1W 0.054(3) 0.035(3) 0.020(2) 0.009(2) -0.017(2) -0.020(2) O2W 0.0136(12) 0.0175(12) 0.0110(11) 0.0057(9) 0.0023(10) 0.0003(10) O3W 0.0078(11) 0.0081(11) 0.0130(11) 0.0024(9) -0.0048(9) 0.0014(9) O9 0.0345(11) 0.0233(9) 0.0415(11) 0.0033(8) 0.0049(9) 0.0053(8) O10 0.0384(10) 0.0201(9) 0.0273(9) 0.0043(7) 0.0026(8) 0.0033(8) C41 0.0332(14) 0.0268(13) 0.0201(12) 0.0010(10) 0.0132(10) 0.0037(11) C42 0.0306(14) 0.0412(15) 0.0249(13) -0.0042(11) 0.0122(11) 0.0045(12) C43 0.0324(15) 0.0525(19) 0.0355(16) -0.0131(14) 0.0059(13) 0.0116(14) Cl1 0.0322(4) 0.0883(7) 0.0479(5) -0.0242(4) -0.0023(3) 0.0176(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 O1 C2 1.376(2) . ? O2 C4 1.378(3) . ? O3 C9 1.378(3) . ? O4 C11 1.376(3) . ? O5 C16 1.379(3) . ? O6 C18 1.364(3) . ? O7 C23 1.382(3) . ? O8 C25 1.387(3) . ? C1 C6 1.390(3) . ? C1 C2 1.399(3) . ? C1 C28 1.520(3) . ? C2 C3 1.385(3) . ? C3 C4 1.393(3) . ? C4 C5 1.400(3) . ? C5 C6 1.399(3) . ? C5 C7 1.528(3) . ? C7 C8 1.530(3) . ? C7 C29 1.541(3) . ? C8 C13 1.395(3) . ? C8 C9 1.400(3) . ? C9 C10 1.390(3) . ? C10 C11 1.389(3) . ? C11 C12 1.401(3) . ? C12 C13 1.391(3) . ? C12 C14 1.529(3) . ? C14 C15 1.525(3) . ? C14 C31 1.535(3) . ? C15 C20 1.398(3) . ? C15 C16 1.400(3) . ? C16 C17 1.389(3) . ? C17 C18 1.389(3) . ? C18 C19 1.402(3) . ? C19 C20 1.394(3) . ? C19 C21 1.521(3) . ? C21 C22 1.531(3) . ? C21 C33 1.537(3) . ? C22 C27 1.397(3) . ? C22 C23 1.399(3) . ? C23 C24 1.385(3) . ? C24 C25 1.385(3) . ? C25 C26 1.392(3) . ? C26 C27 1.395(3) . ? C26 C28 1.532(3) . ? C28 C35 1.532(3) . ? C29 C30 1.523(3) . ? C31 C32 1.530(3) . ? C33 C34 1.527(3) . ? C35 C36 1.528(3) . ? O1S C1S 1.431(3) . ? O2S C2S 1.424(4) . ? O9 C41 1.310(3) . ? O10 C41 1.222(3) . ? C41 C42 1.484(4) . ? C42 C43 1.309(4) . ? C43 Cl1 1.717(3) . ? 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 C6 C1 C2 117.08(19) . . ? C6 C1 C28 123.54(18) . . ? C2 C1 C28 119.35(18) . . ? O1 C2 C3 121.20(19) . . ? O1 C2 C1 117.38(18) . . ? C3 C2 C1 121.42(19) . . ? C2 C3 C4 119.67(19) . . ? O2 C4 C3 115.33(18) . . ? O2 C4 C5 123.39(18) . . ? C3 C4 C5 121.27(19) . . ? C6 C5 C4 116.84(18) . . ? C6 C5 C7 122.11(18) . . ? C4 C5 C7 121.02(18) . . ? C1 C6 C5 123.71(19) . . ? C5 C7 C8 110.77(16) . . ? C5 C7 C29 113.27(17) . . ? C8 C7 C29 111.79(17) . . ? C13 C8 C9 117.03(19) . . ? C13 C8 C7 121.54(18) . . ? C9 C8 C7 121.43(18) . . ? O3 C9 C10 121.35(19) . . ? O3 C9 C8 117.32(18) . . ? C10 C9 C8 121.32(19) . . ? C11 C10 C9 119.71(19) . . ? O4 C11 C10 121.42(19) . . ? O4 C11 C12 117.51(19) . . ? C10 C11 C12 121.07(19) . . ? C13 C12 C11 117.32(19) . . ? C13 C12 C14 121.28(18) . . ? C11 C12 C14 121.40(18) . . ? C12 C13 C8 123.53(19) . . ? C15 C14 C12 110.70(16) . . ? C15 C14 C31 114.95(17) . . ? C12 C14 C31 111.15(17) . . ? C20 C15 C16 116.78(19) . . ? C20 C15 C14 122.78(18) . . ? C16 C15 C14 120.43(18) . . ? O5 C16 C17 115.79(18) . . ? O5 C16 C15 122.66(19) . . ? C17 C16 C15 121.55(19) . . ? C16 C17 C18 119.84(19) . . ? O6 C18 C17 121.82(19) . . ? O6 C18 C19 117.23(18) . . ? C17 C18 C19 120.94(19) . . ? C20 C19 C18 117.37(19) . . ? C20 C19 C21 123.93(18) . . ? C18 C19 C21 118.70(18) . . ? C19 C20 C15 123.52(19) . . ? C19 C21 C22 110.79(16) . . ? C19 C21 C33 113.75(17) . . ? C22 C21 C33 111.97(16) . . ? C27 C22 C23 116.60(18) . . ? C27 C22 C21 120.51(18) . . ? C23 C22 C21 122.89(18) . . ? O7 C23 C24 114.66(18) . . ? O7 C23 C22 124.15(19) . . ? C24 C23 C22 121.19(19) . . ? C23 C24 C25 120.18(19) . . ? C24 C25 O8 116.63(18) . . ? C24 C25 C26 121.14(19) . . ? O8 C25 C26 122.21(19) . . ? C25 C26 C27 116.97(19) . . ? C25 C26 C28 121.56(18) . . ? C27 C26 C28 121.46(18) . . ? C26 C27 C22 123.85(19) . . ? C1 C28 C35 113.49(17) . . ? C1 C28 C26 111.00(16) . . ? C35 C28 C26 112.05(17) . . ? C30 C29 C7 112.48(17) . . ? C32 C31 C14 111.45(18) . . ? C34 C33 C21 112.54(17) . . ? C36 C35 C28 112.30(18) . . ? O10 C41 O9 122.9(2) . . ? O10 C41 C42 122.0(2) . . ? O9 C41 C42 115.1(2) . . ? C43 C42 C41 120.8(3) . . ? C42 C43 Cl1 122.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 O1 -179.44(17) . . . . ? C28 C1 C2 O1 2.4(3) . . . . ? C6 C1 C2 C3 0.5(3) . . . . ? C28 C1 C2 C3 -177.69(18) . . . . ? O1 C2 C3 C4 179.98(17) . . . . ? C1 C2 C3 C4 0.1(3) . . . . ? C2 C3 C4 O2 -179.57(17) . . . . ? C2 C3 C4 C5 -0.8(3) . . . . ? O2 C4 C5 C6 179.62(18) . . . . ? C3 C4 C5 C6 1.0(3) . . . . ? O2 C4 C5 C7 -2.0(3) . . . . ? C3 C4 C5 C7 179.31(18) . . . . ? C2 C1 C6 C5 -0.3(3) . . . . ? C28 C1 C6 C5 177.78(18) . . . . ? C4 C5 C6 C1 -0.4(3) . . . . ? C7 C5 C6 C1 -178.72(18) . . . . ? C6 C5 C7 C8 99.4(2) . . . . ? C4 C5 C7 C8 -78.9(2) . . . . ? C6 C5 C7 C29 -27.1(3) . . . . ? C4 C5 C7 C29 154.62(18) . . . . ? C5 C7 C8 C13 -77.7(2) . . . . ? C29 C7 C8 C13 49.7(3) . . . . ? C5 C7 C8 C9 101.0(2) . . . . ? C29 C7 C8 C9 -131.7(2) . . . . ? C13 C8 C9 O3 177.76(17) . . . . ? C7 C8 C9 O3 -1.0(3) . . . . ? C13 C8 C9 C10 -1.4(3) . . . . ? C7 C8 C9 C10 179.86(18) . . . . ? O3 C9 C10 C11 -178.04(18) . . . . ? C8 C9 C10 C11 1.1(3) . . . . ? C9 C10 C11 O4 178.74(18) . . . . ? C9 C10 C11 C12 -0.7(3) . . . . ? O4 C11 C12 C13 -178.82(17) . . . . ? C10 C11 C12 C13 0.6(3) . . . . ? O4 C11 C12 C14 1.0(3) . . . . ? C10 C11 C12 C14 -179.61(18) . . . . ? C11 C12 C13 C8 -1.0(3) . . . . ? C14 C12 C13 C8 179.22(18) . . . . ? C9 C8 C13 C12 1.4(3) . . . . ? C7 C8 C13 C12 -179.87(18) . . . . ? C13 C12 C14 C15 77.5(2) . . . . ? C11 C12 C14 C15 -102.3(2) . . . . ? C13 C12 C14 C31 -51.6(2) . . . . ? C11 C12 C14 C31 128.7(2) . . . . ? C12 C14 C15 C20 -99.0(2) . . . . ? C31 C14 C15 C20 27.9(3) . . . . ? C12 C14 C15 C16 79.5(2) . . . . ? C31 C14 C15 C16 -153.55(19) . . . . ? C20 C15 C16 O5 -179.19(18) . . . . ? C14 C15 C16 O5 2.2(3) . . . . ? C20 C15 C16 C17 0.1(3) . . . . ? C14 C15 C16 C17 -178.49(18) . . . . ? O5 C16 C17 C18 179.32(18) . . . . ? C15 C16 C17 C18 0.0(3) . . . . ? C16 C17 C18 O6 179.63(18) . . . . ? C16 C17 C18 C19 -0.2(3) . . . . ? O6 C18 C19 C20 -179.56(17) . . . . ? C17 C18 C19 C20 0.2(3) . . . . ? O6 C18 C19 C21 -0.3(3) . . . . ? C17 C18 C19 C21 179.54(18) . . . . ? C18 C19 C20 C15 -0.1(3) . . . . ? C21 C19 C20 C15 -179.40(18) . . . . ? C16 C15 C20 C19 0.0(3) . . . . ? C14 C15 C20 C19 178.55(18) . . . . ? C20 C19 C21 C22 100.1(2) . . . . ? C18 C19 C21 C22 -79.1(2) . . . . ? C20 C19 C21 C33 -27.1(3) . . . . ? C18 C19 C21 C33 153.69(18) . . . . ? C19 C21 C22 C27 -73.6(2) . . . . ? C33 C21 C22 C27 54.5(2) . . . . ? C19 C21 C22 C23 106.7(2) . . . . ? C33 C21 C22 C23 -125.1(2) . . . . ? C27 C22 C23 O7 -179.25(18) . . . . ? C21 C22 C23 O7 0.4(3) . . . . ? C27 C22 C23 C24 0.8(3) . . . . ? C21 C22 C23 C24 -179.52(19) . . . . ? O7 C23 C24 C25 179.22(18) . . . . ? C22 C23 C24 C25 -0.8(3) . . . . ? C23 C24 C25 O8 -179.53(19) . . . . ? C23 C24 C25 C26 -1.2(3) . . . . ? C24 C25 C26 C27 3.0(3) . . . . ? O8 C25 C26 C27 -178.72(18) . . . . ? C24 C25 C26 C28 -175.73(19) . . . . ? O8 C25 C26 C28 2.6(3) . . . . ? C25 C26 C27 C22 -3.1(3) . . . . ? C28 C26 C27 C22 175.65(18) . . . . ? C23 C22 C27 C26 1.2(3) . . . . ? C21 C22 C27 C26 -178.46(18) . . . . ? C6 C1 C28 C35 28.0(3) . . . . ? C2 C1 C28 C35 -153.92(18) . . . . ? C6 C1 C28 C26 -99.2(2) . . . . ? C2 C1 C28 C26 78.8(2) . . . . ? C25 C26 C28 C1 -104.6(2) . . . . ? C27 C26 C28 C1 76.7(2) . . . . ? C25 C26 C28 C35 127.4(2) . . . . ? C27 C26 C28 C35 -51.3(3) . . . . ? C5 C7 C29 C30 -172.23(18) . . . . ? C8 C7 C29 C30 61.8(2) . . . . ? C15 C14 C31 C32 173.34(18) . . . . ? C12 C14 C31 C32 -59.9(2) . . . . ? C19 C21 C33 C34 -173.77(17) . . . . ? C22 C21 C33 C34 59.7(2) . . . . ? C1 C28 C35 C36 171.18(18) . . . . ? C26 C28 C35 C36 -62.1(2) . . . . ? O10 C41 C42 C43 171.5(3) . . . . ? O9 C41 C42 C43 -8.4(4) . . . . ? C41 C42 C43 Cl1 -177.23(19) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1S H1S O2S 0.95 1.70 2.655(3) 177.3 . O2S H2S O8 0.79 1.97 2.749(3) 169.6 2_766 O1 H1O O7 0.76(3) 1.94(3) 2.678(2) 162(3) 2_766 O2 H2O O3 0.82(3) 1.93(3) 2.746(2) 170(3) . O3 H3O O5 0.72(3) 2.02(3) 2.707(2) 162(3) 2_665 O5 H5O O4 0.80(3) 1.98(3) 2.757(2) 166(3) . O6 H6O O10 0.75(3) 1.96(3) 2.705(2) 170(3) . O7 H7O O2 0.77(3) 2.13(3) 2.768(2) 141(3) 1_655 O7 H7O O6 0.77(3) 2.34(3) 2.877(2) 128(3) . O8 H8O O1 0.79(3) 1.97(3) 2.730(2) 164(3) . O9 H9O O1S 1.04(3) 1.50(3) 2.539(3) 177(3) . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.768 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.060 #=======================================END data_CECR-E-HClA-2MeOH-1.5H2O@200k _database_code_depnum_ccdc_archive 'CCDC 629569' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CECR-E-HClA-2MeOH-1.5H2O@200k _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C41 H54 Cl O13.50' _chemical_formula_weight 798.29 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4557(9) _cell_length_b 13.3257(11) _cell_length_c 14.6792(12) _cell_angle_alpha 98.972(2) _cell_angle_beta 109.090(2) _cell_angle_gamma 95.411(2) _cell_volume 2066.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 865 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 0.157 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.9749 _exptl_absorpt_correction_T_max 0.9842 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10648 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7221 _reflns_number_gt 5233 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1146P)^2^+0.8899P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7221 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1897 _refine_ls_wR_factor_gt 0.1706 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 O1 O 0.79665(16) 0.60410(15) 0.57805(13) 0.0308(4) Uani 1 1 d . . . O2 O 0.42098(16) 0.60328(15) 0.31456(14) 0.0346(5) Uani 1 1 d . . . O3 O 0.32196(17) 0.65257(17) 0.13223(15) 0.0336(5) Uani 1 1 d . . . O4 O 0.54826(18) 0.61577(17) -0.09341(14) 0.0367(5) Uani 1 1 d . . . O5 O 0.77458(19) 0.54431(16) -0.03585(14) 0.0353(5) Uani 1 1 d . . . O6 O 1.14168(17) 0.54290(16) 0.23434(14) 0.0373(5) Uani 1 1 d . . . O7 O 1.28462(16) 0.59679(14) 0.44192(15) 0.0333(4) Uani 1 1 d . . . O8 O 1.0535(2) 0.63313(17) 0.65284(14) 0.0359(5) Uani 1 1 d . . . C1 C 0.7832(2) 0.74301(19) 0.49385(17) 0.0243(5) Uani 1 1 d . . . C2 C 0.7273(2) 0.65022(19) 0.50423(17) 0.0249(5) Uani 1 1 d . . . C3 C 0.6073(2) 0.6052(2) 0.44411(18) 0.0272(5) Uani 1 1 d . . . H3A H 0.5714 0.5419 0.4530 0.033 Uiso 1 1 calc R . . C4 C 0.5395(2) 0.65323(19) 0.37049(18) 0.0264(5) Uani 1 1 d . . . C5 C 0.5904(2) 0.74697(19) 0.35688(17) 0.0245(5) Uani 1 1 d . . . C6 C 0.7121(2) 0.78884(19) 0.41948(17) 0.0246(5) Uani 1 1 d . . . H6A H 0.7485 0.8521 0.4109 0.029 Uiso 1 1 calc R . . C7 C 0.5172(2) 0.79887(19) 0.27475(18) 0.0256(5) Uani 1 1 d . . . H7A H 0.4274 0.7854 0.2690 0.031 Uiso 1 1 calc R . . C8 C 0.5241(2) 0.74920(19) 0.17604(18) 0.0255(5) Uani 1 1 d . . . C9 C 0.4253(2) 0.6779(2) 0.10674(18) 0.0269(6) Uani 1 1 d . . . C10 C 0.4312(2) 0.6335(2) 0.01687(19) 0.0316(6) Uani 1 1 d . . . H10A H 0.3627 0.5858 -0.0292 0.038 Uiso 1 1 calc R . . C11 C 0.5380(2) 0.6589(2) -0.00587(18) 0.0286(6) Uani 1 1 d . . . C12 C 0.6397(2) 0.72884(19) 0.06141(17) 0.0263(5) Uani 1 1 d . . . C13 C 0.6297(2) 0.77138(19) 0.15080(18) 0.0259(5) Uani 1 1 d . . . H13A H 0.6988 0.8182 0.1974 0.031 Uiso 1 1 calc R . . C14 C 0.7573(2) 0.7580(2) 0.03759(18) 0.0276(6) Uani 1 1 d . . . H14A H 0.7350 0.7321 -0.0346 0.033 Uiso 1 1 calc R . . C15 C 0.8618(2) 0.70088(19) 0.08907(17) 0.0256(5) Uani 1 1 d . . . C16 C 0.8632(2) 0.5991(2) 0.05074(18) 0.0276(6) Uani 1 1 d . . . C17 C 0.9556(2) 0.5448(2) 0.09793(18) 0.0293(6) Uani 1 1 d . . . H17A H 0.9544 0.4750 0.0707 0.035 Uiso 1 1 calc R . . C18 C 1.0492(2) 0.5938(2) 0.18520(18) 0.0277(6) Uani 1 1 d . . . C19 C 1.0533(2) 0.69579(19) 0.22705(17) 0.0251(5) Uani 1 1 d . . . C20 C 0.9583(2) 0.74704(19) 0.17725(17) 0.0248(5) Uani 1 1 d . . . H20A H 0.9594 0.8167 0.2047 0.030 Uiso 1 1 calc R . . C21 C 1.1574(2) 0.74497(19) 0.32336(17) 0.0253(5) Uani 1 1 d . . . H21A H 1.2339 0.7155 0.3213 0.030 Uiso 1 1 calc R . . C22 C 1.1289(2) 0.71380(18) 0.41083(17) 0.0247(5) Uani 1 1 d . . . C23 C 1.1922(2) 0.64416(19) 0.46364(18) 0.0267(5) Uani 1 1 d . . . C24 C 1.1643(2) 0.6186(2) 0.54261(19) 0.0313(6) Uani 1 1 d . . . H24A H 1.2074 0.5707 0.5769 0.038 Uiso 1 1 calc R . . C25 C 1.0745(2) 0.6619(2) 0.57234(18) 0.0279(6) Uani 1 1 d . . . C26 C 1.0109(2) 0.73374(19) 0.52386(17) 0.0252(5) Uani 1 1 d . . . C27 C 1.0390(2) 0.75516(19) 0.44339(17) 0.0260(5) Uani 1 1 d . . . H27A H 0.9937 0.8013 0.4079 0.031 Uiso 1 1 calc R . . C28 C 0.9169(2) 0.78724(19) 0.55961(17) 0.0254(5) Uani 1 1 d . . . H28A H 0.9269 0.7711 0.6258 0.030 Uiso 1 1 calc R . . C29 C 0.5551(2) 0.9164(2) 0.2979(2) 0.0313(6) Uani 1 1 d . . . H29A H 0.5536 0.9443 0.3640 0.038 Uiso 1 1 calc R . . H29B H 0.6417 0.9330 0.2991 0.038 Uiso 1 1 calc R . . C30 C 0.4685(3) 0.9681(2) 0.2226(2) 0.0458(8) Uani 1 1 d . . . H30A H 0.4958 1.0427 0.2404 0.069 Uiso 1 1 calc R . . H30B H 0.3827 0.9527 0.2218 0.069 Uiso 1 1 calc R . . H30C H 0.4713 0.9421 0.1572 0.069 Uiso 1 1 calc R . . C31 C 0.7938(2) 0.8746(2) 0.0553(2) 0.0340(6) Uani 1 1 d . . . H31A H 0.8111 0.9045 0.1253 0.041 Uiso 1 1 calc R . . H31B H 0.8713 0.8903 0.0407 0.041 Uiso 1 1 calc R . . C32 C 0.6903(3) 0.9238(2) -0.0092(2) 0.0495(8) Uani 1 1 d . . . H32A H 0.7174 0.9981 0.0028 0.074 Uiso 1 1 calc R . . H32B H 0.6145 0.9108 0.0070 0.074 Uiso 1 1 calc R . . H32C H 0.6727 0.8940 -0.0786 0.074 Uiso 1 1 calc R . . C33 C 1.1905(2) 0.8621(2) 0.33714(19) 0.0306(6) Uani 1 1 d . . . H33A H 1.2068 0.8784 0.2785 0.037 Uiso 1 1 calc R . . H33B H 1.1181 0.8946 0.3424 0.037 Uiso 1 1 calc R . . C34 C 1.3050(3) 0.9075(2) 0.4286(2) 0.0424(7) Uani 1 1 d . . . H34A H 1.3220 0.9821 0.4345 0.064 Uiso 1 1 calc R . . H34B H 1.3775 0.8770 0.4230 0.064 Uiso 1 1 calc R . . H34C H 1.2889 0.8925 0.4871 0.064 Uiso 1 1 calc R . . C35 C 0.9458(2) 0.9046(2) 0.5748(2) 0.0323(6) Uani 1 1 d . . . H35A H 0.9443 0.9237 0.5120 0.039 Uiso 1 1 calc R . . H35B H 0.8800 0.9356 0.5941 0.039 Uiso 1 1 calc R . . C36 C 1.0732(3) 0.9482(2) 0.6538(2) 0.0450(8) Uani 1 1 d . . . H36A H 1.0882 1.0231 0.6608 0.067 Uiso 1 1 calc R . . H36B H 1.1387 0.9183 0.6347 0.067 Uiso 1 1 calc R . . H36C H 1.0743 0.9311 0.7167 0.067 Uiso 1 1 calc R . . O9 O 1.1183(3) 0.1754(2) 0.1724(2) 0.0751(8) Uani 1 1 d . . . O10 O 1.0996(2) 0.33750(18) 0.16825(19) 0.0637(7) Uani 1 1 d . . . C41 C 1.1622(3) 0.2721(3) 0.1951(2) 0.0511(8) Uani 1 1 d . . . C42 C 1.2986(3) 0.2987(3) 0.2573(3) 0.0634(10) Uani 1 1 d . . . H42A H 1.3398 0.3672 0.2694 0.076 Uiso 1 1 calc R . . C43 C 1.3601(4) 0.2305(4) 0.2944(3) 0.0883(15) Uani 1 1 d . . . H43A H 1.3197 0.1613 0.2793 0.106 Uiso 1 1 calc R . . Cl1 Cl 1.51264(12) 0.26087(16) 0.36997(12) 0.1395(8) Uani 1 1 d . . . O1S O 0.8894(3) 0.1485(2) 0.0652(2) 0.0758(8) Uani 1 1 d . . . H1S H 0.8497 0.1912 0.1011 0.114 Uiso 1 1 d R . . C1S C 0.8651(4) 0.1817(4) -0.0248(3) 0.0866(15) Uani 1 1 d . . . H1S1 H 0.7838 0.2056 -0.0431 0.130 Uiso 1 1 calc R . . H1S2 H 0.8640 0.1245 -0.0760 0.130 Uiso 1 1 calc R . . H1S3 H 0.9307 0.2382 -0.0178 0.130 Uiso 1 1 calc R . . O2S O 0.7775(3) 0.2642(3) 0.1665(2) 0.0916(10) Uani 1 1 d . . . H2S H 0.8268 0.2854 0.2198 0.137 Uiso 1 1 d R . . C2S C 0.6780(4) 0.2104(4) 0.1833(4) 0.0859(14) Uani 1 1 d . . . H2S1 H 0.7108 0.1785 0.2404 0.129 Uiso 1 1 calc R . . H2S2 H 0.6312 0.1570 0.1253 0.129 Uiso 1 1 calc R . . H2S3 H 0.6225 0.2581 0.1960 0.129 Uiso 1 1 calc R . . O1W O 0.3385(7) 0.5266(6) 0.7639(5) 0.090(3) Uani 0.40 1 d P A 1 H1WA H 0.2727 0.4772 0.7136 0.135 Uiso 0.40 1 d PR A 1 H1WB H 0.3261 0.5601 0.8241 0.135 Uiso 0.40 1 d PR A 1 O2W O 0.2359(3) 0.4501(3) 0.7433(2) 0.0417(8) Uani 0.60 1 d P B 2 H2WA H 0.1889 0.3911 0.7234 0.062 Uiso 0.60 1 d PR B 2 H2WB H 0.2403 0.4684 0.6896 0.062 Uiso 0.60 1 d PR B 2 O3W O 0.3577(4) 0.4655(3) 0.8090(3) 0.0496(12) Uani 0.50 1 d P C 3 H3WA H 0.2786 0.4548 0.8127 0.074 Uiso 0.50 1 d PR C 3 H3WB H 0.3588 0.4914 0.7593 0.074 Uiso 0.50 1 d PR C 3 H1O H 0.766(3) 0.543(3) 0.570(3) 0.056(11) Uiso 1 1 d . . . H2O H 0.399(4) 0.626(3) 0.254(3) 0.071(12) Uiso 1 1 d . . . H3O H 0.291(3) 0.606(3) 0.100(3) 0.046(11) Uiso 1 1 d . . . H40 H 0.490(4) 0.580(3) -0.131(3) 0.055(11) Uiso 1 1 d . . . H5O H 0.723(4) 0.575(3) -0.046(3) 0.064(13) Uiso 1 1 d . . . H6O H 1.132(3) 0.481(3) 0.208(2) 0.040(9) Uiso 1 1 d . . . H7O H 1.280(4) 0.603(3) 0.383(3) 0.073(13) Uiso 1 1 d . . . H8O H 0.988(4) 0.626(3) 0.647(3) 0.066(14) Uiso 1 1 d . . . H9O H 1.033(2) 0.1634(17) 0.1154(18) 0.014(6) 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 O1 0.0246(9) 0.0374(11) 0.0308(10) 0.0187(8) 0.0035(8) 0.0090(8) O2 0.0179(9) 0.0458(11) 0.0350(11) 0.0161(9) 0.0001(8) -0.0005(8) O3 0.0215(9) 0.0426(12) 0.0319(11) 0.0043(10) 0.0059(8) -0.0016(9) O4 0.0246(10) 0.0553(13) 0.0214(10) 0.0034(9) 0.0004(8) -0.0015(9) O5 0.0246(10) 0.0423(11) 0.0291(10) 0.0004(8) -0.0003(8) 0.0030(9) O6 0.0278(10) 0.0357(11) 0.0391(11) 0.0050(9) -0.0017(8) 0.0134(8) O7 0.0268(10) 0.0427(11) 0.0385(11) 0.0191(9) 0.0141(8) 0.0165(8) O8 0.0260(11) 0.0570(13) 0.0327(10) 0.0254(9) 0.0106(8) 0.0160(9) C1 0.0184(12) 0.0335(13) 0.0220(12) 0.0089(10) 0.0050(9) 0.0102(10) C2 0.0222(12) 0.0340(13) 0.0228(12) 0.0137(10) 0.0077(10) 0.0116(10) C3 0.0220(12) 0.0341(13) 0.0292(13) 0.0144(11) 0.0095(10) 0.0073(10) C4 0.0164(11) 0.0360(14) 0.0260(13) 0.0088(11) 0.0048(10) 0.0048(10) C5 0.0199(12) 0.0327(13) 0.0208(12) 0.0082(10) 0.0044(9) 0.0089(10) C6 0.0201(12) 0.0304(13) 0.0233(12) 0.0098(10) 0.0053(10) 0.0059(10) C7 0.0159(11) 0.0333(13) 0.0259(13) 0.0112(10) 0.0018(9) 0.0070(10) C8 0.0203(12) 0.0310(13) 0.0235(12) 0.0120(10) 0.0011(9) 0.0080(10) C9 0.0188(12) 0.0361(14) 0.0257(13) 0.0144(11) 0.0030(10) 0.0078(10) C10 0.0222(13) 0.0391(14) 0.0253(13) 0.0073(11) -0.0017(10) 0.0008(11) C11 0.0238(13) 0.0385(14) 0.0212(12) 0.0115(11) 0.0017(10) 0.0070(11) C12 0.0200(12) 0.0332(13) 0.0240(13) 0.0137(11) 0.0012(10) 0.0066(10) C13 0.0196(12) 0.0301(13) 0.0232(12) 0.0104(10) -0.0015(9) 0.0041(10) C14 0.0226(12) 0.0381(14) 0.0204(12) 0.0125(11) 0.0022(10) 0.0043(10) C15 0.0197(12) 0.0360(14) 0.0230(12) 0.0133(11) 0.0063(10) 0.0046(10) C16 0.0206(12) 0.0386(14) 0.0208(12) 0.0057(11) 0.0045(10) 0.0012(10) C17 0.0248(13) 0.0340(14) 0.0279(13) 0.0048(11) 0.0079(10) 0.0053(10) C18 0.0195(12) 0.0365(14) 0.0275(13) 0.0099(11) 0.0063(10) 0.0073(10) C19 0.0188(12) 0.0340(13) 0.0222(12) 0.0103(10) 0.0049(10) 0.0037(10) C20 0.0206(12) 0.0316(13) 0.0230(12) 0.0092(10) 0.0067(10) 0.0048(10) C21 0.0169(11) 0.0332(13) 0.0247(13) 0.0094(10) 0.0034(10) 0.0066(10) C22 0.0177(11) 0.0305(13) 0.0221(12) 0.0075(10) 0.0008(9) 0.0031(10) C23 0.0186(12) 0.0336(13) 0.0279(13) 0.0090(11) 0.0060(10) 0.0066(10) C24 0.0248(13) 0.0368(14) 0.0331(14) 0.0166(12) 0.0052(11) 0.0107(11) C25 0.0207(12) 0.0390(14) 0.0236(12) 0.0126(11) 0.0038(10) 0.0062(10) C26 0.0169(11) 0.0327(13) 0.0220(12) 0.0073(10) 0.0006(9) 0.0045(10) C27 0.0190(12) 0.0303(13) 0.0233(12) 0.0093(10) -0.0020(9) 0.0048(10) C28 0.0204(12) 0.0343(13) 0.0196(12) 0.0087(10) 0.0022(9) 0.0070(10) C29 0.0251(13) 0.0335(14) 0.0332(14) 0.0107(11) 0.0040(11) 0.0089(11) C30 0.0386(16) 0.0411(16) 0.0530(19) 0.0196(14) 0.0027(14) 0.0146(13) C31 0.0273(13) 0.0414(15) 0.0305(14) 0.0165(12) 0.0023(11) 0.0049(11) C32 0.0445(18) 0.0474(18) 0.0510(19) 0.0274(15) 0.0000(15) 0.0112(14) C33 0.0239(13) 0.0359(14) 0.0297(14) 0.0108(11) 0.0048(11) 0.0036(11) C34 0.0304(15) 0.0426(16) 0.0425(17) 0.0057(13) 0.0009(13) -0.0032(12) C35 0.0238(13) 0.0350(14) 0.0335(14) 0.0075(12) 0.0030(11) 0.0067(11) C36 0.0353(16) 0.0410(16) 0.0427(17) 0.0051(14) -0.0045(13) 0.0002(13) O9 0.0618(17) 0.0581(16) 0.088(2) 0.0114(14) 0.0041(15) 0.0125(13) O10 0.0665(16) 0.0450(13) 0.0631(16) 0.0144(12) -0.0006(13) 0.0079(12) C41 0.056(2) 0.055(2) 0.0446(18) 0.0072(16) 0.0225(16) 0.0074(17) C42 0.047(2) 0.091(3) 0.050(2) 0.004(2) 0.0174(17) 0.016(2) C43 0.051(2) 0.119(4) 0.071(3) -0.020(3) 0.006(2) 0.023(3) Cl1 0.0558(7) 0.2048(18) 0.1044(10) -0.0515(11) -0.0094(7) 0.0356(9) O1S 0.0558(16) 0.0855(19) 0.0738(19) 0.0167(15) 0.0109(14) -0.0066(14) C1S 0.061(3) 0.128(4) 0.057(2) 0.037(3) 0.001(2) -0.008(3) O2S 0.0591(18) 0.141(3) 0.0568(17) 0.0051(18) 0.0082(14) -0.0035(18) C2S 0.051(2) 0.118(4) 0.087(3) 0.030(3) 0.016(2) 0.013(2) O1W 0.077(5) 0.095(5) 0.045(4) 0.034(4) -0.042(3) -0.048(4) O2W 0.0318(17) 0.058(2) 0.0339(18) 0.0203(16) 0.0058(14) 0.0034(15) O3W 0.027(2) 0.044(2) 0.056(3) 0.003(2) -0.0121(19) 0.0056(18) _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 O1 C2 1.386(3) . ? O2 C4 1.375(3) . ? O3 C9 1.382(3) . ? O4 C11 1.370(3) . ? O5 C16 1.381(3) . ? O6 C18 1.375(3) . ? O7 C23 1.380(3) . ? O8 C25 1.382(3) . ? C1 C2 1.391(4) . ? C1 C6 1.396(3) . ? C1 C28 1.520(3) . ? C2 C3 1.383(3) . ? C3 C4 1.393(3) . ? C4 C5 1.399(4) . ? C5 C6 1.399(3) . ? C5 C7 1.531(3) . ? C7 C8 1.526(3) . ? C7 C29 1.538(4) . ? C8 C13 1.396(4) . ? C8 C9 1.400(3) . ? C9 C10 1.385(4) . ? C10 C11 1.395(4) . ? C11 C12 1.399(3) . ? C12 C13 1.391(4) . ? C12 C14 1.529(3) . ? C14 C31 1.529(4) . ? C14 C15 1.531(3) . ? C15 C16 1.389(4) . ? C15 C20 1.401(3) . ? C16 C17 1.394(4) . ? C17 C18 1.388(3) . ? C18 C19 1.391(4) . ? C19 C20 1.400(3) . ? C19 C21 1.521(3) . ? C21 C22 1.531(4) . ? C21 C33 1.536(3) . ? C22 C27 1.393(4) . ? C22 C23 1.404(3) . ? C23 C24 1.381(4) . ? C24 C25 1.382(4) . ? C25 C26 1.399(3) . ? C26 C27 1.384(4) . ? C26 C28 1.531(3) . ? C28 C35 1.533(4) . ? C29 C30 1.526(4) . ? C31 C32 1.529(4) . ? C33 C34 1.528(4) . ? C35 C36 1.528(4) . ? O9 C41 1.289(4) . ? O10 C41 1.211(4) . ? C41 C42 1.504(5) . ? C42 C43 1.281(6) . ? C43 Cl1 1.705(4) . ? O1S C1S 1.408(5) . ? O2S C2S 1.400(5) . ? 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 C2 C1 C6 116.7(2) . . ? C2 C1 C28 119.8(2) . . ? C6 C1 C28 123.5(2) . . ? C3 C2 O1 120.8(2) . . ? C3 C2 C1 121.9(2) . . ? O1 C2 C1 117.2(2) . . ? C2 C3 C4 119.7(2) . . ? O2 C4 C3 115.7(2) . . ? O2 C4 C5 123.3(2) . . ? C3 C4 C5 121.0(2) . . ? C6 C5 C4 116.9(2) . . ? C6 C5 C7 121.9(2) . . ? C4 C5 C7 121.2(2) . . ? C1 C6 C5 123.8(2) . . ? C8 C7 C5 110.83(19) . . ? C8 C7 C29 112.3(2) . . ? C5 C7 C29 113.20(19) . . ? C13 C8 C9 116.6(2) . . ? C13 C8 C7 121.8(2) . . ? C9 C8 C7 121.6(2) . . ? O3 C9 C10 121.2(2) . . ? O3 C9 C8 117.2(2) . . ? C10 C9 C8 121.6(2) . . ? C9 C10 C11 119.9(2) . . ? O4 C11 C10 121.7(2) . . ? O4 C11 C12 117.6(2) . . ? C10 C11 C12 120.6(2) . . ? C13 C12 C11 117.5(2) . . ? C13 C12 C14 121.1(2) . . ? C11 C12 C14 121.4(2) . . ? C12 C13 C8 123.8(2) . . ? C31 C14 C12 111.8(2) . . ? C31 C14 C15 115.0(2) . . ? C12 C14 C15 110.6(2) . . ? C16 C15 C20 116.9(2) . . ? C16 C15 C14 120.9(2) . . ? C20 C15 C14 122.2(2) . . ? O5 C16 C15 123.1(2) . . ? O5 C16 C17 115.1(2) . . ? C15 C16 C17 121.8(2) . . ? C18 C17 C16 119.2(2) . . ? O6 C18 C17 121.1(2) . . ? O6 C18 C19 117.2(2) . . ? C17 C18 C19 121.7(2) . . ? C18 C19 C20 117.0(2) . . ? C18 C19 C21 119.3(2) . . ? C20 C19 C21 123.7(2) . . ? C19 C20 C15 123.4(2) . . ? C19 C21 C22 110.90(19) . . ? C19 C21 C33 113.8(2) . . ? C22 C21 C33 112.1(2) . . ? C27 C22 C23 116.3(2) . . ? C27 C22 C21 121.1(2) . . ? C23 C22 C21 122.6(2) . . ? O7 C23 C24 115.3(2) . . ? O7 C23 C22 123.8(2) . . ? C24 C23 C22 120.8(2) . . ? C23 C24 C25 120.8(2) . . ? C24 C25 O8 117.1(2) . . ? C24 C25 C26 120.7(2) . . ? O8 C25 C26 122.3(2) . . ? C27 C26 C25 116.8(2) . . ? C27 C26 C28 121.9(2) . . ? C25 C26 C28 121.3(2) . . ? C26 C27 C22 124.6(2) . . ? C1 C28 C26 111.30(19) . . ? C1 C28 C35 113.48(19) . . ? C26 C28 C35 112.0(2) . . ? C30 C29 C7 112.3(2) . . ? C32 C31 C14 111.5(2) . . ? C34 C33 C21 112.5(2) . . ? C36 C35 C28 112.1(2) . . ? O10 C41 O9 123.2(3) . . ? O10 C41 C42 121.9(3) . . ? O9 C41 C42 114.9(3) . . ? C43 C42 C41 121.2(4) . . ? C42 C43 Cl1 121.7(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.585 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.066 #=======================================END data_CECR-E-HClA-2MeOH-1.5H2O@90k-1h _database_code_depnum_ccdc_archive 'CCDC 629570' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CECR-E-HClA-2MeOH-1.5H2O@90k-1h _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C41 H54 Cl O13.50' _chemical_formula_weight 798.29 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3771(5) _cell_length_b 13.3223(7) _cell_length_c 14.6324(6) _cell_angle_alpha 99.0998(15) _cell_angle_beta 109.2728(13) _cell_angle_gamma 95.2633(15) _cell_volume 2042.38(16) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 675 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.9747 _exptl_absorpt_correction_T_max 0.9841 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9715 _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6944 _reflns_number_gt 5298 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+2.3738P] 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 6944 _refine_ls_number_parameters 546 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0822 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1730 _refine_ls_wR_factor_gt 0.1589 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.151 _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 O1 O 0.79607(18) 0.60467(15) 0.57882(14) 0.0216(5) Uani 1 1 d . . . O2 O 0.41982(18) 0.60425(16) 0.31300(15) 0.0250(5) Uani 1 1 d . . . O3 O 0.32073(18) 0.65300(16) 0.13121(14) 0.0238(5) Uani 1 1 d . . . O4 O 0.54889(19) 0.61352(16) -0.09473(14) 0.0260(5) Uani 1 1 d . . . O5 O 0.77612(19) 0.54391(16) -0.03735(14) 0.0251(5) Uani 1 1 d . . . O6 O 1.14382(19) 0.54111(15) 0.23562(15) 0.0265(5) Uani 1 1 d . . . O7 O 1.2881(2) 0.59662(16) 0.44304(15) 0.0272(5) Uani 1 1 d . . . O8 O 1.05177(19) 0.63235(16) 0.65247(14) 0.0244(5) Uani 1 1 d . . . C1 C 0.7836(3) 0.7440(2) 0.49418(19) 0.0165(6) Uani 1 1 d . . . C2 C 0.7276(3) 0.6513(2) 0.50493(19) 0.0178(6) Uani 1 1 d . . . C3 C 0.6066(3) 0.6069(2) 0.4441(2) 0.0188(6) Uani 1 1 d . . . H3A H 0.5697 0.5439 0.4530 0.023 Uiso 1 1 calc R . . C4 C 0.5393(3) 0.6548(2) 0.3697(2) 0.0181(6) Uani 1 1 d . . . C5 C 0.5904(3) 0.7481(2) 0.35616(19) 0.0165(6) Uani 1 1 d . . . C6 C 0.7127(3) 0.7901(2) 0.41979(19) 0.0167(6) Uani 1 1 d . . . H6A H 0.7494 0.8536 0.4118 0.020 Uiso 1 1 calc R . . C7 C 0.5167(3) 0.8002(2) 0.27389(19) 0.0175(6) Uani 1 1 d . . . H7A H 0.4263 0.7873 0.2681 0.021 Uiso 1 1 calc R . . C8 C 0.5236(3) 0.7496(2) 0.17441(19) 0.0173(6) Uani 1 1 d . . . C9 C 0.4247(3) 0.6783(2) 0.1056(2) 0.0199(6) Uani 1 1 d . . . C10 C 0.4308(3) 0.6329(2) 0.0153(2) 0.0220(6) Uani 1 1 d . . . H10A H 0.3619 0.5850 -0.0311 0.026 Uiso 1 1 calc R . . C11 C 0.5384(3) 0.6580(2) -0.0065(2) 0.0206(6) Uani 1 1 d . . . C12 C 0.6404(3) 0.7287(2) 0.06020(19) 0.0184(6) Uani 1 1 d . . . C13 C 0.6298(3) 0.7723(2) 0.14952(19) 0.0174(6) Uani 1 1 d . . . H13A H 0.6987 0.8201 0.1960 0.021 Uiso 1 1 calc R . . C14 C 0.7587(3) 0.7574(2) 0.0363(2) 0.0201(6) Uani 1 1 d . . . H14A H 0.7364 0.7310 -0.0361 0.024 Uiso 1 1 calc R . . C15 C 0.8636(3) 0.7010(2) 0.08868(19) 0.0175(6) Uani 1 1 d . . . C16 C 0.8650(3) 0.5979(2) 0.0504(2) 0.0197(6) Uani 1 1 d . . . C17 C 0.9573(3) 0.5440(2) 0.0982(2) 0.0217(6) Uani 1 1 d . . . H17A H 0.9559 0.4741 0.0708 0.026 Uiso 1 1 calc R . . C18 C 1.0516(3) 0.5922(2) 0.1861(2) 0.0204(6) Uani 1 1 d . . . C19 C 1.0553(3) 0.6952(2) 0.22742(19) 0.0172(6) Uani 1 1 d . . . C20 C 0.9604(3) 0.7463(2) 0.17729(19) 0.0168(6) Uani 1 1 d . . . H20A H 0.9616 0.8161 0.2050 0.020 Uiso 1 1 calc R . . C21 C 1.1607(3) 0.7449(2) 0.32423(19) 0.0178(6) Uani 1 1 d . . . H21A H 1.2378 0.7155 0.3222 0.021 Uiso 1 1 calc R . . C22 C 1.1326(3) 0.7143(2) 0.41245(19) 0.0182(6) Uani 1 1 d . . . C23 C 1.1949(3) 0.6442(2) 0.4648(2) 0.0199(6) Uani 1 1 d . . . C24 C 1.1660(3) 0.6179(2) 0.5438(2) 0.0221(6) Uani 1 1 d . . . H24A H 1.2083 0.5692 0.5779 0.027 Uiso 1 1 calc R . . C25 C 1.0756(3) 0.6625(2) 0.5728(2) 0.0196(6) Uani 1 1 d . . . C26 C 1.0129(2) 0.7348(2) 0.52520(19) 0.0168(6) Uani 1 1 d . . . C27 C 1.0421(3) 0.7571(2) 0.44454(19) 0.0180(6) Uani 1 1 d . . . H27A H 0.9978 0.8042 0.4093 0.022 Uiso 1 1 calc R . . C28 C 0.9185(3) 0.7890(2) 0.56098(19) 0.0173(6) Uani 1 1 d . . . H28A H 0.9287 0.7732 0.6275 0.021 Uiso 1 1 calc R . . C29 C 0.5556(3) 0.9176(2) 0.2964(2) 0.0216(6) Uani 1 1 d . . . H29A H 0.5539 0.9464 0.3625 0.026 Uiso 1 1 calc R . . H29B H 0.6432 0.9334 0.2981 0.026 Uiso 1 1 calc R . . C30 C 0.4695(3) 0.9693(2) 0.2201(2) 0.0299(7) Uani 1 1 d . . . H30A H 0.4972 1.0439 0.2382 0.045 Uiso 1 1 calc R . . H30B H 0.3827 0.9542 0.2182 0.045 Uiso 1 1 calc R . . H30C H 0.4734 0.9431 0.1548 0.045 Uiso 1 1 calc R . . C31 C 0.7962(3) 0.8740(2) 0.0541(2) 0.0226(6) Uani 1 1 d . . . H31A H 0.8743 0.8891 0.0396 0.027 Uiso 1 1 calc R . . H31B H 0.8140 0.9040 0.1245 0.027 Uiso 1 1 calc R . . C32 C 0.6921(3) 0.9242(3) -0.0108(2) 0.0337(8) Uani 1 1 d . . . H32A H 0.7199 0.9985 0.0016 0.051 Uiso 1 1 calc R . . H32B H 0.6155 0.9116 0.0052 0.051 Uiso 1 1 calc R . . H32C H 0.6742 0.8946 -0.0806 0.051 Uiso 1 1 calc R . . C33 C 1.1937(3) 0.8619(2) 0.3378(2) 0.0204(6) Uani 1 1 d . . . H33A H 1.2095 0.8779 0.2787 0.024 Uiso 1 1 calc R . . H33B H 1.1207 0.8945 0.3431 0.024 Uiso 1 1 calc R . . C34 C 1.3090(3) 0.9079(2) 0.4292(2) 0.0278(7) Uani 1 1 d . . . H34A H 1.3256 0.9826 0.4347 0.042 Uiso 1 1 calc R . . H34B H 1.3822 0.8775 0.4236 0.042 Uiso 1 1 calc R . . H34C H 1.2935 0.8933 0.4882 0.042 Uiso 1 1 calc R . . C35 C 0.9471(3) 0.9061(2) 0.5757(2) 0.0220(6) Uani 1 1 d . . . H35A H 0.9455 0.9247 0.5125 0.026 Uiso 1 1 calc R . . H35B H 0.8804 0.9371 0.5945 0.026 Uiso 1 1 calc R . . C36 C 1.0747(3) 0.9506(2) 0.6551(2) 0.0287(7) Uani 1 1 d . . . H36A H 1.0892 1.0255 0.6617 0.043 Uiso 1 1 calc R . . H36B H 1.1412 0.9209 0.6365 0.043 Uiso 1 1 calc R . . H36C H 1.0760 0.9340 0.7183 0.043 Uiso 1 1 calc R . . O2S O 0.7766(3) 0.2710(3) 0.1713(2) 0.0638(9) Uani 1 1 d . . . H2S H 0.8259 0.2922 0.2246 0.096 Uiso 1 1 d R . . C2S C 0.6775(4) 0.2069(4) 0.1811(3) 0.0586(12) Uani 1 1 d . . . H2S1 H 0.7108 0.1749 0.2384 0.088 Uiso 1 1 calc R . . H2S2 H 0.6392 0.1532 0.1213 0.088 Uiso 1 1 calc R . . H2S3 H 0.6138 0.2480 0.1905 0.088 Uiso 1 1 calc R . . O1W O 0.3250(5) 0.5386(4) 0.7708(3) 0.0453(14) Uani 0.50 1 d P A 1 H1WA H 0.2593 0.4893 0.7205 0.068 Uiso 0.50 1 d PR A 1 H1WB H 0.3127 0.5722 0.8311 0.068 Uiso 0.50 1 d PR A 1 O2W O 0.2363(3) 0.4468(3) 0.7423(2) 0.0211(7) Uani 0.60 1 d P B 2 H2WA H 0.1893 0.3878 0.7224 0.032 Uiso 0.60 1 d PR B 2 H2WB H 0.2407 0.4651 0.6886 0.032 Uiso 0.60 1 d PR B 2 O3W O 0.3578(5) 0.4627(4) 0.8101(4) 0.0294(12) Uani 0.40 1 d P C 3 H3WA H 0.2787 0.4520 0.8138 0.044 Uiso 0.40 1 d PR C 3 H3WB H 0.3589 0.4886 0.7603 0.044 Uiso 0.40 1 d PR C 3 H1O H 0.7595 0.5513 0.5751 0.044 Uiso 1 1 d R . . H2O H 0.3934 0.6259 0.2625 0.044 Uiso 1 1 d R . . H3O H 0.2838 0.6090 0.0995 0.044 Uiso 1 1 d R . . H40 H 0.4844 0.5735 -0.1288 0.044 Uiso 1 1 d R . . H5O H 0.7167 0.5712 -0.0529 0.044 Uiso 1 1 d R . . H6O H 1.1335 0.4856 0.2103 0.044 Uiso 1 1 d R . . H7O H 1.2917 0.6038 0.3921 0.044 Uiso 1 1 d R . . H8O H 0.9791 0.6245 0.6426 0.044 Uiso 1 1 d R . . O1S O 0.8911(4) 0.1484(3) 0.0693(3) 0.0622(11) Uani 0.744(5) 1 d PD D 1 H1S H 0.8514 0.1911 0.1053 0.093 Uiso 0.744(5) 1 d PR D 1 C1S C 0.8717(7) 0.1800(10) -0.0248(8) 0.052(2) Uani 0.744(5) 1 d PD D 1 H1S1 H 0.7937 0.2098 -0.0441 0.078 Uiso 0.744(5) 1 calc PR D 1 H1S2 H 0.8654 0.1201 -0.0755 0.078 Uiso 0.744(5) 1 calc PR D 1 H1S3 H 0.9429 0.2314 -0.0181 0.078 Uiso 0.744(5) 1 calc PR D 1 O9 O 1.1123(9) 0.1719(6) 0.1718(6) 0.0744(19) Uani 0.709(4) 1 d PD E 1 H9O H 1.0192 0.1620 0.1265 0.112 Uiso 0.709(4) 1 d PR E 1 O10 O 1.0991(13) 0.3394(8) 0.1702(10) 0.0474(18) Uani 0.709(4) 1 d PD E 1 C41 C 1.1569(6) 0.2681(6) 0.1942(7) 0.0423(18) Uani 0.709(4) 1 d PD E 1 C42 C 1.2959(6) 0.2999(8) 0.2566(6) 0.066(3) Uani 0.709(4) 1 d PD E 1 H42A H 1.3363 0.3686 0.2673 0.080 Uiso 0.709(4) 1 calc PR E 1 C43 C 1.3584(7) 0.2298(6) 0.2951(4) 0.071(2) Uani 0.709(4) 1 d PD E 1 H43A H 1.3168 0.1611 0.2817 0.086 Uiso 0.709(4) 1 calc PR E 1 Cl1 Cl 1.51567(17) 0.2605(2) 0.37011(16) 0.1100(13) Uani 0.709(4) 1 d PD E 1 O1SB O 0.8818(12) 0.2816(9) 0.0437(8) 0.0622(11) Uani 0.256(5) 1 d PD D 2 H1SB H 0.9685 0.2965 0.0865 0.093 Uiso 0.256(5) 1 d PR D 2 C1SB C 0.838(3) 0.183(3) -0.026(3) 0.052(2) Uani 0.256(5) 1 d PD D 2 H1S4 H 0.9110 0.1494 -0.0280 0.078 Uiso 0.256(5) 1 calc PR D 2 H1S5 H 0.7914 0.1939 -0.0919 0.078 Uiso 0.256(5) 1 calc PR D 2 H1S6 H 0.7831 0.1382 -0.0045 0.078 Uiso 0.256(5) 1 calc PR D 2 O9B O 1.152(3) 0.1847(17) 0.2007(17) 0.0744(19) Uani 0.291(4) 1 d PD E 2 H9OB H 1.0730 0.1695 0.1725 0.112 Uiso 0.291(4) 1 d PR E 2 O10B O 1.113(3) 0.318(3) 0.163(3) 0.0474(18) Uani 0.291(4) 1 d PD E 2 C41B C 1.203(2) 0.2793(19) 0.215(2) 0.0423(18) Uani 0.291(4) 1 d PD E 2 C42B C 1.3452(17) 0.322(2) 0.2732(18) 0.066(3) Uani 0.291(4) 1 d PD E 2 H42B H 1.3652 0.3867 0.2575 0.080 Uiso 0.291(4) 1 calc PR E 2 C43B C 1.4423(17) 0.3007(12) 0.3337(11) 0.071(2) Uani 0.291(4) 1 d PD E 2 H43B H 1.5221 0.3435 0.3607 0.086 Uiso 0.291(4) 1 calc PR E 2 Cl1B Cl 1.4078(6) 0.1763(4) 0.3617(4) 0.095(2) Uani 0.291(4) 1 d PD E 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 O1 0.0231(11) 0.0225(11) 0.0211(10) 0.0098(8) 0.0070(9) 0.0057(9) O2 0.0165(10) 0.0273(12) 0.0271(11) 0.0115(9) 0.0010(9) -0.0013(9) O3 0.0188(10) 0.0254(11) 0.0220(11) -0.0022(9) 0.0055(8) -0.0040(9) O4 0.0252(11) 0.0320(12) 0.0155(10) -0.0014(9) 0.0050(9) -0.0022(9) O5 0.0222(11) 0.0263(11) 0.0199(10) -0.0037(9) 0.0030(9) 0.0000(9) O6 0.0228(11) 0.0191(11) 0.0315(12) -0.0007(9) 0.0030(9) 0.0076(9) O7 0.0319(12) 0.0263(12) 0.0350(12) 0.0115(10) 0.0223(10) 0.0123(9) O8 0.0258(11) 0.0329(12) 0.0215(10) 0.0125(9) 0.0128(9) 0.0093(9) C1 0.0167(14) 0.0200(15) 0.0138(13) 0.0008(11) 0.0072(11) 0.0052(11) C2 0.0212(15) 0.0199(15) 0.0149(13) 0.0048(11) 0.0078(11) 0.0085(12) C3 0.0203(15) 0.0181(14) 0.0206(14) 0.0058(12) 0.0103(12) 0.0014(11) C4 0.0150(14) 0.0206(15) 0.0192(14) 0.0016(12) 0.0079(11) 0.0024(11) C5 0.0194(14) 0.0168(14) 0.0145(13) 0.0009(11) 0.0076(11) 0.0056(11) C6 0.0195(14) 0.0139(14) 0.0181(14) 0.0021(11) 0.0087(11) 0.0037(11) C7 0.0158(14) 0.0188(15) 0.0171(14) 0.0033(11) 0.0047(11) 0.0035(11) C8 0.0195(14) 0.0155(14) 0.0158(14) 0.0050(11) 0.0034(11) 0.0050(11) C9 0.0183(14) 0.0210(15) 0.0195(14) 0.0052(12) 0.0048(12) 0.0026(12) C10 0.0194(15) 0.0231(16) 0.0183(14) 0.0019(12) 0.0023(12) -0.0024(12) C11 0.0237(15) 0.0215(15) 0.0150(14) 0.0039(12) 0.0044(12) 0.0041(12) C12 0.0206(15) 0.0187(15) 0.0165(14) 0.0076(11) 0.0053(12) 0.0037(12) C13 0.0181(14) 0.0155(14) 0.0154(14) 0.0043(11) 0.0008(11) 0.0031(11) C14 0.0220(15) 0.0233(16) 0.0135(13) 0.0051(12) 0.0043(12) 0.0005(12) C15 0.0188(14) 0.0200(15) 0.0151(14) 0.0042(11) 0.0086(11) -0.0008(11) C16 0.0188(14) 0.0228(15) 0.0145(14) -0.0018(12) 0.0061(11) -0.0031(12) C17 0.0236(15) 0.0193(15) 0.0223(15) -0.0019(12) 0.0112(12) 0.0025(12) C18 0.0184(14) 0.0216(15) 0.0228(15) 0.0044(12) 0.0096(12) 0.0028(12) C19 0.0178(14) 0.0199(15) 0.0158(14) 0.0038(11) 0.0088(11) 0.0006(11) C20 0.0192(14) 0.0166(14) 0.0152(13) 0.0023(11) 0.0081(11) -0.0001(11) C21 0.0159(14) 0.0199(15) 0.0173(14) 0.0035(11) 0.0058(11) 0.0018(11) C22 0.0169(14) 0.0194(15) 0.0152(14) 0.0019(11) 0.0030(11) -0.0007(11) C23 0.0208(15) 0.0177(15) 0.0220(15) 0.0019(12) 0.0095(12) 0.0028(12) C24 0.0230(15) 0.0213(15) 0.0240(15) 0.0089(12) 0.0080(12) 0.0070(12) C25 0.0215(15) 0.0209(15) 0.0151(14) 0.0039(11) 0.0052(12) 0.0008(12) C26 0.0141(13) 0.0177(14) 0.0150(13) -0.0003(11) 0.0026(11) -0.0002(11) C27 0.0176(14) 0.0170(14) 0.0151(13) 0.0018(11) 0.0014(11) 0.0008(11) C28 0.0183(14) 0.0179(14) 0.0147(13) 0.0020(11) 0.0045(11) 0.0040(11) C29 0.0206(15) 0.0200(15) 0.0230(15) 0.0044(12) 0.0056(12) 0.0040(12) C30 0.0286(17) 0.0235(17) 0.0362(18) 0.0119(14) 0.0061(14) 0.0065(13) C31 0.0227(15) 0.0235(16) 0.0206(15) 0.0074(12) 0.0055(12) 0.0009(12) C32 0.0382(19) 0.0271(18) 0.0338(18) 0.0151(15) 0.0058(15) 0.0055(15) C33 0.0206(15) 0.0212(15) 0.0189(14) 0.0037(12) 0.0073(12) 0.0005(12) C34 0.0264(17) 0.0268(17) 0.0250(16) 0.0007(13) 0.0060(13) -0.0029(13) C35 0.0209(15) 0.0192(15) 0.0214(15) -0.0006(12) 0.0038(12) 0.0027(12) C36 0.0276(17) 0.0233(16) 0.0253(16) -0.0014(13) 0.0001(13) 0.0001(13) O2S 0.0533(18) 0.082(2) 0.0419(16) 0.0121(15) 0.0042(14) -0.0113(16) C2S 0.037(2) 0.077(3) 0.056(3) 0.019(2) 0.008(2) 0.001(2) O1W 0.054(3) 0.035(3) 0.020(2) 0.008(2) -0.017(2) -0.020(2) O2W 0.0243(18) 0.0213(18) 0.0198(17) 0.0085(14) 0.0096(14) -0.0003(14) O3W 0.019(3) 0.029(3) 0.030(3) 0.000(2) 0.000(2) 0.002(2) O1S 0.076(3) 0.054(2) 0.054(2) 0.0040(18) 0.028(2) -0.012(2) C1S 0.041(6) 0.068(3) 0.046(2) 0.001(2) 0.021(4) -0.012(4) O9 0.107(7) 0.053(3) 0.049(5) 0.008(3) 0.004(4) 0.032(4) O10 0.063(4) 0.026(6) 0.049(3) 0.012(3) 0.010(2) 0.013(3) C41 0.041(5) 0.057(4) 0.032(5) 0.006(3) 0.015(4) 0.020(4) C42 0.032(6) 0.144(7) 0.026(4) 0.008(4) 0.009(5) 0.043(6) C43 0.077(5) 0.088(5) 0.041(4) -0.008(3) 0.011(3) 0.047(4) Cl1 0.0384(11) 0.162(3) 0.0822(14) -0.0591(15) -0.0044(9) 0.0249(13) O1SB 0.076(3) 0.054(2) 0.054(2) 0.0040(18) 0.028(2) -0.012(2) C1SB 0.041(6) 0.068(3) 0.046(2) 0.001(2) 0.021(4) -0.012(4) O9B 0.107(7) 0.053(3) 0.049(5) 0.008(3) 0.004(4) 0.032(4) O10B 0.063(4) 0.026(6) 0.049(3) 0.012(3) 0.010(2) 0.013(3) C41B 0.041(5) 0.057(4) 0.032(5) 0.006(3) 0.015(4) 0.020(4) C42B 0.032(6) 0.144(7) 0.026(4) 0.008(4) 0.009(5) 0.043(6) C43B 0.077(5) 0.088(5) 0.041(4) -0.008(3) 0.011(3) 0.047(4) Cl1B 0.137(6) 0.081(4) 0.089(4) 0.022(3) 0.054(4) 0.057(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 O1 C2 1.381(3) . ? O2 C4 1.378(3) . ? O3 C9 1.382(3) . ? O4 C11 1.380(3) . ? O5 C16 1.380(3) . ? O6 C18 1.369(3) . ? O7 C23 1.382(3) . ? O8 C25 1.390(3) . ? C1 C6 1.392(4) . ? C1 C2 1.393(4) . ? C1 C28 1.525(4) . ? C2 C3 1.382(4) . ? C3 C4 1.393(4) . ? C4 C5 1.393(4) . ? C5 C6 1.397(4) . ? C5 C7 1.530(4) . ? C7 C8 1.534(4) . ? C7 C29 1.538(4) . ? C8 C9 1.391(4) . ? C8 C13 1.394(4) . ? C9 C10 1.390(4) . ? C10 C11 1.389(4) . ? C11 C12 1.395(4) . ? C12 C13 1.392(4) . ? C12 C14 1.529(4) . ? C14 C15 1.522(4) . ? C14 C31 1.530(4) . ? C15 C20 1.395(4) . ? C15 C16 1.402(4) . ? C16 C17 1.387(4) . ? C17 C18 1.385(4) . ? C18 C19 1.400(4) . ? C19 C20 1.392(4) . ? C19 C21 1.523(4) . ? C21 C22 1.533(4) . ? C21 C33 1.535(4) . ? C22 C27 1.396(4) . ? C22 C23 1.397(4) . ? C23 C24 1.387(4) . ? C24 C25 1.382(4) . ? C25 C26 1.390(4) . ? C26 C27 1.394(4) . ? C26 C28 1.530(4) . ? C28 C35 1.530(4) . ? C29 C30 1.525(4) . ? C31 C32 1.535(4) . ? C33 C34 1.524(4) . ? C35 C36 1.524(4) . ? O2S C2S 1.411(5) . ? O1S C1S 1.457(15) . ? O9 C41 1.283(8) . ? O10 C41 1.237(8) . ? C41 C42 1.522(8) . ? C42 C43 1.311(10) . ? C43 Cl1 1.732(7) . ? O1SB C1SB 1.46(2) . ? O9B C41B 1.290(16) . ? O10B C41B 1.259(17) . ? C41B C42B 1.562(17) . ? C42B C43B 1.257(17) . ? C43B Cl1B 1.808(15) . ? 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 C6 C1 C2 117.2(3) . . ? C6 C1 C28 123.0(2) . . ? C2 C1 C28 119.8(2) . . ? O1 C2 C3 120.5(2) . . ? O1 C2 C1 118.1(2) . . ? C3 C2 C1 121.4(2) . . ? C2 C3 C4 119.7(3) . . ? O2 C4 C3 115.1(2) . . ? O2 C4 C5 123.5(2) . . ? C3 C4 C5 121.3(3) . . ? C4 C5 C6 116.8(2) . . ? C4 C5 C7 121.3(2) . . ? C6 C5 C7 121.9(2) . . ? C1 C6 C5 123.6(3) . . ? C5 C7 C8 110.5(2) . . ? C5 C7 C29 113.6(2) . . ? C8 C7 C29 112.0(2) . . ? C9 C8 C13 117.1(3) . . ? C9 C8 C7 121.5(3) . . ? C13 C8 C7 121.4(2) . . ? O3 C9 C10 121.2(3) . . ? O3 C9 C8 117.4(2) . . ? C10 C9 C8 121.4(3) . . ? C11 C10 C9 119.5(3) . . ? O4 C11 C10 121.3(3) . . ? O4 C11 C12 117.4(3) . . ? C10 C11 C12 121.3(3) . . ? C13 C12 C11 117.1(3) . . ? C13 C12 C14 121.3(3) . . ? C11 C12 C14 121.6(2) . . ? C12 C13 C8 123.5(3) . . ? C15 C14 C12 110.4(2) . . ? C15 C14 C31 114.5(2) . . ? C12 C14 C31 112.0(2) . . ? C20 C15 C16 116.4(2) . . ? C20 C15 C14 122.9(3) . . ? C16 C15 C14 120.7(2) . . ? O5 C16 C17 115.7(3) . . ? O5 C16 C15 122.6(2) . . ? C17 C16 C15 121.7(3) . . ? C18 C17 C16 119.8(3) . . ? O6 C18 C17 121.4(3) . . ? O6 C18 C19 117.8(2) . . ? C17 C18 C19 120.8(3) . . ? C20 C19 C18 117.5(3) . . ? C20 C19 C21 123.6(3) . . ? C18 C19 C21 118.9(2) . . ? C19 C20 C15 123.7(3) . . ? C19 C21 C22 110.9(2) . . ? C19 C21 C33 113.9(2) . . ? C22 C21 C33 112.0(2) . . ? C27 C22 C23 116.7(2) . . ? C27 C22 C21 120.4(2) . . ? C23 C22 C21 122.9(2) . . ? O7 C23 C24 115.3(2) . . ? O7 C23 C22 123.6(2) . . ? C24 C23 C22 121.1(3) . . ? C25 C24 C23 119.9(3) . . ? C24 C25 C26 121.6(3) . . ? C24 C25 O8 116.7(2) . . ? C26 C25 O8 121.7(3) . . ? C25 C26 C27 116.7(3) . . ? C25 C26 C28 121.7(2) . . ? C27 C26 C28 121.6(2) . . ? C26 C27 C22 123.9(3) . . ? C1 C28 C26 110.7(2) . . ? C1 C28 C35 113.5(2) . . ? C26 C28 C35 112.4(2) . . ? C30 C29 C7 112.5(2) . . ? C14 C31 C32 111.8(2) . . ? C34 C33 C21 112.7(2) . . ? C36 C35 C28 112.3(2) . . ? O10 C41 O9 127.0(9) . . ? O10 C41 C42 115.2(10) . . ? O9 C41 C42 117.8(7) . . ? C43 C42 C41 118.1(8) . . ? C42 C43 Cl1 121.0(7) . . ? O10B C41B O9B 102(3) . . ? O10B C41B C42B 133(3) . . ? O9B C41B C42B 125(2) . . ? C43B C42B C41B 142(3) . . ? C42B C43B Cl1B 110(2) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.573 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.064 #=======================================END data_CECR-E-HClA-2MeOH-1.5H2O@90k-2h _database_code_depnum_ccdc_archive 'CCDC 629571' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CECR-E-HClA-2MeOH-1.5H2O@90k-2h _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C41 H54 Cl O13.50' _chemical_formula_weight 798.29 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3717(4) _cell_length_b 13.3231(5) _cell_length_c 14.6367(5) _cell_angle_alpha 99.0890(11) _cell_angle_beta 109.3441(10) _cell_angle_gamma 95.2480(11) _cell_volume 2041.34(13) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 675 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.9747 _exptl_absorpt_correction_T_max 0.9841 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14686 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7191 _reflns_number_gt 5640 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+2.3738P] 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 7191 _refine_ls_number_parameters 546 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1753 _refine_ls_wR_factor_gt 0.1638 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.184 _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 O1 O 0.79630(18) 0.60488(14) 0.57895(14) 0.0229(4) Uani 1 1 d . . . O2 O 0.41995(17) 0.60451(15) 0.31321(14) 0.0251(4) Uani 1 1 d . . . O3 O 0.32088(18) 0.65276(15) 0.13108(14) 0.0244(4) Uani 1 1 d . . . O4 O 0.54845(19) 0.61341(16) -0.09486(13) 0.0272(5) Uani 1 1 d . . . O5 O 0.77598(18) 0.54393(15) -0.03752(14) 0.0263(5) Uani 1 1 d . . . O6 O 1.14387(18) 0.54085(15) 0.23557(15) 0.0272(5) Uani 1 1 d . . . O7 O 1.28839(19) 0.59643(15) 0.44331(15) 0.0284(5) Uani 1 1 d . . . O8 O 1.05232(18) 0.63247(15) 0.65267(14) 0.0250(4) Uani 1 1 d . . . C1 C 0.7841(2) 0.7442(2) 0.49416(18) 0.0172(5) Uani 1 1 d . . . C2 C 0.7277(3) 0.6513(2) 0.50508(19) 0.0184(6) Uani 1 1 d . . . C3 C 0.6069(3) 0.6071(2) 0.44409(19) 0.0198(6) Uani 1 1 d . . . H3A H 0.5699 0.5442 0.4530 0.024 Uiso 1 1 calc R . . C4 C 0.5392(2) 0.6548(2) 0.36956(19) 0.0188(6) Uani 1 1 d . . . C5 C 0.5905(2) 0.7480(2) 0.35609(18) 0.0170(5) Uani 1 1 d . . . C6 C 0.7127(2) 0.79017(19) 0.41977(18) 0.0167(5) Uani 1 1 d . . . H6A H 0.7492 0.8538 0.4119 0.020 Uiso 1 1 calc R . . C7 C 0.5166(2) 0.8002(2) 0.27400(18) 0.0177(5) Uani 1 1 d . . . H7A H 0.4262 0.7872 0.2681 0.021 Uiso 1 1 calc R . . C8 C 0.5236(3) 0.7498(2) 0.17430(19) 0.0182(6) Uani 1 1 d . . . C9 C 0.4246(3) 0.6780(2) 0.10564(19) 0.0202(6) Uani 1 1 d . . . C10 C 0.4310(3) 0.6327(2) 0.0155(2) 0.0231(6) Uani 1 1 d . . . H10A H 0.3623 0.5844 -0.0307 0.028 Uiso 1 1 calc R . . C11 C 0.5378(3) 0.6580(2) -0.00686(19) 0.0214(6) Uani 1 1 d . . . C12 C 0.6402(2) 0.7289(2) 0.05998(19) 0.0189(6) Uani 1 1 d . . . C13 C 0.6299(2) 0.77195(19) 0.14947(19) 0.0179(5) Uani 1 1 d . . . H13A H 0.6992 0.8192 0.1963 0.021 Uiso 1 1 calc R . . C14 C 0.7586(3) 0.7575(2) 0.03632(19) 0.0198(6) Uani 1 1 d . . . H14A H 0.7363 0.7313 -0.0362 0.024 Uiso 1 1 calc R . . C15 C 0.8633(2) 0.7007(2) 0.08856(18) 0.0183(6) Uani 1 1 d . . . C16 C 0.8651(3) 0.5980(2) 0.05024(19) 0.0207(6) Uani 1 1 d . . . C17 C 0.9573(3) 0.5439(2) 0.0982(2) 0.0222(6) Uani 1 1 d . . . H17A H 0.9557 0.4740 0.0709 0.027 Uiso 1 1 calc R . . C18 C 1.0517(3) 0.5921(2) 0.1862(2) 0.0211(6) Uani 1 1 d . . . C19 C 1.0553(2) 0.6952(2) 0.22779(19) 0.0179(5) Uani 1 1 d . . . C20 C 0.9604(2) 0.7461(2) 0.17747(18) 0.0179(5) Uani 1 1 d . . . H20A H 0.9616 0.8158 0.2051 0.021 Uiso 1 1 calc R . . C21 C 1.1611(2) 0.7448(2) 0.32460(19) 0.0190(6) Uani 1 1 d . . . H21A H 1.2381 0.7152 0.3226 0.023 Uiso 1 1 calc R . . C22 C 1.1329(2) 0.7143(2) 0.41263(18) 0.0181(6) Uani 1 1 d . . . C23 C 1.1951(3) 0.6441(2) 0.4648(2) 0.0202(6) Uani 1 1 d . . . C24 C 1.1663(3) 0.6178(2) 0.5440(2) 0.0233(6) Uani 1 1 d . . . H24A H 1.2088 0.5693 0.5783 0.028 Uiso 1 1 calc R . . C25 C 1.0758(3) 0.6623(2) 0.57292(19) 0.0207(6) Uani 1 1 d . . . C26 C 1.0133(2) 0.7348(2) 0.52527(18) 0.0176(5) Uani 1 1 d . . . C27 C 1.0423(2) 0.7570(2) 0.44452(19) 0.0185(6) Uani 1 1 d . . . H27A H 0.9978 0.8040 0.4092 0.022 Uiso 1 1 calc R . . C28 C 0.9187(2) 0.7889(2) 0.56085(19) 0.0180(5) Uani 1 1 d . . . H28A H 0.9287 0.7730 0.6273 0.022 Uiso 1 1 calc R . . C29 C 0.5556(3) 0.9177(2) 0.2964(2) 0.0216(6) Uani 1 1 d . . . H29A H 0.5539 0.9466 0.3625 0.026 Uiso 1 1 calc R . . H29B H 0.6432 0.9335 0.2982 0.026 Uiso 1 1 calc R . . C30 C 0.4693(3) 0.9691(2) 0.2199(2) 0.0306(7) Uani 1 1 d . . . H30A H 0.4968 1.0437 0.2378 0.046 Uiso 1 1 calc R . . H30B H 0.3824 0.9539 0.2179 0.046 Uiso 1 1 calc R . . H30C H 0.4732 0.9428 0.1547 0.046 Uiso 1 1 calc R . . C31 C 0.7963(3) 0.8741(2) 0.0544(2) 0.0244(6) Uani 1 1 d . . . H31A H 0.8746 0.8893 0.0402 0.029 Uiso 1 1 calc R . . H31B H 0.8139 0.9041 0.1248 0.029 Uiso 1 1 calc R . . C32 C 0.6923(3) 0.9243(2) -0.0105(2) 0.0339(7) Uani 1 1 d . . . H32A H 0.7202 0.9986 0.0019 0.051 Uiso 1 1 calc R . . H32B H 0.6156 0.9117 0.0052 0.051 Uiso 1 1 calc R . . H32C H 0.6745 0.8947 -0.0803 0.051 Uiso 1 1 calc R . . C33 C 1.1939(3) 0.8615(2) 0.3378(2) 0.0210(6) Uani 1 1 d . . . H33A H 1.2098 0.8772 0.2786 0.025 Uiso 1 1 calc R . . H33B H 1.1208 0.8940 0.3427 0.025 Uiso 1 1 calc R . . C34 C 1.3094(3) 0.9077(2) 0.4294(2) 0.0281(7) Uani 1 1 d . . . H34A H 1.3259 0.9823 0.4348 0.042 Uiso 1 1 calc R . . H34B H 1.3827 0.8773 0.4240 0.042 Uiso 1 1 calc R . . H34C H 1.2938 0.8931 0.4883 0.042 Uiso 1 1 calc R . . C35 C 0.9473(3) 0.9063(2) 0.5759(2) 0.0223(6) Uani 1 1 d . . . H35A H 0.9454 0.9250 0.5126 0.027 Uiso 1 1 calc R . . H35B H 0.8807 0.9372 0.5948 0.027 Uiso 1 1 calc R . . C36 C 1.0755(3) 0.9509(2) 0.6552(2) 0.0294(7) Uani 1 1 d . . . H36A H 1.0898 1.0258 0.6617 0.044 Uiso 1 1 calc R . . H36B H 1.1419 0.9212 0.6364 0.044 Uiso 1 1 calc R . . H36C H 1.0770 0.9344 0.7185 0.044 Uiso 1 1 calc R . . O2S O 0.7761(3) 0.2709(3) 0.1714(2) 0.0666(9) Uani 1 1 d . . . H2S H 0.8255 0.2921 0.2247 0.100 Uiso 1 1 d R . . C2S C 0.6777(4) 0.2056(4) 0.1806(3) 0.0593(11) Uani 1 1 d . . . H2S1 H 0.7113 0.1737 0.2379 0.089 Uiso 1 1 calc R . . H2S2 H 0.6404 0.1519 0.1207 0.089 Uiso 1 1 calc R . . H2S3 H 0.6129 0.2458 0.1896 0.089 Uiso 1 1 calc R . . O1W O 0.3244(5) 0.5391(3) 0.7710(3) 0.0436(13) Uani 0.50 1 d P A 1 H1WA H 0.2587 0.4898 0.7207 0.065 Uiso 0.50 1 d PR A 1 H1WB H 0.3121 0.5727 0.8313 0.065 Uiso 0.50 1 d PR A 1 O2W O 0.2365(3) 0.4466(2) 0.7422(2) 0.0211(7) Uani 0.60 1 d P B 2 H2WA H 0.1895 0.3876 0.7223 0.032 Uiso 0.60 1 d PR B 2 H2WB H 0.2409 0.4649 0.6886 0.032 Uiso 0.60 1 d PR B 2 O3W O 0.3574(5) 0.4625(4) 0.8095(4) 0.0324(12) Uani 0.40 1 d P C 3 H3WA H 0.2783 0.4517 0.8132 0.049 Uiso 0.40 1 d PR C 3 H3WB H 0.3585 0.4883 0.7598 0.049 Uiso 0.40 1 d PR C 3 H1O H 0.7591 0.5511 0.5746 0.049 Uiso 1 1 d R . . H2O H 0.3930 0.6257 0.2619 0.049 Uiso 1 1 d R . . H3O H 0.2835 0.6088 0.0989 0.049 Uiso 1 1 d R . . H40 H 0.4840 0.5733 -0.1294 0.049 Uiso 1 1 d R . . H5O H 0.7164 0.5710 -0.0535 0.049 Uiso 1 1 d R . . H6O H 1.1331 0.4854 0.2097 0.049 Uiso 1 1 d R . . H7O H 1.2913 0.6036 0.3915 0.049 Uiso 1 1 d R . . H8O H 0.9788 0.6243 0.6420 0.049 Uiso 1 1 d R . . O1S O 0.8923(4) 0.1481(3) 0.0698(3) 0.0661(11) Uani 0.730(5) 1 d PD D 1 H1S H 0.8526 0.1908 0.1058 0.099 Uiso 0.730(5) 1 d PR D 1 C1S C 0.8732(7) 0.1794(10) -0.0241(7) 0.054(2) Uani 0.730(5) 1 d PD D 1 H1S1 H 0.7952 0.2093 -0.0437 0.081 Uiso 0.730(5) 1 calc PR D 1 H1S2 H 0.8670 0.1193 -0.0746 0.081 Uiso 0.730(5) 1 calc PR D 1 H1S3 H 0.9446 0.2307 -0.0174 0.081 Uiso 0.730(5) 1 calc PR D 1 O9 O 1.1125(12) 0.1720(7) 0.1719(7) 0.082(2) Uani 0.680(4) 1 d PD E 1 H9O H 1.0195 0.1622 0.1266 0.123 Uiso 0.680(4) 1 d PR E 1 O10 O 1.0995(14) 0.3401(9) 0.1713(10) 0.0486(19) Uani 0.680(4) 1 d PD E 1 C41 C 1.1565(6) 0.2683(7) 0.1951(8) 0.045(2) Uani 0.680(4) 1 d PD E 1 C42 C 1.2963(6) 0.3010(9) 0.2568(7) 0.069(3) Uani 0.680(4) 1 d PD E 1 H42A H 1.3370 0.3695 0.2671 0.083 Uiso 0.680(4) 1 calc PR E 1 C43 C 1.3577(7) 0.2299(6) 0.2950(5) 0.077(2) Uani 0.680(4) 1 d PD E 1 H43A H 1.3155 0.1614 0.2816 0.092 Uiso 0.680(4) 1 calc PR E 1 Cl1 Cl 1.51580(18) 0.2609(2) 0.36990(17) 0.1168(13) Uani 0.680(4) 1 d PD E 1 O1SB O 0.8809(12) 0.2812(8) 0.0447(8) 0.0661(11) Uani 0.270(5) 1 d PD D 2 H1SB H 0.9676 0.2961 0.0874 0.099 Uiso 0.270(5) 1 d PR D 2 C1SB C 0.838(3) 0.184(3) -0.026(2) 0.054(2) Uani 0.270(5) 1 d PD D 2 H1S4 H 0.9103 0.1507 -0.0282 0.081 Uiso 0.270(5) 1 calc PR D 2 H1S5 H 0.7915 0.1966 -0.0918 0.081 Uiso 0.270(5) 1 calc PR D 2 H1S6 H 0.7816 0.1390 -0.0060 0.081 Uiso 0.270(5) 1 calc PR D 2 O9B O 1.153(3) 0.1849(17) 0.1995(18) 0.082(2) Uani 0.320(4) 1 d PD E 2 H9OB H 1.0736 0.1697 0.1713 0.123 Uiso 0.320(4) 1 d PR E 2 O10B O 1.112(3) 0.318(2) 0.163(2) 0.0486(19) Uani 0.320(4) 1 d PD E 2 C41B C 1.2024(19) 0.2795(19) 0.212(2) 0.045(2) Uani 0.320(4) 1 d PD E 2 C42B C 1.3457(16) 0.323(2) 0.2722(17) 0.069(3) Uani 0.320(4) 1 d PD E 2 H42B H 1.3674 0.3855 0.2544 0.083 Uiso 0.320(4) 1 calc PR E 2 C43B C 1.4400(16) 0.3024(11) 0.3347(10) 0.077(2) Uani 0.320(4) 1 d PD E 2 H43B H 1.5186 0.3468 0.3648 0.092 Uiso 0.320(4) 1 calc PR E 2 Cl1B Cl 1.4069(5) 0.1759(4) 0.3610(4) 0.091(2) Uani 0.320(4) 1 d PD E 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 O1 0.0240(10) 0.0238(10) 0.0226(10) 0.0103(8) 0.0072(8) 0.0061(8) O2 0.0165(10) 0.0267(11) 0.0276(11) 0.0102(8) 0.0008(8) -0.0011(8) O3 0.0202(10) 0.0265(11) 0.0219(10) -0.0023(8) 0.0066(8) -0.0032(8) O4 0.0260(11) 0.0342(12) 0.0151(9) -0.0016(8) 0.0043(8) -0.0033(9) O5 0.0230(11) 0.0282(11) 0.0199(10) -0.0046(8) 0.0030(8) -0.0004(8) O6 0.0236(11) 0.0195(10) 0.0321(11) -0.0008(8) 0.0029(9) 0.0076(8) O7 0.0326(12) 0.0279(11) 0.0359(12) 0.0116(9) 0.0225(10) 0.0117(9) O8 0.0259(11) 0.0333(11) 0.0213(10) 0.0118(8) 0.0113(8) 0.0086(9) C1 0.0172(13) 0.0197(13) 0.0147(12) 0.0002(10) 0.0066(11) 0.0050(10) C2 0.0218(14) 0.0205(14) 0.0157(13) 0.0045(10) 0.0083(11) 0.0093(11) C3 0.0202(14) 0.0186(13) 0.0221(14) 0.0046(11) 0.0096(11) 0.0018(11) C4 0.0156(13) 0.0204(14) 0.0203(13) 0.0013(11) 0.0073(11) 0.0030(11) C5 0.0188(13) 0.0182(13) 0.0155(13) 0.0015(10) 0.0079(11) 0.0060(10) C6 0.0197(13) 0.0148(13) 0.0165(13) 0.0016(10) 0.0081(11) 0.0027(10) C7 0.0155(13) 0.0194(13) 0.0170(13) 0.0031(10) 0.0041(11) 0.0037(10) C8 0.0212(14) 0.0167(13) 0.0156(13) 0.0056(10) 0.0032(11) 0.0064(11) C9 0.0193(14) 0.0215(14) 0.0187(13) 0.0044(11) 0.0050(11) 0.0031(11) C10 0.0207(14) 0.0236(14) 0.0180(13) 0.0009(11) 0.0006(11) -0.0019(11) C11 0.0247(15) 0.0234(14) 0.0139(13) 0.0038(11) 0.0043(11) 0.0021(11) C12 0.0198(14) 0.0199(14) 0.0170(13) 0.0070(11) 0.0044(11) 0.0046(11) C13 0.0185(13) 0.0158(13) 0.0156(13) 0.0040(10) 0.0009(11) 0.0022(10) C14 0.0214(14) 0.0222(14) 0.0136(12) 0.0032(10) 0.0042(11) 0.0000(11) C15 0.0199(14) 0.0211(14) 0.0155(13) 0.0044(10) 0.0091(11) -0.0002(11) C16 0.0205(14) 0.0245(14) 0.0151(13) -0.0011(11) 0.0075(11) -0.0029(11) C17 0.0240(15) 0.0189(14) 0.0234(14) -0.0028(11) 0.0113(12) 0.0022(11) C18 0.0201(14) 0.0225(14) 0.0219(14) 0.0033(11) 0.0093(11) 0.0038(11) C19 0.0191(13) 0.0198(13) 0.0161(13) 0.0025(10) 0.0091(11) 0.0001(11) C20 0.0205(14) 0.0184(13) 0.0162(13) 0.0033(10) 0.0089(11) 0.0008(11) C21 0.0171(13) 0.0217(14) 0.0178(13) 0.0037(11) 0.0059(11) 0.0023(11) C22 0.0175(13) 0.0181(13) 0.0154(13) 0.0005(10) 0.0037(11) -0.0006(10) C23 0.0193(14) 0.0192(14) 0.0224(14) 0.0014(11) 0.0086(11) 0.0040(11) C24 0.0245(15) 0.0227(15) 0.0249(14) 0.0079(11) 0.0089(12) 0.0076(12) C25 0.0221(14) 0.0231(14) 0.0159(13) 0.0038(11) 0.0057(11) 0.0017(11) C26 0.0150(13) 0.0186(13) 0.0156(13) 0.0000(10) 0.0027(10) 0.0004(10) C27 0.0178(13) 0.0171(13) 0.0165(13) 0.0020(10) 0.0018(11) 0.0015(10) C28 0.0184(14) 0.0198(14) 0.0150(13) 0.0025(10) 0.0050(11) 0.0041(11) C29 0.0198(14) 0.0202(14) 0.0227(14) 0.0026(11) 0.0053(11) 0.0042(11) C30 0.0305(17) 0.0231(15) 0.0356(17) 0.0107(13) 0.0053(14) 0.0070(13) C31 0.0257(15) 0.0234(15) 0.0218(14) 0.0081(11) 0.0046(12) 0.0001(12) C32 0.0388(18) 0.0280(16) 0.0334(17) 0.0151(13) 0.0061(15) 0.0063(14) C33 0.0201(14) 0.0223(14) 0.0201(14) 0.0032(11) 0.0075(11) 0.0011(11) C34 0.0257(16) 0.0266(16) 0.0256(15) 0.0002(12) 0.0047(13) -0.0028(12) C35 0.0221(14) 0.0192(14) 0.0219(14) 0.0009(11) 0.0043(12) 0.0036(11) C36 0.0277(16) 0.0233(15) 0.0271(15) -0.0022(12) 0.0004(13) 0.0004(12) O2S 0.0570(18) 0.085(2) 0.0426(16) 0.0108(15) 0.0046(14) -0.0129(16) C2S 0.041(2) 0.077(3) 0.056(3) 0.018(2) 0.0106(19) 0.002(2) O1W 0.056(3) 0.033(2) 0.015(2) 0.0068(18) -0.017(2) -0.019(2) O2W 0.0259(17) 0.0211(16) 0.0182(15) 0.0067(13) 0.0099(14) 0.0000(13) O3W 0.025(3) 0.031(3) 0.033(3) 0.001(2) 0.002(2) 0.005(2) O1S 0.082(3) 0.058(2) 0.055(2) 0.0019(18) 0.031(2) -0.015(2) C1S 0.039(5) 0.072(3) 0.049(2) 0.000(2) 0.024(4) -0.011(4) O9 0.122(9) 0.056(3) 0.054(6) 0.008(4) 0.008(4) 0.040(4) O10 0.067(4) 0.026(6) 0.048(3) 0.009(4) 0.012(2) 0.012(3) C41 0.044(6) 0.062(4) 0.036(5) 0.007(3) 0.018(5) 0.024(5) C42 0.033(6) 0.149(7) 0.028(4) 0.009(4) 0.011(5) 0.045(6) C43 0.091(6) 0.092(6) 0.042(4) -0.007(3) 0.014(3) 0.056(4) Cl1 0.0415(11) 0.173(3) 0.0856(15) -0.0648(16) -0.0047(10) 0.0272(13) O1SB 0.082(3) 0.058(2) 0.055(2) 0.0019(18) 0.031(2) -0.015(2) C1SB 0.039(5) 0.072(3) 0.049(2) 0.000(2) 0.024(4) -0.011(4) O9B 0.122(9) 0.056(3) 0.054(6) 0.008(4) 0.008(4) 0.040(4) O10B 0.067(4) 0.026(6) 0.048(3) 0.009(4) 0.012(2) 0.012(3) C41B 0.044(6) 0.062(4) 0.036(5) 0.007(3) 0.018(5) 0.024(5) C42B 0.033(6) 0.149(7) 0.028(4) 0.009(4) 0.011(5) 0.045(6) C43B 0.091(6) 0.092(6) 0.042(4) -0.007(3) 0.014(3) 0.056(4) Cl1B 0.126(5) 0.078(3) 0.085(3) 0.016(2) 0.047(3) 0.051(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.378(3) . ? O2 C4 1.373(3) . ? O3 C9 1.379(3) . ? O4 C11 1.379(3) . ? O5 C16 1.381(3) . ? O6 C18 1.369(3) . ? O7 C23 1.382(3) . ? O8 C25 1.387(3) . ? C1 C6 1.391(4) . ? C1 C2 1.398(4) . ? C1 C28 1.520(4) . ? C2 C3 1.380(4) . ? C3 C4 1.392(4) . ? C4 C5 1.394(4) . ? C5 C6 1.397(4) . ? C5 C7 1.528(3) . ? C7 C8 1.537(4) . ? C7 C29 1.539(4) . ? C8 C13 1.393(4) . ? C8 C9 1.393(4) . ? C9 C10 1.390(4) . ? C10 C11 1.385(4) . ? C11 C12 1.399(4) . ? C12 C13 1.392(4) . ? C12 C14 1.528(4) . ? C14 C15 1.522(4) . ? C14 C31 1.531(4) . ? C15 C20 1.398(4) . ? C15 C16 1.399(4) . ? C16 C17 1.386(4) . ? C17 C18 1.385(4) . ? C18 C19 1.402(4) . ? C19 C20 1.390(4) . ? C19 C21 1.524(4) . ? C21 C22 1.531(4) . ? C21 C33 1.531(4) . ? C22 C27 1.395(4) . ? C22 C23 1.395(4) . ? C23 C24 1.390(4) . ? C24 C25 1.382(4) . ? C25 C26 1.391(4) . ? C26 C27 1.394(4) . ? C26 C28 1.531(4) . ? C28 C35 1.533(4) . ? C29 C30 1.525(4) . ? C31 C32 1.533(4) . ? C33 C34 1.526(4) . ? C35 C36 1.526(4) . ? O2S C2S 1.410(5) . ? O1S C1S 1.453(14) . ? O9 C41 1.282(8) . ? O10 C41 1.235(9) . ? C41 C42 1.526(8) . ? C42 C43 1.313(10) . ? C43 Cl1 1.738(8) . ? O1SB C1SB 1.45(2) . ? O9B C41B 1.289(16) . ? O10B C41B 1.254(17) . ? C41B C42B 1.574(16) . ? C42B C43B 1.242(16) . ? C43B Cl1B 1.821(15) . ? 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 C6 C1 C2 117.1(2) . . ? C6 C1 C28 123.2(2) . . ? C2 C1 C28 119.7(2) . . ? O1 C2 C3 120.8(2) . . ? O1 C2 C1 118.0(2) . . ? C3 C2 C1 121.2(2) . . ? C2 C3 C4 120.0(2) . . ? O2 C4 C3 115.3(2) . . ? O2 C4 C5 123.6(2) . . ? C3 C4 C5 121.1(2) . . ? C4 C5 C6 117.0(2) . . ? C4 C5 C7 121.2(2) . . ? C6 C5 C7 121.8(2) . . ? C1 C6 C5 123.7(2) . . ? C5 C7 C8 110.5(2) . . ? C5 C7 C29 113.6(2) . . ? C8 C7 C29 111.8(2) . . ? C13 C8 C9 117.0(2) . . ? C13 C8 C7 121.6(2) . . ? C9 C8 C7 121.3(2) . . ? O3 C9 C10 121.3(2) . . ? O3 C9 C8 117.5(2) . . ? C10 C9 C8 121.2(3) . . ? C11 C10 C9 119.9(2) . . ? O4 C11 C10 121.5(2) . . ? O4 C11 C12 117.3(2) . . ? C10 C11 C12 121.1(2) . . ? C13 C12 C11 117.0(2) . . ? C13 C12 C14 121.3(2) . . ? C11 C12 C14 121.7(2) . . ? C12 C13 C8 123.7(2) . . ? C15 C14 C12 110.4(2) . . ? C15 C14 C31 114.6(2) . . ? C12 C14 C31 111.9(2) . . ? C20 C15 C16 116.3(2) . . ? C20 C15 C14 122.8(2) . . ? C16 C15 C14 120.9(2) . . ? O5 C16 C17 115.6(2) . . ? O5 C16 C15 122.5(2) . . ? C17 C16 C15 121.9(2) . . ? C18 C17 C16 119.8(3) . . ? O6 C18 C17 121.3(2) . . ? O6 C18 C19 117.8(2) . . ? C17 C18 C19 120.9(3) . . ? C20 C19 C18 117.3(2) . . ? C20 C19 C21 123.8(2) . . ? C18 C19 C21 118.9(2) . . ? C19 C20 C15 123.9(2) . . ? C19 C21 C22 110.8(2) . . ? C19 C21 C33 113.6(2) . . ? C22 C21 C33 112.2(2) . . ? C27 C22 C23 116.8(2) . . ? C27 C22 C21 120.4(2) . . ? C23 C22 C21 122.7(2) . . ? O7 C23 C24 115.2(2) . . ? O7 C23 C22 123.8(2) . . ? C24 C23 C22 121.0(2) . . ? C25 C24 C23 120.0(3) . . ? C24 C25 O8 116.8(2) . . ? C24 C25 C26 121.3(2) . . ? O8 C25 C26 121.9(2) . . ? C25 C26 C27 116.9(2) . . ? C25 C26 C28 121.5(2) . . ? C27 C26 C28 121.6(2) . . ? C26 C27 C22 123.8(2) . . ? C1 C28 C26 110.8(2) . . ? C1 C28 C35 113.5(2) . . ? C26 C28 C35 112.3(2) . . ? C30 C29 C7 112.4(2) . . ? C14 C31 C32 111.7(2) . . ? C34 C33 C21 112.7(2) . . ? C36 C35 C28 112.5(2) . . ? O10 C41 O9 127.6(10) . . ? O10 C41 C42 114.4(11) . . ? O9 C41 C42 118.0(8) . . ? C43 C42 C41 116.9(9) . . ? C42 C43 Cl1 120.2(7) . . ? O10B C41B O9B 103(3) . . ? O10B C41B C42B 133(3) . . ? O9B C41B C42B 124(2) . . ? C43B C42B C41B 141(3) . . ? C42B C43B Cl1B 110.7(19) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.654 _refine_diff_density_min -0.774 _refine_diff_density_rms 0.067 #=======================================END data_CECR-E-HClA-2MeOH-1.5H2O@90k-6h _database_code_depnum_ccdc_archive 'CCDC 629572' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CECR-E-HClA-2MeOH-1.5H2O@90k-6h _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C41 H54 Cl O13.50' _chemical_formula_weight 798.29 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3799(5) _cell_length_b 13.3742(6) _cell_length_c 14.6526(6) _cell_angle_alpha 99.0913(14) _cell_angle_beta 109.7794(13) _cell_angle_gamma 95.1761(14) _cell_volume 2047.22(15) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 675 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 0.158 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.9747 _exptl_absorpt_correction_T_max 0.9841 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12241 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7091 _reflns_number_gt 5161 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+2.3738P] 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 7091 _refine_ls_number_parameters 547 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0932 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1882 _refine_ls_wR_factor_gt 0.1715 _refine_ls_goodness_of_fit_ref 1.200 _refine_ls_restrained_S_all 1.200 _refine_ls_shift/su_max 0.027 _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 O1 O 0.7983(2) 0.60559(16) 0.57981(15) 0.0290(5) Uani 1 1 d . . . O2 O 0.41954(19) 0.60517(16) 0.31323(16) 0.0313(5) Uani 1 1 d . . . O3 O 0.3199(2) 0.65163(16) 0.13051(16) 0.0308(5) Uani 1 1 d . . . O4 O 0.5457(2) 0.61372(17) -0.09529(15) 0.0350(6) Uani 1 1 d . . . O5 O 0.7739(2) 0.54522(17) -0.03851(16) 0.0333(5) Uani 1 1 d . . . O6 O 1.1433(2) 0.54155(16) 0.23563(17) 0.0346(6) Uani 1 1 d . . . O7 O 1.2879(2) 0.59613(17) 0.44332(18) 0.0363(6) Uani 1 1 d . . . O8 O 1.0546(2) 0.63271(17) 0.65318(16) 0.0323(5) Uani 1 1 d . . . C1 C 0.7855(3) 0.7441(2) 0.4950(2) 0.0216(6) Uani 1 1 d . . . C2 C 0.7291(3) 0.6516(2) 0.5058(2) 0.0237(6) Uani 1 1 d . . . C3 C 0.6074(3) 0.6075(2) 0.4444(2) 0.0253(7) Uani 1 1 d . . . H3A H 0.5704 0.5449 0.4533 0.030 Uiso 1 1 calc R . . C4 C 0.5395(3) 0.6549(2) 0.3700(2) 0.0233(6) Uani 1 1 d . . . C5 C 0.5907(3) 0.7479(2) 0.3564(2) 0.0206(6) Uani 1 1 d . . . C6 C 0.7135(3) 0.7898(2) 0.4197(2) 0.0214(6) Uani 1 1 d . . . H6A H 0.7501 0.8528 0.4113 0.026 Uiso 1 1 calc R . . C7 C 0.5163(3) 0.7992(2) 0.2739(2) 0.0229(6) Uani 1 1 d . . . H7A H 0.4258 0.7862 0.2677 0.027 Uiso 1 1 calc R . . C8 C 0.5228(3) 0.7492(2) 0.1741(2) 0.0227(6) Uani 1 1 d . . . C9 C 0.4235(3) 0.6774(2) 0.1052(2) 0.0251(7) Uani 1 1 d . . . C10 C 0.4290(3) 0.6327(2) 0.0152(2) 0.0289(7) Uani 1 1 d . . . H10A H 0.3599 0.5847 -0.0313 0.035 Uiso 1 1 calc R . . C11 C 0.5357(3) 0.6580(2) -0.0071(2) 0.0271(7) Uani 1 1 d . . . C12 C 0.6383(3) 0.7288(2) 0.0598(2) 0.0243(7) Uani 1 1 d . . . C13 C 0.6284(3) 0.7718(2) 0.1495(2) 0.0228(6) Uani 1 1 d . . . H13A H 0.6978 0.8193 0.1964 0.027 Uiso 1 1 calc R . . C14 C 0.7566(3) 0.7575(2) 0.0362(2) 0.0259(7) Uani 1 1 d . . . H14A H 0.7336 0.7315 -0.0365 0.031 Uiso 1 1 calc R . . C15 C 0.8617(3) 0.7009(2) 0.0884(2) 0.0239(6) Uani 1 1 d . . . C16 C 0.8637(3) 0.5984(2) 0.0500(2) 0.0260(7) Uani 1 1 d . . . C17 C 0.9560(3) 0.5451(2) 0.0979(2) 0.0280(7) Uani 1 1 d . . . H17A H 0.9544 0.4755 0.0703 0.034 Uiso 1 1 calc R . . C18 C 1.0509(3) 0.5925(2) 0.1860(2) 0.0271(7) Uani 1 1 d . . . C19 C 1.0546(3) 0.6957(2) 0.2277(2) 0.0224(6) Uani 1 1 d . . . C20 C 0.9596(3) 0.7463(2) 0.1774(2) 0.0217(6) Uani 1 1 d . . . H20A H 0.9610 0.8158 0.2049 0.026 Uiso 1 1 calc R . . C21 C 1.1604(3) 0.7445(2) 0.3249(2) 0.0228(6) Uani 1 1 d . . . H21A H 1.2375 0.7151 0.3232 0.027 Uiso 1 1 calc R . . C22 C 1.1327(3) 0.7143(2) 0.4128(2) 0.0231(6) Uani 1 1 d . . . C23 C 1.1954(3) 0.6440(2) 0.4653(2) 0.0263(7) Uani 1 1 d . . . C24 C 1.1669(3) 0.6179(2) 0.5442(2) 0.0294(7) Uani 1 1 d . . . H24A H 1.2092 0.5692 0.5783 0.035 Uiso 1 1 calc R . . C25 C 1.0778(3) 0.6623(2) 0.5733(2) 0.0262(7) Uani 1 1 d . . . C26 C 1.0146(3) 0.7351(2) 0.5258(2) 0.0218(6) Uani 1 1 d . . . C27 C 1.0428(3) 0.7568(2) 0.4454(2) 0.0218(6) Uani 1 1 d . . . H27A H 0.9979 0.8037 0.4102 0.026 Uiso 1 1 calc R . . C28 C 0.9203(3) 0.7890(2) 0.5616(2) 0.0222(6) Uani 1 1 d . . . H28A H 0.9313 0.7733 0.6283 0.027 Uiso 1 1 calc R . . C29 C 0.5549(3) 0.9167(2) 0.2959(2) 0.0263(7) Uani 1 1 d . . . H29A H 0.5536 0.9457 0.3620 0.032 Uiso 1 1 calc R . . H29B H 0.6425 0.9325 0.2979 0.032 Uiso 1 1 calc R . . C30 C 0.4684(3) 0.9673(2) 0.2194(3) 0.0367(8) Uani 1 1 d . . . H30A H 0.4958 1.0417 0.2373 0.055 Uiso 1 1 calc R . . H30B H 0.3815 0.9521 0.2172 0.055 Uiso 1 1 calc R . . H30C H 0.4720 0.9410 0.1542 0.055 Uiso 1 1 calc R . . C31 C 0.7939(3) 0.8740(2) 0.0544(2) 0.0299(7) Uani 1 1 d . . . H31A H 0.8115 0.9037 0.1249 0.036 Uiso 1 1 calc R . . H31B H 0.8724 0.8893 0.0408 0.036 Uiso 1 1 calc R . . C32 C 0.6906(4) 0.9239(3) -0.0105(3) 0.0426(9) Uani 1 1 d . . . H32A H 0.7188 0.9978 0.0021 0.064 Uiso 1 1 calc R . . H32B H 0.6138 0.9115 0.0049 0.064 Uiso 1 1 calc R . . H32C H 0.6726 0.8944 -0.0803 0.064 Uiso 1 1 calc R . . C33 C 1.1934(3) 0.8613(2) 0.3388(2) 0.0261(7) Uani 1 1 d . . . H33A H 1.2084 0.8774 0.2795 0.031 Uiso 1 1 calc R . . H33B H 1.1206 0.8938 0.3443 0.031 Uiso 1 1 calc R . . C34 C 1.3099(3) 0.9068(3) 0.4302(2) 0.0336(8) Uani 1 1 d . . . H34A H 1.3266 0.9812 0.4358 0.050 Uiso 1 1 calc R . . H34B H 1.3828 0.8764 0.4244 0.050 Uiso 1 1 calc R . . H34C H 1.2951 0.8923 0.4892 0.050 Uiso 1 1 calc R . . C35 C 0.9493(3) 0.9061(2) 0.5765(2) 0.0270(7) Uani 1 1 d . . . H35A H 0.9467 0.9244 0.5130 0.032 Uiso 1 1 calc R . . H35B H 0.8829 0.9370 0.5953 0.032 Uiso 1 1 calc R . . C36 C 1.0770(3) 0.9505(2) 0.6553(2) 0.0355(8) Uani 1 1 d . . . H36A H 1.0911 1.0251 0.6616 0.053 Uiso 1 1 calc R . . H36B H 1.1433 0.9210 0.6365 0.053 Uiso 1 1 calc R . . H36C H 1.0794 0.9342 0.7187 0.053 Uiso 1 1 calc R . . O2S O 0.7754(4) 0.2717(3) 0.1705(3) 0.0689(14) Uani 0.843(8) 1 d PD A 1 H2S H 0.8247 0.2928 0.2238 0.103 Uiso 0.843(8) 1 d PR A 1 O2SB O 0.7940(4) 0.2114(4) 0.1726(4) 0.0689(14) Uani 0.157(8) 1 d PD A 2 H2SB H 0.8439 0.2626 0.2300 0.103 Uiso 0.157(8) 1 d PR A 2 C2S C 0.6767(4) 0.2056(4) 0.1797(4) 0.0698(14) Uani 1 1 d RD . . H2S1 H 0.7091 0.1732 0.2369 0.105 Uiso 1 1 d R . . H2S2 H 0.6372 0.1525 0.1195 0.105 Uiso 1 1 d R . . H2S3 H 0.6138 0.2476 0.1889 0.105 Uiso 1 1 d R . . O1W O 0.3176(6) 0.5393(4) 0.7707(4) 0.0639(19) Uani 0.50 1 d P B 1 H1WA H 0.2518 0.4900 0.7204 0.096 Uiso 0.50 1 d PR B 1 H1WB H 0.3052 0.5729 0.8309 0.096 Uiso 0.50 1 d PR B 1 O2W O 0.2354(3) 0.4454(3) 0.7416(2) 0.0271(8) Uani 0.60 1 d P C 2 H2WA H 0.1885 0.3864 0.7217 0.041 Uiso 0.60 1 d PR C 2 H2WB H 0.2399 0.4637 0.6879 0.041 Uiso 0.60 1 d PR C 2 O3W O 0.3563(5) 0.4616(4) 0.8088(4) 0.0395(14) Uani 0.40 1 d P D 3 H3WA H 0.2772 0.4508 0.8125 0.059 Uiso 0.40 1 d PR D 3 H3WB H 0.3574 0.4874 0.7591 0.059 Uiso 0.40 1 d PR D 3 H1O H 0.7580 0.5502 0.5739 0.059 Uiso 1 1 d R . . H2O H 0.3919 0.6248 0.2612 0.059 Uiso 1 1 d R . . H3O H 0.2824 0.6079 0.0982 0.059 Uiso 1 1 d R . . H40 H 0.4829 0.5724 -0.1301 0.059 Uiso 1 1 d R . . H5O H 0.7153 0.5701 -0.0542 0.059 Uiso 1 1 d R . . H6O H 1.1320 0.4845 0.2090 0.059 Uiso 1 1 d R . . H7O H 1.2902 0.6027 0.3908 0.059 Uiso 1 1 d R . . H8O H 0.9777 0.6234 0.6413 0.059 Uiso 1 1 d R . . O1S O 0.8951(5) 0.1475(3) 0.0696(3) 0.0838(14) Uani 0.782(5) 1 d PD E 1 H1S H 0.8555 0.1902 0.1056 0.126 Uiso 0.782(5) 1 d PR E 1 C1S C 0.871(2) 0.1790(14) -0.0240(11) 0.077(3) Uani 0.782(5) 1 d PD E 1 H1S1 H 0.7930 0.2085 -0.0417 0.115 Uiso 0.782(5) 1 calc PR E 1 H1S2 H 0.8634 0.1194 -0.0753 0.115 Uiso 0.782(5) 1 calc PR E 1 H1S3 H 0.9419 0.2304 -0.0185 0.115 Uiso 0.782(5) 1 calc PR E 1 O9 O 1.1191(19) 0.1740(9) 0.1698(11) 0.096(3) Uani 0.597(4) 1 d PD F 1 H9O H 1.0261 0.1642 0.1245 0.144 Uiso 0.597(4) 1 d PR F 1 O10 O 1.1087(13) 0.3283(7) 0.1733(11) 0.0573(18) Uani 0.597(4) 1 d PD F 1 C41 C 1.1794(13) 0.2701(9) 0.2034(16) 0.057(2) Uani 0.597(4) 1 d PD F 1 C42 C 1.3160(16) 0.3235(19) 0.262(2) 0.100(4) Uani 0.597(4) 1 d PD F 1 H42A H 1.3568 0.3919 0.2740 0.120 Uiso 0.597(4) 1 calc PR F 1 C43 C 1.3599(8) 0.2315(7) 0.2932(6) 0.077(2) Uani 0.597(4) 1 d PD F 1 H43A H 1.3103 0.1655 0.2751 0.092 Uiso 0.597(4) 1 calc PR F 1 Cl1 Cl 1.5185(2) 0.2622(3) 0.3691(2) 0.1227(15) Uani 0.597(4) 1 d PD F 1 O1SB O 0.8895(18) 0.2783(12) 0.0508(12) 0.0838(14) Uani 0.218(5) 1 d PD E 2 H1SB H 0.9763 0.2932 0.0936 0.126 Uiso 0.218(5) 1 d PR E 2 C1SB C 0.858(8) 0.183(5) -0.021(4) 0.077(3) Uani 0.218(5) 1 d PD E 2 H1S4 H 0.9358 0.1553 -0.0181 0.115 Uiso 0.218(5) 1 calc PR E 2 H1S5 H 0.8151 0.1954 -0.0871 0.115 Uiso 0.218(5) 1 calc PR E 2 H1S6 H 0.8025 0.1337 -0.0050 0.115 Uiso 0.218(5) 1 calc PR E 2 O9B O 1.153(3) 0.1886(15) 0.1988(19) 0.096(3) Uani 0.403(4) 1 d PD F 2 H9OB H 1.0739 0.1734 0.1706 0.144 Uiso 0.403(4) 1 d PR F 2 O10B O 1.092(2) 0.3501(13) 0.1674(18) 0.0573(18) Uani 0.403(4) 1 d PD F 2 C41B C 1.158(2) 0.2885(16) 0.197(3) 0.057(2) Uani 0.403(4) 1 d PD F 2 C42B C 1.300(2) 0.299(3) 0.259(3) 0.100(4) Uani 0.403(4) 1 d PD F 2 H42B H 1.3286 0.3329 0.2170 0.120 Uiso 0.403(4) 1 calc PR F 2 C43B C 1.4248(14) 0.2985(9) 0.3304(9) 0.077(2) Uani 0.403(4) 1 d PD F 2 H43B H 1.4971 0.3501 0.3546 0.092 Uiso 0.403(4) 1 calc PR F 2 Cl1B Cl 1.4058(5) 0.1756(3) 0.3601(3) 0.0984(16) Uani 0.403(4) 1 d PD F 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 O1 0.0314(12) 0.0275(11) 0.0311(12) 0.0134(9) 0.0106(10) 0.0076(9) O2 0.0238(11) 0.0301(12) 0.0351(12) 0.0111(10) 0.0037(10) -0.0008(9) O3 0.0276(11) 0.0297(12) 0.0301(12) -0.0023(9) 0.0095(10) -0.0025(9) O4 0.0379(13) 0.0396(13) 0.0208(11) -0.0023(10) 0.0086(10) -0.0049(10) O5 0.0319(12) 0.0316(12) 0.0277(12) -0.0062(9) 0.0071(10) -0.0028(10) O6 0.0325(12) 0.0218(11) 0.0427(14) -0.0014(10) 0.0069(11) 0.0104(9) O7 0.0452(14) 0.0319(12) 0.0483(14) 0.0163(10) 0.0311(12) 0.0169(10) O8 0.0380(13) 0.0385(13) 0.0298(12) 0.0169(10) 0.0176(10) 0.0141(10) C1 0.0231(15) 0.0223(15) 0.0197(14) 0.0001(11) 0.0089(12) 0.0073(12) C2 0.0288(16) 0.0250(15) 0.0215(15) 0.0077(12) 0.0114(13) 0.0104(12) C3 0.0271(16) 0.0233(15) 0.0299(16) 0.0082(12) 0.0145(13) 0.0040(12) C4 0.0212(15) 0.0241(15) 0.0247(15) 0.0030(12) 0.0094(12) 0.0028(12) C5 0.0242(15) 0.0188(14) 0.0202(14) 0.0012(11) 0.0098(12) 0.0076(11) C6 0.0254(15) 0.0172(14) 0.0234(15) 0.0043(11) 0.0105(12) 0.0050(12) C7 0.0230(15) 0.0189(14) 0.0254(16) 0.0037(12) 0.0069(13) 0.0048(12) C8 0.0266(15) 0.0186(14) 0.0217(15) 0.0068(11) 0.0051(13) 0.0060(12) C9 0.0243(15) 0.0242(15) 0.0253(16) 0.0056(12) 0.0068(13) 0.0039(12) C10 0.0274(16) 0.0279(16) 0.0233(16) 0.0014(13) 0.0018(13) -0.0015(13) C11 0.0307(17) 0.0295(16) 0.0197(15) 0.0059(12) 0.0071(13) 0.0028(13) C12 0.0267(16) 0.0233(15) 0.0220(15) 0.0088(12) 0.0054(13) 0.0045(12) C13 0.0251(15) 0.0177(14) 0.0216(15) 0.0065(11) 0.0021(12) 0.0032(12) C14 0.0296(16) 0.0266(16) 0.0186(15) 0.0051(12) 0.0061(13) -0.0007(13) C15 0.0279(16) 0.0247(15) 0.0211(15) 0.0055(12) 0.0118(13) 0.0005(12) C16 0.0280(16) 0.0253(16) 0.0211(15) -0.0033(12) 0.0103(13) -0.0055(13) C17 0.0309(17) 0.0212(15) 0.0313(17) -0.0037(13) 0.0146(14) 0.0030(13) C18 0.0279(16) 0.0243(16) 0.0313(17) 0.0024(13) 0.0147(14) 0.0038(13) C19 0.0247(15) 0.0215(15) 0.0226(15) 0.0021(12) 0.0120(12) 0.0016(12) C20 0.0277(15) 0.0185(14) 0.0190(14) 0.0029(11) 0.0098(12) 0.0002(12) C21 0.0231(15) 0.0207(15) 0.0250(15) 0.0035(12) 0.0095(13) 0.0034(12) C22 0.0253(15) 0.0186(14) 0.0227(15) 0.0021(12) 0.0067(13) 0.0009(12) C23 0.0274(16) 0.0226(15) 0.0320(17) 0.0048(13) 0.0146(14) 0.0059(12) C24 0.0335(17) 0.0264(16) 0.0334(17) 0.0132(13) 0.0134(14) 0.0114(13) C25 0.0306(16) 0.0263(16) 0.0225(15) 0.0064(12) 0.0095(13) 0.0060(13) C26 0.0223(15) 0.0187(14) 0.0214(15) 0.0001(11) 0.0060(12) 0.0017(11) C27 0.0211(14) 0.0182(14) 0.0210(15) 0.0014(11) 0.0028(12) 0.0021(11) C28 0.0251(15) 0.0224(15) 0.0183(14) 0.0033(11) 0.0063(12) 0.0066(12) C29 0.0259(16) 0.0202(15) 0.0298(16) 0.0032(12) 0.0066(13) 0.0046(12) C30 0.0373(19) 0.0232(16) 0.045(2) 0.0118(14) 0.0052(16) 0.0081(14) C31 0.0321(17) 0.0267(16) 0.0283(17) 0.0096(13) 0.0070(14) -0.0010(13) C32 0.048(2) 0.0340(19) 0.044(2) 0.0197(16) 0.0093(18) 0.0078(16) C33 0.0289(16) 0.0224(15) 0.0261(16) 0.0036(12) 0.0100(13) 0.0014(12) C34 0.0330(18) 0.0295(17) 0.0327(18) 0.0011(14) 0.0088(15) -0.0025(14) C35 0.0286(16) 0.0201(15) 0.0277(16) -0.0003(12) 0.0063(13) 0.0042(12) C36 0.0341(18) 0.0261(17) 0.0336(18) -0.0017(14) 0.0006(15) 0.0009(14) O2S 0.067(2) 0.078(3) 0.051(2) 0.017(2) 0.0108(17) -0.007(2) O2SB 0.067(2) 0.078(3) 0.051(2) 0.017(2) 0.0108(17) -0.007(2) C2S 0.047(3) 0.086(4) 0.069(3) 0.022(3) 0.009(2) 0.004(2) O1W 0.091(4) 0.041(3) 0.021(2) 0.011(2) -0.021(3) -0.034(3) O2W 0.035(2) 0.0242(18) 0.0238(18) 0.0067(14) 0.0125(16) 0.0026(15) O3W 0.032(3) 0.037(3) 0.040(3) 0.001(3) 0.004(3) 0.005(3) O1S 0.108(4) 0.068(3) 0.070(3) 0.006(2) 0.039(3) -0.021(3) C1S 0.072(6) 0.097(4) 0.061(3) 0.008(3) 0.033(3) -0.014(4) O9 0.146(10) 0.051(4) 0.085(9) 0.009(4) 0.032(7) 0.032(4) O10 0.087(4) 0.019(5) 0.059(3) 0.020(3) 0.008(3) 0.024(3) C41 0.088(6) 0.046(5) 0.060(4) 0.018(4) 0.043(5) 0.045(4) C42 0.114(6) 0.170(12) 0.052(3) 0.036(7) 0.055(5) 0.086(7) C43 0.090(6) 0.081(6) 0.054(5) -0.008(4) 0.018(4) 0.048(5) Cl1 0.0551(15) 0.167(3) 0.098(2) -0.0525(19) -0.0025(13) 0.0336(17) O1SB 0.108(4) 0.068(3) 0.070(3) 0.006(2) 0.039(3) -0.021(3) C1SB 0.072(6) 0.097(4) 0.061(3) 0.008(3) 0.033(3) -0.014(4) O9B 0.146(10) 0.051(4) 0.085(9) 0.009(4) 0.032(7) 0.032(4) O10B 0.087(4) 0.019(5) 0.059(3) 0.020(3) 0.008(3) 0.024(3) C41B 0.088(6) 0.046(5) 0.060(4) 0.018(4) 0.043(5) 0.045(4) C42B 0.114(6) 0.170(12) 0.052(3) 0.036(7) 0.055(5) 0.086(7) C43B 0.090(6) 0.081(6) 0.054(5) -0.008(4) 0.018(4) 0.048(5) Cl1B 0.130(4) 0.080(3) 0.100(3) 0.017(2) 0.052(3) 0.051(2) _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 O1 C2 1.376(3) . ? O2 C4 1.375(4) . ? O3 C9 1.381(4) . ? O4 C11 1.379(4) . ? O5 C16 1.383(4) . ? O6 C18 1.367(4) . ? O7 C23 1.380(4) . ? O8 C25 1.390(4) . ? C1 C6 1.398(4) . ? C1 C2 1.399(4) . ? C1 C28 1.517(4) . ? C2 C3 1.385(4) . ? C3 C4 1.387(4) . ? C4 C5 1.397(4) . ? C5 C6 1.394(4) . ? C5 C7 1.525(4) . ? C7 C8 1.537(4) . ? C7 C29 1.544(4) . ? C8 C13 1.389(4) . ? C8 C9 1.394(4) . ? C9 C10 1.384(4) . ? C10 C11 1.388(5) . ? C11 C12 1.397(4) . ? C12 C13 1.394(4) . ? C12 C14 1.531(4) . ? C14 C15 1.522(4) . ? C14 C31 1.533(4) . ? C15 C20 1.397(4) . ? C15 C16 1.402(4) . ? C16 C17 1.378(4) . ? C17 C18 1.382(4) . ? C18 C19 1.408(4) . ? C19 C20 1.387(4) . ? C19 C21 1.519(4) . ? C21 C22 1.528(4) . ? C21 C33 1.539(4) . ? C22 C27 1.396(4) . ? C22 C23 1.401(4) . ? C23 C24 1.388(4) . ? C24 C25 1.372(4) . ? C25 C26 1.396(4) . ? C26 C27 1.385(4) . ? C26 C28 1.533(4) . ? C28 C35 1.536(4) . ? C29 C30 1.516(4) . ? C31 C32 1.523(5) . ? C33 C34 1.522(4) . ? C35 C36 1.513(4) . ? O2S C2S 1.422(6) . ? O2SB C2S 1.3705 . ? O1S C1S 1.44(2) . ? O9 C41 1.332(11) . ? O10 C41 1.196(9) . ? C41 C42 1.539(13) . ? C42 C43 1.450(19) . ? C43 Cl1 1.739(9) . ? O1SB C1SB 1.45(3) . ? O9B C41B 1.338(15) . ? O10B C41B 1.202(14) . ? C41B C42B 1.538(15) . ? C42B C43B 1.454(18) . ? C43B Cl1B 1.779(13) . ? 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 C6 C1 C2 117.0(3) . . ? C6 C1 C28 123.0(3) . . ? C2 C1 C28 120.0(3) . . ? O1 C2 C3 120.9(3) . . ? O1 C2 C1 117.9(3) . . ? C3 C2 C1 121.2(3) . . ? C2 C3 C4 119.9(3) . . ? O2 C4 C3 115.5(3) . . ? O2 C4 C5 123.3(3) . . ? C3 C4 C5 121.3(3) . . ? C6 C5 C4 117.1(3) . . ? C6 C5 C7 121.7(3) . . ? C4 C5 C7 121.1(3) . . ? C5 C6 C1 123.4(3) . . ? C5 C7 C8 110.8(2) . . ? C5 C7 C29 113.7(2) . . ? C8 C7 C29 111.5(2) . . ? C13 C8 C9 117.1(3) . . ? C13 C8 C7 121.6(3) . . ? C9 C8 C7 121.2(3) . . ? O3 C9 C10 121.1(3) . . ? O3 C9 C8 117.6(3) . . ? C10 C9 C8 121.3(3) . . ? C9 C10 C11 119.9(3) . . ? O4 C11 C10 121.6(3) . . ? O4 C11 C12 117.3(3) . . ? C10 C11 C12 121.1(3) . . ? C13 C12 C11 117.0(3) . . ? C13 C12 C14 121.4(3) . . ? C11 C12 C14 121.6(3) . . ? C8 C13 C12 123.6(3) . . ? C15 C14 C12 110.3(2) . . ? C15 C14 C31 114.9(2) . . ? C12 C14 C31 111.8(3) . . ? C20 C15 C16 116.2(3) . . ? C20 C15 C14 122.6(3) . . ? C16 C15 C14 121.1(3) . . ? C17 C16 O5 116.1(3) . . ? C17 C16 C15 121.9(3) . . ? O5 C16 C15 122.0(3) . . ? C16 C17 C18 120.2(3) . . ? O6 C18 C17 121.6(3) . . ? O6 C18 C19 117.9(3) . . ? C17 C18 C19 120.5(3) . . ? C20 C19 C18 117.4(3) . . ? C20 C19 C21 123.9(3) . . ? C18 C19 C21 118.7(3) . . ? C19 C20 C15 123.8(3) . . ? C19 C21 C22 111.2(2) . . ? C19 C21 C33 113.6(2) . . ? C22 C21 C33 111.9(2) . . ? C27 C22 C23 116.3(3) . . ? C27 C22 C21 121.0(3) . . ? C23 C22 C21 122.7(3) . . ? O7 C23 C24 115.5(3) . . ? O7 C23 C22 123.6(3) . . ? C24 C23 C22 121.0(3) . . ? C25 C24 C23 120.3(3) . . ? C24 C25 O8 117.0(3) . . ? C24 C25 C26 121.5(3) . . ? O8 C25 C26 121.5(3) . . ? C27 C26 C25 116.6(3) . . ? C27 C26 C28 121.8(3) . . ? C25 C26 C28 121.6(3) . . ? C26 C27 C22 124.4(3) . . ? C1 C28 C26 110.7(2) . . ? C1 C28 C35 113.8(2) . . ? C26 C28 C35 112.1(2) . . ? C30 C29 C7 112.6(2) . . ? C32 C31 C14 112.0(3) . . ? C34 C33 C21 112.7(3) . . ? C36 C35 C28 112.7(3) . . ? O2SB C2S O2S 35.6(3) . . ? O10 C41 O9 109.9(14) . . ? O10 C41 C42 113.1(12) . . ? O9 C41 C42 136.8(14) . . ? C43 C42 C41 94.2(14) . . ? C42 C43 Cl1 108.6(9) . . ? O10B C41B O9B 141(3) . . ? O10B C41B C42B 133(2) . . ? O9B C41B C42B 86(2) . . ? C43B C42B C41B 169(4) . . ? C42B C43B Cl1B 101.1(19) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.881 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.072 #=======================================END data_CECR-E-HClA-2MeOH-1.5H2O@90k-10h _database_code_depnum_ccdc_archive 'CCDC 629573' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CECR-E-HClA-2MeOH-1.5H2O@90k-10h _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C41 H54 Cl O13.50' _chemical_formula_weight 798.29 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3847(5) _cell_length_b 13.3860(7) _cell_length_c 14.6572(6) _cell_angle_alpha 99.1048(16) _cell_angle_beta 109.8419(13) _cell_angle_gamma 95.1665(15) _cell_volume 2049.61(16) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 675 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 0.158 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.9747 _exptl_absorpt_correction_T_max 0.9841 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9151 _diffrn_reflns_av_R_equivalents 0.0132 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6788 _reflns_number_gt 4831 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+2.3738P] 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 6788 _refine_ls_number_parameters 547 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0966 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1911 _refine_ls_wR_factor_gt 0.1732 _refine_ls_goodness_of_fit_ref 1.212 _refine_ls_restrained_S_all 1.213 _refine_ls_shift/su_max 0.002 _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 O1 O 0.7986(2) 0.60558(17) 0.57994(17) 0.0305(5) Uani 1 1 d . . . O2 O 0.4195(2) 0.60533(18) 0.31344(17) 0.0324(6) Uani 1 1 d . . . O3 O 0.3196(2) 0.65166(18) 0.13045(17) 0.0316(6) Uani 1 1 d . . . O4 O 0.5451(2) 0.61387(19) -0.09540(16) 0.0365(6) Uani 1 1 d . . . O5 O 0.7735(2) 0.54546(18) -0.03856(17) 0.0351(6) Uani 1 1 d . . . O6 O 1.1430(2) 0.54160(17) 0.23560(18) 0.0354(6) Uani 1 1 d . . . O7 O 1.2880(2) 0.59601(18) 0.44348(19) 0.0377(6) Uani 1 1 d . . . O8 O 1.0551(2) 0.63270(19) 0.65354(17) 0.0341(6) Uani 1 1 d . . . C1 C 0.7854(3) 0.7441(2) 0.4951(2) 0.0229(7) Uani 1 1 d . . . C2 C 0.7293(3) 0.6517(2) 0.5059(2) 0.0244(7) Uani 1 1 d . . . C3 C 0.6076(3) 0.6078(2) 0.4446(2) 0.0258(7) Uani 1 1 d . . . H3A H 0.5707 0.5453 0.4536 0.031 Uiso 1 1 calc R . . C4 C 0.5391(3) 0.6550(2) 0.3701(2) 0.0239(7) Uani 1 1 d . . . C5 C 0.5909(3) 0.7478(2) 0.3564(2) 0.0211(7) Uani 1 1 d . . . C6 C 0.7135(3) 0.7895(2) 0.4198(2) 0.0220(7) Uani 1 1 d . . . H6A H 0.7502 0.8523 0.4113 0.026 Uiso 1 1 calc R . . C7 C 0.5162(3) 0.7993(2) 0.2738(2) 0.0232(7) Uani 1 1 d . . . H7A H 0.4257 0.7862 0.2676 0.028 Uiso 1 1 calc R . . C8 C 0.5224(3) 0.7491(2) 0.1742(2) 0.0229(7) Uani 1 1 d . . . C9 C 0.4234(3) 0.6776(2) 0.1055(2) 0.0264(7) Uani 1 1 d . . . C10 C 0.4285(3) 0.6326(3) 0.0150(2) 0.0297(8) Uani 1 1 d . . . H10A H 0.3593 0.5846 -0.0315 0.036 Uiso 1 1 calc R . . C11 C 0.5353(3) 0.6582(3) -0.0071(2) 0.0283(8) Uani 1 1 d . . . C12 C 0.6378(3) 0.7287(2) 0.0597(2) 0.0251(7) Uani 1 1 d . . . C13 C 0.6279(3) 0.7718(2) 0.1493(2) 0.0231(7) Uani 1 1 d . . . H13A H 0.6972 0.8194 0.1961 0.028 Uiso 1 1 calc R . . C14 C 0.7561(3) 0.7575(2) 0.0359(2) 0.0268(7) Uani 1 1 d . . . H14A H 0.7331 0.7316 -0.0368 0.032 Uiso 1 1 calc R . . C15 C 0.8616(3) 0.7013(2) 0.0884(2) 0.0237(7) Uani 1 1 d . . . C16 C 0.8632(3) 0.5986(2) 0.0498(2) 0.0265(7) Uani 1 1 d . . . C17 C 0.9556(3) 0.5453(3) 0.0982(2) 0.0293(8) Uani 1 1 d . . . H17A H 0.9536 0.4757 0.0709 0.035 Uiso 1 1 calc R . . C18 C 1.0505(3) 0.5926(3) 0.1857(2) 0.0279(7) Uani 1 1 d . . . C19 C 1.0544(3) 0.6955(2) 0.2275(2) 0.0229(7) Uani 1 1 d . . . C20 C 0.9592(3) 0.7462(2) 0.1772(2) 0.0226(7) Uani 1 1 d . . . H20A H 0.9607 0.8156 0.2050 0.027 Uiso 1 1 calc R . . C21 C 1.1602(3) 0.7447(2) 0.3249(2) 0.0231(7) Uani 1 1 d . . . H21A H 1.2374 0.7155 0.3232 0.028 Uiso 1 1 calc R . . C22 C 1.1328(3) 0.7140(2) 0.4130(2) 0.0231(7) Uani 1 1 d . . . C23 C 1.1954(3) 0.6439(2) 0.4651(2) 0.0267(7) Uani 1 1 d . . . C24 C 1.1670(3) 0.6180(3) 0.5441(3) 0.0304(8) Uani 1 1 d . . . H24A H 1.2093 0.5692 0.5781 0.036 Uiso 1 1 calc R . . C25 C 1.0778(3) 0.6624(2) 0.5736(2) 0.0261(7) Uani 1 1 d . . . C26 C 1.0150(3) 0.7352(2) 0.5258(2) 0.0218(7) Uani 1 1 d . . . C27 C 1.0429(3) 0.7568(2) 0.4454(2) 0.0226(7) Uani 1 1 d . . . H27A H 0.9981 0.8036 0.4101 0.027 Uiso 1 1 calc R . . C28 C 0.9208(3) 0.7891(2) 0.5618(2) 0.0230(7) Uani 1 1 d . . . H28A H 0.9320 0.7734 0.6285 0.028 Uiso 1 1 calc R . . C29 C 0.5547(3) 0.9164(2) 0.2959(2) 0.0268(7) Uani 1 1 d . . . H29A H 0.5537 0.9453 0.3621 0.032 Uiso 1 1 calc R . . H29B H 0.6422 0.9323 0.2977 0.032 Uiso 1 1 calc R . . C30 C 0.4680(4) 0.9672(3) 0.2197(3) 0.0383(9) Uani 1 1 d . . . H30A H 0.4955 1.0415 0.2377 0.057 Uiso 1 1 calc R . . H30B H 0.3812 0.9521 0.2178 0.057 Uiso 1 1 calc R . . H30C H 0.4711 0.9410 0.1544 0.057 Uiso 1 1 calc R . . C31 C 0.7937(3) 0.8738(3) 0.0545(3) 0.0313(8) Uani 1 1 d . . . H31A H 0.8111 0.9034 0.1249 0.038 Uiso 1 1 calc R . . H31B H 0.8723 0.8891 0.0410 0.038 Uiso 1 1 calc R . . C32 C 0.6901(4) 0.9235(3) -0.0109(3) 0.0440(10) Uani 1 1 d . . . H32A H 0.7182 0.9974 0.0017 0.066 Uiso 1 1 calc R . . H32B H 0.6133 0.9111 0.0044 0.066 Uiso 1 1 calc R . . H32C H 0.6722 0.8940 -0.0806 0.066 Uiso 1 1 calc R . . C33 C 1.1931(3) 0.8615(2) 0.3389(2) 0.0264(7) Uani 1 1 d . . . H33A H 1.2076 0.8777 0.2796 0.032 Uiso 1 1 calc R . . H33B H 1.1204 0.8938 0.3448 0.032 Uiso 1 1 calc R . . C34 C 1.3099(3) 0.9066(3) 0.4303(3) 0.0335(8) Uani 1 1 d . . . H34A H 1.3268 0.9809 0.4361 0.050 Uiso 1 1 calc R . . H34B H 1.3826 0.8760 0.4242 0.050 Uiso 1 1 calc R . . H34C H 1.2954 0.8919 0.4894 0.050 Uiso 1 1 calc R . . C35 C 0.9494(3) 0.9057(2) 0.5768(2) 0.0272(7) Uani 1 1 d . . . H35A H 0.9460 0.9242 0.5133 0.033 Uiso 1 1 calc R . . H35B H 0.8832 0.9364 0.5961 0.033 Uiso 1 1 calc R . . C36 C 1.0771(3) 0.9505(3) 0.6550(3) 0.0356(9) Uani 1 1 d . . . H36A H 1.0908 1.0250 0.6611 0.053 Uiso 1 1 calc R . . H36B H 1.1433 0.9211 0.6360 0.053 Uiso 1 1 calc R . . H36C H 1.0802 0.9344 0.7187 0.053 Uiso 1 1 calc R . . O2S O 0.7758(4) 0.2713(4) 0.1697(3) 0.0713(16) Uani 0.832(8) 1 d PD A 1 H2S H 0.8251 0.2925 0.2230 0.107 Uiso 0.832(8) 1 d PR A 1 O2SB O 0.7938(5) 0.2116(4) 0.1725(4) 0.0713(16) Uani 0.168(8) 1 d PD A 2 H2SB H 0.8437 0.2627 0.2299 0.107 Uiso 0.168(8) 1 d PR A 2 C2S C 0.6765(5) 0.2057(4) 0.1796(4) 0.0734(15) Uani 1 1 d RD . . H2S1 H 0.7089 0.1733 0.2368 0.110 Uiso 1 1 d R . . H2S2 H 0.6370 0.1526 0.1194 0.110 Uiso 1 1 d R . . H2S3 H 0.6136 0.2478 0.1888 0.110 Uiso 1 1 d R . . O1W O 0.3157(7) 0.5393(4) 0.7705(4) 0.067(2) Uani 0.50 1 d P B 1 H1WA H 0.2500 0.4899 0.7202 0.101 Uiso 0.50 1 d PR B 1 H1WB H 0.3034 0.5729 0.8308 0.101 Uiso 0.50 1 d PR B 1 O2W O 0.2353(3) 0.4451(3) 0.7415(3) 0.0284(9) Uani 0.60 1 d P C 2 H2WA H 0.1884 0.3861 0.7216 0.043 Uiso 0.60 1 d PR C 2 H2WB H 0.2398 0.4634 0.6879 0.043 Uiso 0.60 1 d PR C 2 O3W O 0.3563(5) 0.4616(4) 0.8089(4) 0.0392(15) Uani 0.40 1 d P D 3 H3WA H 0.2772 0.4509 0.8125 0.059 Uiso 0.40 1 d PR D 3 H3WB H 0.3574 0.4875 0.7591 0.059 Uiso 0.40 1 d PR D 3 H1O H 0.7580 0.5502 0.5739 0.059 Uiso 1 1 d R . . H2O H 0.3919 0.6248 0.2613 0.059 Uiso 1 1 d R . . H3O H 0.2824 0.6079 0.0982 0.059 Uiso 1 1 d R . . H40 H 0.4829 0.5725 -0.1300 0.059 Uiso 1 1 d R . . H5O H 0.7153 0.5701 -0.0542 0.059 Uiso 1 1 d R . . H6O H 1.1320 0.4845 0.2090 0.059 Uiso 1 1 d R . . H7O H 1.2902 0.6027 0.3909 0.059 Uiso 1 1 d R . . H8O H 0.9777 0.6234 0.6413 0.059 Uiso 1 1 d R . . O1S O 0.8958(5) 0.1474(4) 0.0692(3) 0.0860(16) Uani 0.792(6) 1 d PD E 1 H1S H 0.8561 0.1901 0.1052 0.129 Uiso 0.792(6) 1 d PR E 1 C1S C 0.8738(11) 0.1791(12) -0.0238(9) 0.075(3) Uani 0.792(6) 1 d PD E 1 H1S1 H 0.7955 0.2087 -0.0422 0.112 Uiso 0.792(6) 1 calc PR E 1 H1S2 H 0.8664 0.1196 -0.0751 0.112 Uiso 0.792(6) 1 calc PR E 1 H1S3 H 0.9447 0.2304 -0.0174 0.112 Uiso 0.792(6) 1 calc PR E 1 O9 O 1.122(3) 0.1758(12) 0.1712(17) 0.104(3) Uani 0.589(4) 1 d PD F 1 H9O H 1.0288 0.1660 0.1259 0.156 Uiso 0.589(4) 1 d PR F 1 O10 O 1.1067(18) 0.3290(10) 0.1731(15) 0.063(2) Uani 0.589(4) 1 d PD F 1 C41 C 1.1797(16) 0.2720(11) 0.204(2) 0.062(2) Uani 0.589(4) 1 d PD F 1 C42 C 1.3161(18) 0.322(2) 0.261(2) 0.100(4) Uani 0.589(4) 1 d PD F 1 H42A H 1.3581 0.3896 0.2713 0.119 Uiso 0.589(4) 1 calc PR F 1 C43 C 1.3597(9) 0.2317(8) 0.2924(6) 0.080(3) Uani 0.589(4) 1 d PD F 1 H43A H 1.3102 0.1658 0.2748 0.096 Uiso 0.589(4) 1 calc PR F 1 Cl1 Cl 1.5190(2) 0.2629(3) 0.3688(2) 0.1193(16) Uani 0.589(4) 1 d PD F 1 O1SB O 0.893(2) 0.2785(14) 0.0508(13) 0.0860(16) Uani 0.208(6) 1 d PD E 2 H1SB H 0.9799 0.2934 0.0936 0.129 Uiso 0.208(6) 1 d PR E 2 C1SB C 0.848(6) 0.183(5) -0.021(4) 0.075(3) Uani 0.208(6) 1 d PD E 2 H1S4 H 0.9198 0.1493 -0.0237 0.112 Uiso 0.208(6) 1 calc PR E 2 H1S5 H 0.8012 0.1966 -0.0861 0.112 Uiso 0.208(6) 1 calc PR E 2 H1S6 H 0.7917 0.1383 -0.0011 0.112 Uiso 0.208(6) 1 calc PR E 2 O9B O 1.149(4) 0.1858(19) 0.195(3) 0.104(3) Uani 0.411(4) 1 d PD F 2 H9OB H 1.0694 0.1706 0.1666 0.156 Uiso 0.411(4) 1 d PR F 2 O10B O 1.094(3) 0.3487(17) 0.169(2) 0.063(2) Uani 0.411(4) 1 d PD F 2 C41B C 1.161(3) 0.2861(19) 0.197(3) 0.062(2) Uani 0.411(4) 1 d PD F 2 C42B C 1.300(3) 0.303(3) 0.262(4) 0.100(4) Uani 0.411(4) 1 d PD F 2 H42B H 1.3228 0.3644 0.2431 0.119 Uiso 0.411(4) 1 calc PR F 2 C43B C 1.4235(15) 0.2986(10) 0.3304(10) 0.080(3) Uani 0.411(4) 1 d PD F 2 H43B H 1.4968 0.3491 0.3540 0.096 Uiso 0.411(4) 1 calc PR F 2 Cl1B Cl 1.4058(5) 0.1760(3) 0.3602(3) 0.1016(18) Uani 0.411(4) 1 d PD F 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 O1 0.0333(13) 0.0300(13) 0.0316(13) 0.0138(10) 0.0113(11) 0.0093(10) O2 0.0247(12) 0.0310(13) 0.0356(14) 0.0108(11) 0.0025(11) 0.0002(10) O3 0.0278(13) 0.0301(13) 0.0305(13) -0.0029(10) 0.0081(10) -0.0019(10) O4 0.0391(14) 0.0413(15) 0.0213(12) -0.0025(11) 0.0082(11) -0.0059(12) O5 0.0338(14) 0.0337(14) 0.0286(13) -0.0063(11) 0.0070(11) -0.0017(11) O6 0.0334(13) 0.0211(12) 0.0445(15) -0.0018(10) 0.0072(12) 0.0101(10) O7 0.0473(15) 0.0335(14) 0.0489(15) 0.0175(12) 0.0314(13) 0.0181(12) O8 0.0400(14) 0.0406(14) 0.0320(13) 0.0179(11) 0.0187(11) 0.0166(11) C1 0.0254(17) 0.0242(17) 0.0197(16) 0.0012(13) 0.0092(13) 0.0086(13) C2 0.0305(18) 0.0249(17) 0.0222(16) 0.0073(13) 0.0122(14) 0.0108(14) C3 0.0294(18) 0.0221(16) 0.0294(18) 0.0077(14) 0.0141(15) 0.0029(14) C4 0.0215(16) 0.0246(17) 0.0256(17) 0.0038(14) 0.0088(14) 0.0048(13) C5 0.0243(16) 0.0197(16) 0.0203(16) 0.0009(13) 0.0095(14) 0.0077(13) C6 0.0262(17) 0.0193(16) 0.0211(16) 0.0032(13) 0.0089(14) 0.0058(13) C7 0.0222(16) 0.0190(16) 0.0255(17) 0.0031(13) 0.0048(14) 0.0048(13) C8 0.0256(17) 0.0191(16) 0.0212(16) 0.0058(13) 0.0036(14) 0.0061(13) C9 0.0264(17) 0.0248(17) 0.0267(18) 0.0068(14) 0.0074(14) 0.0038(14) C10 0.0282(18) 0.0280(18) 0.0236(18) 0.0014(14) 0.0005(14) -0.0006(14) C11 0.0328(19) 0.0300(18) 0.0187(17) 0.0044(14) 0.0060(15) 0.0022(15) C12 0.0260(17) 0.0253(17) 0.0224(17) 0.0092(14) 0.0048(14) 0.0045(14) C13 0.0259(17) 0.0181(16) 0.0203(16) 0.0052(13) 0.0013(13) 0.0038(13) C14 0.0326(18) 0.0272(18) 0.0184(16) 0.0050(14) 0.0073(14) 0.0005(14) C15 0.0273(17) 0.0238(17) 0.0202(16) 0.0041(13) 0.0103(14) -0.0017(13) C16 0.0305(18) 0.0258(17) 0.0204(17) -0.0037(14) 0.0118(14) -0.0043(14) C17 0.0329(19) 0.0222(17) 0.0320(19) -0.0037(14) 0.0151(16) 0.0034(14) C18 0.0276(17) 0.0255(17) 0.0307(19) 0.0015(14) 0.0128(15) 0.0038(14) C19 0.0260(17) 0.0218(16) 0.0228(16) 0.0031(13) 0.0123(14) 0.0028(13) C20 0.0288(17) 0.0190(16) 0.0194(16) 0.0025(13) 0.0094(14) 0.0001(13) C21 0.0237(16) 0.0214(16) 0.0233(17) 0.0028(13) 0.0080(14) 0.0040(13) C22 0.0251(17) 0.0200(16) 0.0216(16) 0.0029(13) 0.0066(14) 0.0003(13) C23 0.0283(17) 0.0225(17) 0.0319(19) 0.0039(14) 0.0140(15) 0.0069(14) C24 0.0354(19) 0.0269(18) 0.0345(19) 0.0132(15) 0.0147(16) 0.0127(15) C25 0.0294(18) 0.0269(17) 0.0209(17) 0.0053(14) 0.0073(14) 0.0045(14) C26 0.0224(16) 0.0179(15) 0.0221(16) 0.0005(13) 0.0058(13) 0.0022(12) C27 0.0225(16) 0.0190(16) 0.0200(16) 0.0014(13) 0.0013(13) 0.0020(13) C28 0.0258(17) 0.0220(16) 0.0200(16) 0.0029(13) 0.0063(13) 0.0070(13) C29 0.0258(17) 0.0204(17) 0.0316(18) 0.0038(14) 0.0074(14) 0.0052(13) C30 0.040(2) 0.0261(19) 0.045(2) 0.0118(16) 0.0076(18) 0.0094(16) C31 0.0339(19) 0.0291(18) 0.0271(18) 0.0098(15) 0.0058(15) -0.0010(15) C32 0.051(2) 0.035(2) 0.043(2) 0.0183(18) 0.0084(19) 0.0077(18) C33 0.0292(18) 0.0225(17) 0.0260(17) 0.0045(14) 0.0088(14) 0.0026(14) C34 0.0321(19) 0.0309(19) 0.032(2) 0.0016(15) 0.0082(16) -0.0025(15) C35 0.0277(17) 0.0218(17) 0.0273(18) -0.0002(14) 0.0056(14) 0.0056(14) C36 0.034(2) 0.0258(18) 0.035(2) -0.0026(15) 0.0020(17) 0.0017(15) O2S 0.070(3) 0.081(4) 0.054(2) 0.020(2) 0.0136(19) -0.004(2) O2SB 0.070(3) 0.081(4) 0.054(2) 0.020(2) 0.0136(19) -0.004(2) C2S 0.047(3) 0.089(4) 0.074(4) 0.025(3) 0.008(3) 0.004(3) O1W 0.097(5) 0.042(3) 0.022(3) 0.013(2) -0.022(3) -0.037(3) O2W 0.036(2) 0.025(2) 0.025(2) 0.0076(16) 0.0108(17) 0.0013(17) O3W 0.031(3) 0.035(4) 0.042(4) 0.001(3) 0.004(3) 0.005(3) O1S 0.112(4) 0.070(3) 0.070(3) 0.006(2) 0.038(3) -0.020(3) C1S 0.065(7) 0.096(4) 0.066(4) 0.009(3) 0.035(4) -0.010(4) O9 0.161(10) 0.058(4) 0.101(10) 0.019(4) 0.050(7) 0.044(4) O10 0.097(4) 0.022(5) 0.061(3) 0.015(4) 0.011(3) 0.018(4) C41 0.096(6) 0.051(5) 0.063(5) 0.020(4) 0.046(5) 0.044(4) C42 0.110(6) 0.169(10) 0.057(3) 0.039(6) 0.055(5) 0.084(6) C43 0.091(7) 0.090(7) 0.050(6) -0.011(4) 0.014(5) 0.054(6) Cl1 0.0555(16) 0.160(3) 0.099(2) -0.045(2) 0.0008(14) 0.0335(18) O1SB 0.112(4) 0.070(3) 0.070(3) 0.006(2) 0.038(3) -0.020(3) C1SB 0.065(7) 0.096(4) 0.066(4) 0.009(3) 0.035(4) -0.010(4) O9B 0.161(10) 0.058(4) 0.101(10) 0.019(4) 0.050(7) 0.044(4) O10B 0.097(4) 0.022(5) 0.061(3) 0.015(4) 0.011(3) 0.018(4) C41B 0.096(6) 0.051(5) 0.063(5) 0.020(4) 0.046(5) 0.044(4) C42B 0.110(6) 0.169(10) 0.057(3) 0.039(6) 0.055(5) 0.084(6) C43B 0.091(7) 0.090(7) 0.050(6) -0.011(4) 0.014(5) 0.054(6) Cl1B 0.133(4) 0.085(3) 0.104(3) 0.020(2) 0.054(3) 0.054(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.379(4) . ? O2 C4 1.372(4) . ? O3 C9 1.382(4) . ? O4 C11 1.380(4) . ? O5 C16 1.380(4) . ? O6 C18 1.369(4) . ? O7 C23 1.381(4) . ? O8 C25 1.390(4) . ? C1 C6 1.394(4) . ? C1 C2 1.397(5) . ? C1 C28 1.522(4) . ? C2 C3 1.384(5) . ? C3 C4 1.389(4) . ? C4 C5 1.400(4) . ? C5 C6 1.391(4) . ? C5 C7 1.529(4) . ? C7 C8 1.535(4) . ? C7 C29 1.541(4) . ? C8 C9 1.389(5) . ? C8 C13 1.391(5) . ? C9 C10 1.390(5) . ? C10 C11 1.389(5) . ? C11 C12 1.395(5) . ? C12 C13 1.394(5) . ? C12 C14 1.534(5) . ? C14 C15 1.524(4) . ? C14 C31 1.532(5) . ? C15 C20 1.393(4) . ? C15 C16 1.405(4) . ? C16 C17 1.381(5) . ? C17 C18 1.376(5) . ? C18 C19 1.406(4) . ? C19 C20 1.388(4) . ? C19 C21 1.521(4) . ? C21 C22 1.534(4) . ? C21 C33 1.539(4) . ? C22 C27 1.396(4) . ? C22 C23 1.397(4) . ? C23 C24 1.388(5) . ? C24 C25 1.377(5) . ? C25 C26 1.396(4) . ? C26 C27 1.386(4) . ? C26 C28 1.534(4) . ? C28 C35 1.531(4) . ? C29 C30 1.515(4) . ? C31 C32 1.526(5) . ? C33 C34 1.522(5) . ? C35 C36 1.511(5) . ? O2S C2S 1.430(6) . ? O2SB C2S 1.3712 . ? O1S C1S 1.440(18) . ? O9 C41 1.327(12) . ? O10 C41 1.202(10) . ? C41 C42 1.519(14) . ? C42 C43 1.431(19) . ? C43 Cl1 1.748(9) . ? O1SB C1SB 1.45(3) . ? O9B C41B 1.332(16) . ? O10B C41B 1.208(14) . ? C41B C42B 1.521(15) . ? C42B C43B 1.436(18) . ? C43B Cl1B 1.776(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 C6 C1 C2 117.0(3) . . ? C6 C1 C28 123.0(3) . . ? C2 C1 C28 120.0(3) . . ? O1 C2 C3 120.8(3) . . ? O1 C2 C1 118.0(3) . . ? C3 C2 C1 121.2(3) . . ? C2 C3 C4 120.1(3) . . ? O2 C4 C3 115.6(3) . . ? O2 C4 C5 123.5(3) . . ? C3 C4 C5 120.9(3) . . ? C6 C5 C4 117.1(3) . . ? C6 C5 C7 121.9(3) . . ? C4 C5 C7 121.0(3) . . ? C5 C6 C1 123.7(3) . . ? C5 C7 C8 110.6(2) . . ? C5 C7 C29 113.7(3) . . ? C8 C7 C29 111.7(3) . . ? C9 C8 C13 117.1(3) . . ? C9 C8 C7 121.3(3) . . ? C13 C8 C7 121.6(3) . . ? O3 C9 C8 117.8(3) . . ? O3 C9 C10 120.8(3) . . ? C8 C9 C10 121.4(3) . . ? C11 C10 C9 119.6(3) . . ? O4 C11 C10 121.4(3) . . ? O4 C11 C12 117.3(3) . . ? C10 C11 C12 121.3(3) . . ? C13 C12 C11 116.9(3) . . ? C13 C12 C14 121.5(3) . . ? C11 C12 C14 121.6(3) . . ? C8 C13 C12 123.8(3) . . ? C15 C14 C31 114.5(3) . . ? C15 C14 C12 110.3(2) . . ? C31 C14 C12 111.9(3) . . ? C20 C15 C16 116.2(3) . . ? C20 C15 C14 123.0(3) . . ? C16 C15 C14 120.8(3) . . ? O5 C16 C17 116.2(3) . . ? O5 C16 C15 122.2(3) . . ? C17 C16 C15 121.6(3) . . ? C18 C17 C16 120.4(3) . . ? O6 C18 C17 121.7(3) . . ? O6 C18 C19 117.8(3) . . ? C17 C18 C19 120.6(3) . . ? C20 C19 C18 117.4(3) . . ? C20 C19 C21 123.7(3) . . ? C18 C19 C21 118.9(3) . . ? C19 C20 C15 123.8(3) . . ? C19 C21 C22 111.2(3) . . ? C19 C21 C33 113.7(2) . . ? C22 C21 C33 112.0(3) . . ? C27 C22 C23 116.7(3) . . ? C27 C22 C21 120.6(3) . . ? C23 C22 C21 122.7(3) . . ? O7 C23 C24 115.3(3) . . ? O7 C23 C22 123.9(3) . . ? C24 C23 C22 120.8(3) . . ? C25 C24 C23 120.4(3) . . ? C24 C25 O8 116.9(3) . . ? C24 C25 C26 121.1(3) . . ? O8 C25 C26 122.0(3) . . ? C27 C26 C25 116.8(3) . . ? C27 C26 C28 121.9(3) . . ? C25 C26 C28 121.3(3) . . ? C26 C27 C22 124.1(3) . . ? C1 C28 C35 113.7(2) . . ? C1 C28 C26 110.7(2) . . ? C35 C28 C26 112.3(3) . . ? C30 C29 C7 112.7(3) . . ? C32 C31 C14 111.7(3) . . ? C34 C33 C21 112.5(3) . . ? C36 C35 C28 112.9(3) . . ? O2SB C2S O2S 35.1(3) . . ? O10 C41 O9 109.7(18) . . ? O10 C41 C42 115.8(16) . . ? O9 C41 C42 134.1(18) . . ? C43 C42 C41 95.7(16) . . ? C42 C43 Cl1 108.8(11) . . ? O10B C41B O9B 138(3) . . ? O10B C41B C42B 129(3) . . ? O9B C41B C42B 93(3) . . ? C43B C42B C41B 167(4) . . ? C42B C43B Cl1B 103(2) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.898 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.072 #=======================================END data_CECR-Z-HClA-2MeOH-1.5H2O@90k _database_code_depnum_ccdc_archive 'CCDC 629574' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CECR-Z-HClA-2MeOH-1.5H2O@90k _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C41 H54 Cl O13.50' _chemical_formula_weight 798.29 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2946(4) _cell_length_b 13.4660(5) _cell_length_c 14.6284(5) _cell_angle_alpha 98.6809(10) _cell_angle_beta 111.1014(9) _cell_angle_gamma 94.8602(10) _cell_volume 2028.45(13) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 675 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 0.160 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.9687 _exptl_absorpt_correction_T_max 0.9811 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22694 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7140 _reflns_number_gt 6290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+2.2830P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7140 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1279 _refine_ls_wR_factor_gt 0.1228 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 O1 O 0.81055(13) 0.60403(11) 0.58242(10) 0.0157(3) Uani 1 1 d . . . O2 O 0.41852(12) 0.60453(10) 0.31433(11) 0.0159(3) Uani 1 1 d . . . O3 O 0.31272(13) 0.65038(11) 0.12897(10) 0.0171(3) Uani 1 1 d . . . O4 O 0.53335(15) 0.61704(12) -0.09862(11) 0.0206(3) Uani 1 1 d . . . O5 O 0.76680(14) 0.54810(11) -0.04046(10) 0.0185(3) Uani 1 1 d . . . O6 O 1.14444(13) 0.54413(12) 0.24038(11) 0.0202(3) Uani 1 1 d . . . O7 O 1.29929(13) 0.59646(10) 0.44944(11) 0.0164(3) Uani 1 1 d . . . O8 O 1.07248(14) 0.63505(11) 0.66195(10) 0.0175(3) Uani 1 1 d . . . C1 C 0.79186(17) 0.74225(14) 0.49693(13) 0.0121(4) Uani 1 1 d . . . C2 C 0.73724(18) 0.65017(14) 0.50763(13) 0.0130(4) Uani 1 1 d . . . C3 C 0.61284(18) 0.60629(14) 0.44600(14) 0.0139(4) Uani 1 1 d . . . H3A H 0.5767 0.5440 0.4550 0.017 Uiso 1 1 calc R . . C4 C 0.54132(17) 0.65392(14) 0.37102(14) 0.0130(4) Uani 1 1 d . . . C5 C 0.59110(17) 0.74635(14) 0.35686(13) 0.0124(4) Uani 1 1 d . . . C6 C 0.71682(17) 0.78780(14) 0.42155(13) 0.0123(4) Uani 1 1 d . . . H6A H 0.7528 0.8506 0.4134 0.015 Uiso 1 1 calc R . . C7 C 0.51325(17) 0.79755(14) 0.27328(14) 0.0130(4) Uani 1 1 d . . . H7A H 0.4218 0.7845 0.2668 0.016 Uiso 1 1 calc R . . C8 C 0.51763(17) 0.74850(14) 0.17363(14) 0.0132(4) Uani 1 1 d . . . C9 C 0.41655(18) 0.67692(14) 0.10371(14) 0.0146(4) Uani 1 1 d . . . C10 C 0.41976(18) 0.63338(15) 0.01280(14) 0.0166(4) Uani 1 1 d . . . H10A H 0.3494 0.5857 -0.0341 0.020 Uiso 1 1 calc R . . C11 C 0.52631(18) 0.65980(14) -0.00952(14) 0.0154(4) Uani 1 1 d . . . C12 C 0.63084(17) 0.73020(14) 0.05826(14) 0.0137(4) Uani 1 1 d . . . C13 C 0.62330(17) 0.77210(14) 0.14839(14) 0.0131(4) Uani 1 1 d . . . H13A H 0.6939 0.8194 0.1955 0.016 Uiso 1 1 calc R . . C14 C 0.74904(18) 0.75862(14) 0.03443(14) 0.0144(4) Uani 1 1 d . . . H14A H 0.7241 0.7336 -0.0389 0.017 Uiso 1 1 calc R . . C15 C 0.85729(17) 0.70206(14) 0.08766(14) 0.0133(4) Uani 1 1 d . . . C16 C 0.85843(18) 0.60099(15) 0.04927(14) 0.0149(4) Uani 1 1 d . . . C17 C 0.95347(18) 0.54718(15) 0.09850(14) 0.0162(4) Uani 1 1 d . . . H17A H 0.9523 0.4784 0.0707 0.019 Uiso 1 1 calc R . . C18 C 1.05044(18) 0.59459(15) 0.18874(14) 0.0152(4) Uani 1 1 d . . . C19 C 1.05498(17) 0.69630(14) 0.22972(14) 0.0131(4) Uani 1 1 d . . . C20 C 0.95746(17) 0.74715(14) 0.17801(14) 0.0127(4) Uani 1 1 d . . . H20A H 0.9590 0.8161 0.2055 0.015 Uiso 1 1 calc R . . C21 C 1.16446(17) 0.74539(14) 0.32782(14) 0.0129(4) Uani 1 1 d . . . H21A H 1.2428 0.7170 0.3260 0.015 Uiso 1 1 calc R . . C22 C 1.14066(17) 0.71449(14) 0.41686(14) 0.0128(4) Uani 1 1 d . . . C23 C 1.20672(17) 0.64549(14) 0.47067(14) 0.0136(4) Uani 1 1 d . . . C24 C 1.18163(18) 0.61993(14) 0.55096(14) 0.0154(4) Uani 1 1 d . . . H24A H 1.2265 0.5721 0.5859 0.019 Uiso 1 1 calc R . . C25 C 1.09143(18) 0.66396(14) 0.58019(14) 0.0141(4) Uani 1 1 d . . . C26 C 1.02488(17) 0.73541(14) 0.53122(13) 0.0127(4) Uani 1 1 d . . . C27 C 1.05034(17) 0.75676(14) 0.44923(13) 0.0126(4) Uani 1 1 d . . . H27A H 1.0033 0.8030 0.4130 0.015 Uiso 1 1 calc R . . C28 C 0.92913(17) 0.78819(14) 0.56550(14) 0.0132(4) Uani 1 1 d . . . H28A H 0.9417 0.7734 0.6331 0.016 Uiso 1 1 calc R . . C29 C 0.55180(18) 0.91351(14) 0.29549(14) 0.0154(4) Uani 1 1 d . . . H29A H 0.5498 0.9421 0.3613 0.018 Uiso 1 1 calc R . . H29B H 0.6408 0.9294 0.2993 0.018 Uiso 1 1 calc R . . C30 C 0.4629(2) 0.96344(15) 0.21591(16) 0.0215(4) Uani 1 1 d . . . H30A H 0.4899 1.0372 0.2335 0.032 Uiso 1 1 calc R . . H30B H 0.3746 0.9480 0.2120 0.032 Uiso 1 1 calc R . . H30C H 0.4670 0.9372 0.1511 0.032 Uiso 1 1 calc R . . C31 C 0.78804(18) 0.87440(15) 0.05406(14) 0.0174(4) Uani 1 1 d . . . H31A H 0.8065 0.9031 0.1250 0.021 Uiso 1 1 calc R . . H31B H 0.8675 0.8894 0.0415 0.021 Uiso 1 1 calc R . . C32 C 0.6830(2) 0.92503(16) -0.01217(17) 0.0255(5) Uani 1 1 d . . . H32A H 0.7121 0.9983 0.0010 0.038 Uiso 1 1 calc R . . H32B H 0.6054 0.9130 0.0024 0.038 Uiso 1 1 calc R . . H32C H 0.6640 0.8964 -0.0825 0.038 Uiso 1 1 calc R . . C33 C 1.19561(18) 0.86115(14) 0.34130(14) 0.0151(4) Uani 1 1 d . . . H33A H 1.2087 0.8775 0.2815 0.018 Uiso 1 1 calc R . . H33B H 1.1215 0.8925 0.3464 0.018 Uiso 1 1 calc R . . C34 C 1.31526(19) 0.90703(15) 0.43405(15) 0.0203(4) Uani 1 1 d . . . H34A H 1.3312 0.9807 0.4391 0.030 Uiso 1 1 calc R . . H34B H 1.3893 0.8772 0.4289 0.030 Uiso 1 1 calc R . . H34C H 1.3021 0.8927 0.4937 0.030 Uiso 1 1 calc R . . C35 C 0.95408(18) 0.90424(14) 0.57775(14) 0.0155(4) Uani 1 1 d . . . H35A H 0.9489 0.9215 0.5131 0.019 Uiso 1 1 calc R . . H35B H 0.8862 0.9338 0.5956 0.019 Uiso 1 1 calc R . . C36 C 1.0849(2) 0.95154(16) 0.65773(16) 0.0227(4) Uani 1 1 d . . . H36A H 1.0963 1.0253 0.6624 0.034 Uiso 1 1 calc R . . H36B H 1.1527 0.9234 0.6398 0.034 Uiso 1 1 calc R . . H36C H 1.0899 0.9362 0.7223 0.034 Uiso 1 1 calc R . . O2S O 0.7884(2) 0.2217(2) 0.16680(15) 0.0676(7) Uani 1 1 d . . . H2S H 0.8310 0.2835 0.2197 0.101 Uiso 1 1 d R . . C2S C 0.6717(2) 0.1842(3) 0.1744(2) 0.0502(7) Uani 1 1 d . . . H2S1 H 0.6903 0.1485 0.2305 0.075 Uiso 1 1 calc R . . H2S2 H 0.6177 0.1370 0.1124 0.075 Uiso 1 1 calc R . . H2S3 H 0.6266 0.2410 0.1854 0.075 Uiso 1 1 calc R . . O1W O 0.2908(2) 0.54020(17) 0.77160(17) 0.0205(5) Uani 0.60 1 d P A 1 H1WA H 0.2251 0.4908 0.7213 0.031 Uiso 0.60 1 d PR A 1 H1WB H 0.2785 0.5738 0.8319 0.031 Uiso 0.60 1 d PR A 1 O2W O 0.2356(2) 0.43630(17) 0.74079(17) 0.0196(5) Uani 0.60 1 d P B 2 H2WA H 0.1886 0.3773 0.7209 0.029 Uiso 0.60 1 d PR B 2 H2WB H 0.2400 0.4546 0.6872 0.029 Uiso 0.60 1 d PR B 2 O3W O 0.3555(4) 0.4581(3) 0.8063(3) 0.0133(9) Uani 0.30 1 d P C 3 H3WA H 0.2764 0.4474 0.8100 0.020 Uiso 0.30 1 d PR C 3 H3WB H 0.3565 0.4840 0.7566 0.020 Uiso 0.30 1 d PR C 3 H1O H 0.777(3) 0.550(2) 0.578(2) 0.028(7) Uiso 1 1 d . . . H2O H 0.391(3) 0.626(2) 0.260(2) 0.032(7) Uiso 1 1 d . . . H3O H 0.276(3) 0.596(2) 0.095(2) 0.036(8) Uiso 1 1 d . . . H40 H 0.474(3) 0.585(3) -0.130(3) 0.058(11) Uiso 1 1 d . . . H5O H 0.707(3) 0.578(2) -0.056(2) 0.038(8) Uiso 1 1 d . . . H6O H 1.130(3) 0.486(2) 0.217(2) 0.033(8) Uiso 1 1 d . . . H7O H 1.299(2) 0.6046(19) 0.399(2) 0.024(7) Uiso 1 1 d . . . H8O H 0.997(3) 0.627(2) 0.650(2) 0.038(8) Uiso 1 1 d . . . O9 O 1.16735(17) 0.19177(12) 0.18701(14) 0.0354(4) Uani 1 1 d . . . H9O H 1.073(4) 0.170(3) 0.140(3) 0.092(13) Uiso 1 1 d . . . O10 O 1.10770(16) 0.34335(12) 0.17624(12) 0.0301(4) Uani 1 1 d . . . C41 C 1.1910(2) 0.29090(16) 0.20705(16) 0.0229(5) Uani 1 1 d . . . C42 C 1.3263(2) 0.33783(17) 0.26780(16) 0.0263(5) Uani 1 1 d . . . H42A H 1.3497 0.4046 0.2602 0.032 Uiso 1 1 calc R . . C43 C 1.4185(2) 0.2994(2) 0.33091(18) 0.0337(6) Uani 1 1 d . . . H43A H 1.4996 0.3414 0.3631 0.040 Uiso 1 1 calc R . . Cl1 Cl 1.40689(7) 0.18114(5) 0.36081(5) 0.04429(19) Uani 1 1 d . . . O1S O 0.92819(17) 0.13297(14) 0.07550(14) 0.0429(5) Uani 1 1 d . . . H1S H 0.8821 0.1745 0.1123 0.064 Uiso 1 1 d R . . C1S C 0.8875(3) 0.1689(3) -0.0167(2) 0.0494(8) Uani 1 1 d . . . H1S1 H 0.8039 0.1917 -0.0293 0.074 Uiso 1 1 calc R . . H1S2 H 0.8800 0.1137 -0.0715 0.074 Uiso 1 1 calc R . . H1S3 H 0.9506 0.2257 -0.0126 0.074 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 O1 0.0145(7) 0.0155(7) 0.0161(7) 0.0064(6) 0.0035(6) 0.0011(6) O2 0.0096(6) 0.0179(7) 0.0163(7) 0.0035(6) 0.0014(5) -0.0021(5) O3 0.0125(7) 0.0185(7) 0.0170(7) -0.0019(6) 0.0052(6) -0.0038(6) O4 0.0177(8) 0.0264(8) 0.0125(7) -0.0028(6) 0.0043(6) -0.0067(6) O5 0.0149(7) 0.0193(7) 0.0152(7) -0.0034(6) 0.0021(6) -0.0010(6) O6 0.0152(7) 0.0142(8) 0.0245(8) -0.0013(6) 0.0014(6) 0.0035(6) O7 0.0150(7) 0.0194(7) 0.0200(8) 0.0078(6) 0.0101(6) 0.0072(5) O8 0.0154(7) 0.0242(8) 0.0173(7) 0.0094(6) 0.0083(6) 0.0063(6) C1 0.0118(9) 0.0138(9) 0.0105(9) -0.0007(7) 0.0051(7) 0.0021(7) C2 0.0135(9) 0.0154(9) 0.0116(9) 0.0026(7) 0.0057(7) 0.0054(7) C3 0.0133(9) 0.0131(9) 0.0163(9) 0.0020(7) 0.0074(8) 0.0008(7) C4 0.0096(9) 0.0151(9) 0.0135(9) -0.0011(7) 0.0050(7) 0.0009(7) C5 0.0116(9) 0.0131(9) 0.0123(9) -0.0002(7) 0.0051(7) 0.0024(7) C6 0.0130(9) 0.0115(9) 0.0134(9) 0.0009(7) 0.0067(7) 0.0016(7) C7 0.0099(9) 0.0134(9) 0.0143(9) 0.0015(7) 0.0033(7) 0.0018(7) C8 0.0129(9) 0.0114(9) 0.0135(9) 0.0042(7) 0.0020(7) 0.0032(7) C9 0.0115(9) 0.0161(9) 0.0153(9) 0.0043(7) 0.0035(7) 0.0012(7) C10 0.0140(9) 0.0172(10) 0.0141(9) 0.0011(8) 0.0018(8) -0.0027(8) C11 0.0172(10) 0.0164(10) 0.0103(9) 0.0018(7) 0.0031(8) 0.0004(8) C12 0.0117(9) 0.0139(9) 0.0135(9) 0.0054(7) 0.0015(7) 0.0014(7) C13 0.0115(9) 0.0110(9) 0.0133(9) 0.0029(7) 0.0004(7) 0.0007(7) C14 0.0136(9) 0.0168(10) 0.0108(9) 0.0033(7) 0.0028(7) -0.0003(7) C15 0.0124(9) 0.0161(9) 0.0127(9) 0.0048(7) 0.0058(7) -0.0005(7) C16 0.0119(9) 0.0189(10) 0.0115(9) -0.0004(7) 0.0045(7) -0.0041(7) C17 0.0151(9) 0.0146(9) 0.0182(10) -0.0017(8) 0.0079(8) -0.0004(7) C18 0.0113(9) 0.0173(10) 0.0180(10) 0.0037(8) 0.0068(8) 0.0019(7) C19 0.0116(9) 0.0153(9) 0.0130(9) 0.0020(7) 0.0063(7) -0.0013(7) C20 0.0124(9) 0.0130(9) 0.0132(9) 0.0017(7) 0.0063(7) -0.0007(7) C21 0.0101(9) 0.0138(9) 0.0145(9) 0.0027(7) 0.0044(7) 0.0020(7) C22 0.0102(9) 0.0122(9) 0.0124(9) 0.0001(7) 0.0018(7) -0.0019(7) C23 0.0088(8) 0.0139(9) 0.0166(9) 0.0010(7) 0.0040(7) 0.0004(7) C24 0.0129(9) 0.0158(9) 0.0167(9) 0.0048(8) 0.0038(8) 0.0030(7) C25 0.0136(9) 0.0147(9) 0.0131(9) 0.0023(7) 0.0046(7) 0.0000(7) C26 0.0103(9) 0.0117(9) 0.0126(9) -0.0007(7) 0.0020(7) -0.0013(7) C27 0.0100(9) 0.0117(9) 0.0122(9) 0.0011(7) 0.0005(7) 0.0000(7) C28 0.0117(9) 0.0137(9) 0.0125(9) 0.0012(7) 0.0033(7) 0.0012(7) C29 0.0140(9) 0.0143(9) 0.0152(9) 0.0008(7) 0.0033(8) 0.0014(7) C30 0.0223(10) 0.0169(10) 0.0226(11) 0.0055(8) 0.0043(9) 0.0054(8) C31 0.0157(9) 0.0182(10) 0.0156(9) 0.0056(8) 0.0027(8) -0.0011(8) C32 0.0225(11) 0.0196(11) 0.0281(11) 0.0102(9) 0.0007(9) 0.0000(9) C33 0.0128(9) 0.0153(10) 0.0154(9) 0.0029(7) 0.0039(8) 0.0001(7) C34 0.0169(10) 0.0181(10) 0.0201(10) 0.0009(8) 0.0027(8) -0.0040(8) C35 0.0127(9) 0.0143(9) 0.0172(9) 0.0003(7) 0.0042(8) 0.0016(7) C36 0.0179(10) 0.0180(10) 0.0229(11) -0.0013(8) 0.0000(9) -0.0016(8) O2S 0.0355(11) 0.113(2) 0.0361(11) -0.0181(12) 0.0135(9) -0.0241(12) C2S 0.0231(13) 0.064(2) 0.0536(18) 0.0054(15) 0.0072(12) -0.0003(13) O1W 0.0205(12) 0.0135(11) 0.0161(11) -0.0019(9) -0.0033(10) -0.0024(9) O2W 0.0290(13) 0.0122(11) 0.0200(12) 0.0039(9) 0.0132(10) -0.0041(9) O3W 0.0026(19) 0.013(2) 0.018(2) 0.0008(17) -0.0030(17) 0.0015(16) O9 0.0300(9) 0.0200(8) 0.0477(11) 0.0021(7) 0.0068(8) 0.0022(7) O10 0.0313(9) 0.0217(8) 0.0272(8) 0.0022(6) 0.0004(7) 0.0031(7) C41 0.0287(12) 0.0200(11) 0.0217(11) 0.0008(8) 0.0135(9) 0.0008(9) C42 0.0285(12) 0.0275(12) 0.0244(11) 0.0021(9) 0.0133(10) 0.0022(9) C43 0.0261(12) 0.0424(14) 0.0294(12) -0.0050(11) 0.0110(10) 0.0078(10) Cl1 0.0518(4) 0.0428(4) 0.0373(4) 0.0068(3) 0.0117(3) 0.0267(3) O1S 0.0323(10) 0.0425(11) 0.0430(11) 0.0051(8) 0.0058(8) -0.0081(8) C1S 0.0332(14) 0.075(2) 0.0321(14) 0.0047(14) 0.0099(12) -0.0135(14) _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 O1 C2 1.382(2) . ? O2 C4 1.379(2) . ? O3 C9 1.386(2) . ? O4 C11 1.376(2) . ? O5 C16 1.384(2) . ? O6 C18 1.364(2) . ? O7 C23 1.384(2) . ? O8 C25 1.392(2) . ? C1 C6 1.389(3) . ? C1 C2 1.393(3) . ? C1 C28 1.524(3) . ? C2 C3 1.387(3) . ? C3 C4 1.389(3) . ? C4 C5 1.397(3) . ? C5 C6 1.401(3) . ? C5 C7 1.525(2) . ? C7 C8 1.527(3) . ? C7 C29 1.537(3) . ? C8 C13 1.397(3) . ? C8 C9 1.398(3) . ? C9 C10 1.384(3) . ? C10 C11 1.388(3) . ? C11 C12 1.400(3) . ? C12 C13 1.389(3) . ? C12 C14 1.529(3) . ? C14 C15 1.527(3) . ? C14 C31 1.538(3) . ? C15 C16 1.395(3) . ? C15 C20 1.400(3) . ? C16 C17 1.389(3) . ? C17 C18 1.391(3) . ? C18 C19 1.399(3) . ? C19 C20 1.392(3) . ? C19 C21 1.524(3) . ? C21 C22 1.529(3) . ? C21 C33 1.535(3) . ? C22 C27 1.398(3) . ? C22 C23 1.398(3) . ? C23 C24 1.387(3) . ? C24 C25 1.383(3) . ? C25 C26 1.395(3) . ? C26 C27 1.394(3) . ? C26 C28 1.530(3) . ? C28 C35 1.536(3) . ? C29 C30 1.525(3) . ? C31 C32 1.523(3) . ? C33 C34 1.528(3) . ? C35 C36 1.526(3) . ? O2S C2S 1.419(3) . ? O9 C41 1.305(3) . ? O10 C41 1.221(3) . ? C41 C42 1.488(3) . ? C42 C43 1.322(3) . ? C43 Cl1 1.720(3) . ? O1S C1S 1.433(3) . ? 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 C6 C1 C2 117.22(17) . . ? C6 C1 C28 122.74(16) . . ? C2 C1 C28 120.04(16) . . ? O1 C2 C3 120.77(17) . . ? O1 C2 C1 117.91(16) . . ? C3 C2 C1 121.32(17) . . ? C2 C3 C4 119.66(17) . . ? O2 C4 C3 115.16(16) . . ? O2 C4 C5 123.33(17) . . ? C3 C4 C5 121.50(17) . . ? C4 C5 C6 116.56(17) . . ? C4 C5 C7 121.40(16) . . ? C6 C5 C7 122.02(16) . . ? C1 C6 C5 123.73(17) . . ? C5 C7 C8 110.66(14) . . ? C5 C7 C29 113.54(15) . . ? C8 C7 C29 111.68(15) . . ? C13 C8 C9 116.79(17) . . ? C13 C8 C7 121.66(16) . . ? C9 C8 C7 121.55(16) . . ? C10 C9 O3 120.96(17) . . ? C10 C9 C8 121.57(17) . . ? O3 C9 C8 117.48(17) . . ? C9 C10 C11 119.66(18) . . ? O4 C11 C10 121.17(17) . . ? O4 C11 C12 117.69(17) . . ? C10 C11 C12 121.14(18) . . ? C13 C12 C11 117.21(17) . . ? C13 C12 C14 121.49(16) . . ? C11 C12 C14 121.29(17) . . ? C12 C13 C8 123.62(17) . . ? C15 C14 C12 110.29(15) . . ? C15 C14 C31 114.09(15) . . ? C12 C14 C31 111.89(16) . . ? C16 C15 C20 116.74(17) . . ? C16 C15 C14 120.96(16) . . ? C20 C15 C14 122.27(17) . . ? O5 C16 C17 115.55(17) . . ? O5 C16 C15 122.65(17) . . ? C17 C16 C15 121.79(17) . . ? C16 C17 C18 119.57(18) . . ? O6 C18 C17 121.52(17) . . ? O6 C18 C19 117.53(17) . . ? C17 C18 C19 120.95(17) . . ? C20 C19 C18 117.49(17) . . ? C20 C19 C21 123.52(17) . . ? C18 C19 C21 118.99(16) . . ? C19 C20 C15 123.44(17) . . ? C19 C21 C22 111.12(14) . . ? C19 C21 C33 113.65(15) . . ? C22 C21 C33 111.97(15) . . ? C27 C22 C23 116.52(17) . . ? C27 C22 C21 120.14(16) . . ? C23 C22 C21 123.33(16) . . ? O7 C23 C24 114.37(17) . . ? O7 C23 C22 124.48(17) . . ? C24 C23 C22 121.15(17) . . ? C25 C24 C23 120.14(17) . . ? C24 C25 O8 116.72(17) . . ? C24 C25 C26 121.42(17) . . ? O8 C25 C26 121.85(17) . . ? C27 C26 C25 116.56(17) . . ? C27 C26 C28 121.42(16) . . ? C25 C26 C28 122.02(16) . . ? C26 C27 C22 124.16(17) . . ? C1 C28 C26 110.45(14) . . ? C1 C28 C35 112.84(15) . . ? C26 C28 C35 112.62(15) . . ? C30 C29 C7 112.16(16) . . ? C32 C31 C14 111.76(16) . . ? C34 C33 C21 112.66(16) . . ? C36 C35 C28 112.68(16) . . ? O10 C41 O9 122.3(2) . . ? O10 C41 C42 121.00(19) . . ? O9 C41 C42 116.6(2) . . ? C43 C42 C41 128.9(2) . . ? C42 C43 Cl1 126.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 O1 -179.85(15) . . . . ? C28 C1 C2 O1 0.9(2) . . . . ? C6 C1 C2 C3 -0.4(3) . . . . ? C28 C1 C2 C3 -179.65(16) . . . . ? O1 C2 C3 C4 -179.67(16) . . . . ? C1 C2 C3 C4 0.9(3) . . . . ? C2 C3 C4 O2 -179.57(16) . . . . ? C2 C3 C4 C5 -1.0(3) . . . . ? O2 C4 C5 C6 178.98(16) . . . . ? C3 C4 C5 C6 0.5(3) . . . . ? O2 C4 C5 C7 -2.6(3) . . . . ? C3 C4 C5 C7 178.89(16) . . . . ? C2 C1 C6 C5 0.0(3) . . . . ? C28 C1 C6 C5 179.15(16) . . . . ? C4 C5 C6 C1 0.0(3) . . . . ? C7 C5 C6 C1 -178.37(16) . . . . ? C4 C5 C7 C8 -79.6(2) . . . . ? C6 C5 C7 C8 98.7(2) . . . . ? C4 C5 C7 C29 153.85(17) . . . . ? C6 C5 C7 C29 -27.8(2) . . . . ? C5 C7 C8 C13 -79.3(2) . . . . ? C29 C7 C8 C13 48.2(2) . . . . ? C5 C7 C8 C9 99.9(2) . . . . ? C29 C7 C8 C9 -132.54(18) . . . . ? C13 C8 C9 C10 -1.5(3) . . . . ? C7 C8 C9 C10 179.16(17) . . . . ? C13 C8 C9 O3 178.06(16) . . . . ? C7 C8 C9 O3 -1.3(3) . . . . ? O3 C9 C10 C11 -178.58(17) . . . . ? C8 C9 C10 C11 1.0(3) . . . . ? C9 C10 C11 O4 179.17(17) . . . . ? C9 C10 C11 C12 -0.2(3) . . . . ? O4 C11 C12 C13 -179.34(16) . . . . ? C10 C11 C12 C13 0.1(3) . . . . ? O4 C11 C12 C14 -0.1(3) . . . . ? C10 C11 C12 C14 179.31(17) . . . . ? C11 C12 C13 C8 -0.7(3) . . . . ? C14 C12 C13 C8 -179.93(17) . . . . ? C9 C8 C13 C12 1.4(3) . . . . ? C7 C8 C13 C12 -179.29(16) . . . . ? C13 C12 C14 C15 78.4(2) . . . . ? C11 C12 C14 C15 -100.8(2) . . . . ? C13 C12 C14 C31 -49.8(2) . . . . ? C11 C12 C14 C31 131.06(18) . . . . ? C12 C14 C15 C16 79.8(2) . . . . ? C31 C14 C15 C16 -153.24(17) . . . . ? C12 C14 C15 C20 -98.2(2) . . . . ? C31 C14 C15 C20 28.7(2) . . . . ? C20 C15 C16 O5 -178.50(16) . . . . ? C14 C15 C16 O5 3.3(3) . . . . ? C20 C15 C16 C17 0.6(3) . . . . ? C14 C15 C16 C17 -177.59(17) . . . . ? O5 C16 C17 C18 179.30(16) . . . . ? C15 C16 C17 C18 0.2(3) . . . . ? C16 C17 C18 O6 178.92(17) . . . . ? C16 C17 C18 C19 -1.2(3) . . . . ? O6 C18 C19 C20 -178.68(16) . . . . ? C17 C18 C19 C20 1.4(3) . . . . ? O6 C18 C19 C21 1.0(3) . . . . ? C17 C18 C19 C21 -178.92(17) . . . . ? C18 C19 C20 C15 -0.7(3) . . . . ? C21 C19 C20 C15 179.70(16) . . . . ? C16 C15 C20 C19 -0.3(3) . . . . ? C14 C15 C20 C19 177.83(16) . . . . ? C20 C19 C21 C22 100.9(2) . . . . ? C18 C19 C21 C22 -78.7(2) . . . . ? C20 C19 C21 C33 -26.5(2) . . . . ? C18 C19 C21 C33 153.89(17) . . . . ? C19 C21 C22 C27 -74.9(2) . . . . ? C33 C21 C22 C27 53.4(2) . . . . ? C19 C21 C22 C23 106.0(2) . . . . ? C33 C21 C22 C23 -125.70(18) . . . . ? C27 C22 C23 O7 -179.94(16) . . . . ? C21 C22 C23 O7 -0.8(3) . . . . ? C27 C22 C23 C24 0.9(3) . . . . ? C21 C22 C23 C24 179.99(17) . . . . ? O7 C23 C24 C25 179.73(16) . . . . ? C22 C23 C24 C25 -1.0(3) . . . . ? C23 C24 C25 O8 -179.46(17) . . . . ? C23 C24 C25 C26 -0.8(3) . . . . ? C24 C25 C26 C27 2.5(3) . . . . ? O8 C25 C26 C27 -178.87(16) . . . . ? C24 C25 C26 C28 -177.28(17) . . . . ? O8 C25 C26 C28 1.3(3) . . . . ? C25 C26 C27 C22 -2.7(3) . . . . ? C28 C26 C27 C22 177.11(16) . . . . ? C23 C22 C27 C26 1.0(3) . . . . ? C21 C22 C27 C26 -178.10(16) . . . . ? C6 C1 C28 C26 -100.4(2) . . . . ? C2 C1 C28 C26 78.8(2) . . . . ? C6 C1 C28 C35 26.7(2) . . . . ? C2 C1 C28 C35 -154.15(17) . . . . ? C27 C26 C28 C1 76.9(2) . . . . ? C25 C26 C28 C1 -103.3(2) . . . . ? C27 C26 C28 C35 -50.3(2) . . . . ? C25 C26 C28 C35 129.53(18) . . . . ? C5 C7 C29 C30 -173.79(16) . . . . ? C8 C7 C29 C30 60.2(2) . . . . ? C15 C14 C31 C32 171.73(17) . . . . ? C12 C14 C31 C32 -62.2(2) . . . . ? C19 C21 C33 C34 -173.31(16) . . . . ? C22 C21 C33 C34 59.8(2) . . . . ? C1 C28 C35 C36 171.70(16) . . . . ? C26 C28 C35 C36 -62.4(2) . . . . ? O10 C41 C42 C43 157.5(2) . . . . ? O9 C41 C42 C43 -23.9(3) . . . . ? C41 C42 C43 Cl1 0.1(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1O O7 0.78(3) 2.00(3) 2.772(2) 171(3) 2_766 O2 H2O O3 0.85(3) 1.89(3) 2.731(2) 170(3) . O3 H3O O5 0.80(3) 1.94(3) 2.709(2) 162(3) 2_665 O5 H5O O4 0.80(3) 1.98(3) 2.752(2) 164(3) . O6 H6O O10 0.79(3) 1.89(3) 2.670(2) 173(3) . O7 H7O O2 0.76(3) 2.14(3) 2.773(2) 142(3) 1_655 O7 H7O O6 0.76(3) 2.32(3) 2.863(2) 129(2) . O8 H8O O1 0.80(3) 1.95(3) 2.729(2) 164(3) . O9 H9O O1S 1.03(4) 1.55(4) 2.581(2) 175(4) . O1S H1S O2S 1.02 1.65 2.657(3) 169.1 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.691 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.057 #=======================================END data_CECR-Z-HClA-2MeOH-1.5H2O@200k _database_code_depnum_ccdc_archive 'CCDC 629575' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CECR-Z-HClA-2MeOH-1.5H2O@90k _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C41 H54 Cl O13.50' _chemical_formula_weight 798.29 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3681(4) _cell_length_b 13.4995(5) _cell_length_c 14.7379(6) _cell_angle_alpha 98.6833(11) _cell_angle_beta 111.0001(10) _cell_angle_gamma 95.1494(11) _cell_volume 2061.79(13) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 675 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 0.157 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.9692 _exptl_absorpt_correction_T_max 0.9814 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7979 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6255 _reflns_number_gt 5124 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+2.0034P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6255 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1502 _refine_ls_wR_factor_gt 0.1383 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 O1 O 0.80781(17) 0.60405(16) 0.57988(13) 0.0276(4) Uani 1 1 d . . . O2 O 0.41922(16) 0.60446(14) 0.31409(14) 0.0293(4) Uani 1 1 d . . . O3 O 0.31620(17) 0.64856(17) 0.12818(14) 0.0295(4) Uani 1 1 d . . . O4 O 0.5383(2) 0.61595(17) -0.09627(13) 0.0341(5) Uani 1 1 d . . . O5 O 0.77079(18) 0.54802(15) -0.03716(13) 0.0321(5) Uani 1 1 d . . . O6 O 1.14619(18) 0.54660(17) 0.24093(15) 0.0356(5) Uani 1 1 d . . . O7 O 1.29710(17) 0.59784(14) 0.44898(15) 0.0292(4) Uani 1 1 d . . . O8 O 1.06926(19) 0.63477(15) 0.65847(13) 0.0317(5) Uani 1 1 d . . . C1 C 0.7909(2) 0.74128(18) 0.49439(16) 0.0201(5) Uani 1 1 d . . . C2 C 0.7354(2) 0.64977(19) 0.50519(16) 0.0216(5) Uani 1 1 d . . . C3 C 0.6118(2) 0.60637(19) 0.44451(17) 0.0232(5) Uani 1 1 d . . . H3A H 0.5752 0.5445 0.4539 0.028 Uiso 1 1 calc R . . C4 C 0.5414(2) 0.65334(19) 0.36993(17) 0.0218(5) Uani 1 1 d . . . C5 C 0.5920(2) 0.74505(18) 0.35530(16) 0.0201(5) Uani 1 1 d . . . C6 C 0.7168(2) 0.78607(18) 0.41931(16) 0.0207(5) Uani 1 1 d . . . H6A H 0.7531 0.8485 0.4109 0.025 Uiso 1 1 calc R . . C7 C 0.5154(2) 0.79584(18) 0.27220(17) 0.0217(5) Uani 1 1 d . . . H7A H 0.4244 0.7823 0.2654 0.026 Uiso 1 1 calc R . . C8 C 0.5204(2) 0.74619(19) 0.17316(17) 0.0209(5) Uani 1 1 d . . . C9 C 0.4203(2) 0.6754(2) 0.10366(17) 0.0236(6) Uani 1 1 d . . . C10 C 0.4244(2) 0.6317(2) 0.01383(18) 0.0269(6) Uani 1 1 d . . . H10A H 0.3548 0.5837 -0.0327 0.032 Uiso 1 1 calc R . . C11 C 0.5309(2) 0.6586(2) -0.00791(17) 0.0253(6) Uani 1 1 d . . . C12 C 0.6342(2) 0.72843(19) 0.05945(17) 0.0220(5) Uani 1 1 d . . . C13 C 0.6262(2) 0.77023(19) 0.14884(17) 0.0220(5) Uani 1 1 d . . . H13A H 0.6962 0.8176 0.1958 0.026 Uiso 1 1 calc R . . C14 C 0.7526(2) 0.75823(19) 0.03687(17) 0.0237(5) Uani 1 1 d . . . H14A H 0.7286 0.7331 -0.0358 0.028 Uiso 1 1 calc R . . C15 C 0.8598(2) 0.70222(19) 0.08980(17) 0.0218(5) Uani 1 1 d . . . C16 C 0.8617(2) 0.6017(2) 0.05150(17) 0.0245(6) Uani 1 1 d . . . C17 C 0.9566(2) 0.5488(2) 0.10011(18) 0.0276(6) Uani 1 1 d . . . H17A H 0.9562 0.4805 0.0721 0.033 Uiso 1 1 calc R . . C18 C 1.0519(2) 0.5961(2) 0.18968(18) 0.0256(6) Uani 1 1 d . . . C19 C 1.0562(2) 0.69721(19) 0.23085(17) 0.0205(5) Uani 1 1 d . . . C20 C 0.9591(2) 0.74762(19) 0.17970(16) 0.0213(5) Uani 1 1 d . . . H20A H 0.9602 0.8162 0.2072 0.026 Uiso 1 1 calc R . . C21 C 1.1646(2) 0.74634(19) 0.32892(17) 0.0215(5) Uani 1 1 d . . . H21A H 1.2425 0.7183 0.3275 0.026 Uiso 1 1 calc R . . C22 C 1.1394(2) 0.71482(18) 0.41662(16) 0.0204(5) Uani 1 1 d . . . C23 C 1.2042(2) 0.64604(19) 0.46988(17) 0.0224(5) Uani 1 1 d . . . C24 C 1.1787(2) 0.6205(2) 0.54902(18) 0.0259(6) Uani 1 1 d . . . H24A H 1.2234 0.5731 0.5840 0.031 Uiso 1 1 calc R . . C25 C 1.0886(2) 0.66357(19) 0.57750(17) 0.0230(5) Uani 1 1 d . . . C26 C 1.0227(2) 0.73453(18) 0.52864(16) 0.0207(5) Uani 1 1 d . . . C27 C 1.0492(2) 0.75632(18) 0.44805(16) 0.0205(5) Uani 1 1 d . . . H27A H 1.0029 0.8024 0.4121 0.025 Uiso 1 1 calc R . . C28 C 0.9271(2) 0.78689(19) 0.56230(17) 0.0221(5) Uani 1 1 d . . . H28A H 0.9390 0.7718 0.6291 0.026 Uiso 1 1 calc R . . C29 C 0.5529(2) 0.91144(19) 0.29357(18) 0.0270(6) Uani 1 1 d . . . H29A H 0.5511 0.9402 0.3589 0.032 Uiso 1 1 calc R . . H29B H 0.6413 0.9278 0.2971 0.032 Uiso 1 1 calc R . . C30 C 0.4644(3) 0.9605(2) 0.2147(2) 0.0400(7) Uani 1 1 d . . . H30A H 0.4910 1.0342 0.2320 0.060 Uiso 1 1 calc R . . H30B H 0.3768 0.9447 0.2111 0.060 Uiso 1 1 calc R . . H30C H 0.4684 0.9343 0.1503 0.060 Uiso 1 1 calc R . . C31 C 0.7901(2) 0.8734(2) 0.05575(19) 0.0302(6) Uani 1 1 d . . . H31A H 0.8076 0.9022 0.1260 0.036 Uiso 1 1 calc R . . H31B H 0.8696 0.8890 0.0439 0.036 Uiso 1 1 calc R . . C32 C 0.6866(3) 0.9235(2) -0.0103(2) 0.0456(8) Uani 1 1 d . . . H32A H 0.7157 0.9967 0.0028 0.068 Uiso 1 1 calc R . . H32B H 0.6090 0.9113 0.0036 0.068 Uiso 1 1 calc R . . H32C H 0.6683 0.8948 -0.0800 0.068 Uiso 1 1 calc R . . C33 C 1.1960(2) 0.8616(2) 0.34278(18) 0.0264(6) Uani 1 1 d . . . H33A H 1.2092 0.8782 0.2836 0.032 Uiso 1 1 calc R . . H33B H 1.1226 0.8928 0.3482 0.032 Uiso 1 1 calc R . . C34 C 1.3151(3) 0.9068(2) 0.4350(2) 0.0381(7) Uani 1 1 d . . . H34A H 1.3316 0.9804 0.4405 0.057 Uiso 1 1 calc R . . H34B H 1.3883 0.8769 0.4295 0.057 Uiso 1 1 calc R . . H34C H 1.3017 0.8920 0.4939 0.057 Uiso 1 1 calc R . . C35 C 0.9530(2) 0.9027(2) 0.57569(18) 0.0276(6) Uani 1 1 d . . . H35A H 0.9492 0.9206 0.5121 0.033 Uiso 1 1 calc R . . H35B H 0.8853 0.9320 0.5930 0.033 Uiso 1 1 calc R . . C36 C 1.0823(3) 0.9493(2) 0.6560(2) 0.0416(7) Uani 1 1 d . . . H36A H 1.0944 1.0231 0.6611 0.062 Uiso 1 1 calc R . . H36B H 1.1499 0.9213 0.6388 0.062 Uiso 1 1 calc R . . H36C H 1.0857 0.9337 0.7196 0.062 Uiso 1 1 calc R . . O2S O 0.7848(3) 0.2316(4) 0.1683(2) 0.1149(14) Uani 1 1 d . . . H2S H 0.8275 0.2935 0.2211 0.172 Uiso 1 1 d R . . C2S C 0.6715(4) 0.1916(4) 0.1746(4) 0.0913(15) Uani 1 1 d . . . H2S1 H 0.6907 0.1564 0.2305 0.137 Uiso 1 1 calc R . . H2S2 H 0.6198 0.1436 0.1130 0.137 Uiso 1 1 calc R . . H2S3 H 0.6241 0.2467 0.1847 0.137 Uiso 1 1 calc R . . O1W O 0.2990(5) 0.5380(4) 0.7702(3) 0.0831(16) Uani 0.60 1 d P A 1 H1WA H 0.2333 0.4887 0.7199 0.125 Uiso 0.60 1 d PR A 1 H1WB H 0.2867 0.5716 0.8305 0.125 Uiso 0.60 1 d PR A 1 O2W O 0.2321(3) 0.4423(3) 0.7417(2) 0.0377(8) Uani 0.60 1 d P B 2 H2WA H 0.1852 0.3834 0.7218 0.057 Uiso 0.60 1 d PR B 2 H2WB H 0.2366 0.4606 0.6881 0.057 Uiso 0.60 1 d PR B 2 O3W O 0.3547(5) 0.4614(4) 0.8026(4) 0.0283(14) Uani 0.30 1 d P C 3 H3WA H 0.2757 0.4506 0.8063 0.043 Uiso 0.30 1 d PR C 3 H3WB H 0.3558 0.4872 0.7528 0.043 Uiso 0.30 1 d PR C 3 H1O H 0.776(3) 0.547(3) 0.575(3) 0.046(10) Uiso 1 1 d . . . H2O H 0.387(3) 0.624(3) 0.259(3) 0.058(11) Uiso 1 1 d . . . H3O H 0.279(3) 0.596(3) 0.091(3) 0.052(12) Uiso 1 1 d . . . H40 H 0.474(4) 0.586(4) -0.127(3) 0.086(17) Uiso 1 1 d . . . H5O H 0.711(3) 0.573(3) -0.055(2) 0.043(10) Uiso 1 1 d . . . H6O H 1.138(4) 0.490(3) 0.217(3) 0.053(11) Uiso 1 1 d . . . H7O H 1.296(4) 0.608(3) 0.399(3) 0.060(12) Uiso 1 1 d . . . H8O H 0.990(4) 0.623(3) 0.645(3) 0.055(11) Uiso 1 1 d . . . O1S O 0.9242(3) 0.1411(2) 0.0781(2) 0.0750(8) Uani 1 1 d . . . H1S H 0.8781 0.1826 0.1149 0.112 Uiso 1 1 d R . . C1S C 0.8851(4) 0.1770(4) -0.0134(3) 0.0909(16) Uani 1 1 d . . . H1S1 H 0.8021 0.1997 -0.0263 0.136 Uiso 1 1 calc R . . H1S2 H 0.8779 0.1219 -0.0676 0.136 Uiso 1 1 calc R . . H1S3 H 0.9484 0.2337 -0.0088 0.136 Uiso 1 1 calc R . . O9 O 1.1630(3) 0.19378(19) 0.1890(2) 0.0655(7) Uani 1 1 d . . . H9O H 1.071(6) 0.165(4) 0.145(4) 0.120(19) Uiso 1 1 d . . . O10 O 1.1122(2) 0.34603(17) 0.17870(17) 0.0586(7) Uani 1 1 d . . . C41 C 1.1914(3) 0.2921(2) 0.2089(2) 0.0409(7) Uani 1 1 d . . . C42 C 1.3268(3) 0.3357(3) 0.2688(2) 0.0501(8) Uani 1 1 d . . . H42A H 1.3525 0.4023 0.2623 0.060 Uiso 1 1 calc R . . C43 C 1.4167(4) 0.2949(3) 0.3300(3) 0.0643(11) Uani 1 1 d . . . H43A H 1.4987 0.3351 0.3617 0.077 Uiso 1 1 calc R . . Cl1 Cl 1.40013(13) 0.17686(9) 0.35796(8) 0.0894(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0260(10) 0.0271(12) 0.0287(9) 0.0121(9) 0.0069(8) 0.0035(10) O2 0.0186(9) 0.0325(12) 0.0315(10) 0.0088(9) 0.0041(8) -0.0036(9) O3 0.0216(9) 0.0318(13) 0.0285(9) -0.0027(9) 0.0079(8) -0.0066(10) O4 0.0285(11) 0.0449(14) 0.0208(9) -0.0040(9) 0.0067(8) -0.0069(11) O5 0.0251(10) 0.0329(12) 0.0272(9) -0.0052(8) 0.0025(8) -0.0007(10) O6 0.0285(10) 0.0256(12) 0.0419(11) -0.0014(10) 0.0027(9) 0.0089(10) O7 0.0268(10) 0.0324(11) 0.0373(11) 0.0148(9) 0.0177(8) 0.0122(9) O8 0.0290(10) 0.0429(12) 0.0312(10) 0.0183(9) 0.0150(8) 0.0122(10) C1 0.0200(12) 0.0215(14) 0.0195(11) 0.0016(10) 0.0091(10) 0.0035(12) C2 0.0225(12) 0.0243(15) 0.0189(11) 0.0044(11) 0.0085(10) 0.0059(12) C3 0.0237(13) 0.0209(14) 0.0266(12) 0.0044(11) 0.0121(10) 0.0006(12) C4 0.0160(12) 0.0249(15) 0.0222(11) 0.0012(11) 0.0066(10) -0.0007(12) C5 0.0197(12) 0.0192(14) 0.0201(11) 0.0008(10) 0.0075(10) 0.0021(12) C6 0.0213(12) 0.0174(14) 0.0228(11) 0.0018(10) 0.0090(10) 0.0007(12) C7 0.0179(12) 0.0217(14) 0.0232(11) 0.0033(10) 0.0057(10) 0.0029(11) C8 0.0196(12) 0.0191(14) 0.0209(11) 0.0050(10) 0.0038(10) 0.0024(12) C9 0.0185(12) 0.0234(15) 0.0249(12) 0.0042(11) 0.0045(10) 0.0003(12) C10 0.0220(12) 0.0285(16) 0.0214(12) -0.0005(11) 0.0024(10) -0.0058(12) C11 0.0260(13) 0.0261(15) 0.0189(11) 0.0023(11) 0.0045(10) 0.0002(13) C12 0.0196(12) 0.0232(15) 0.0206(11) 0.0084(11) 0.0033(10) 0.0019(12) C13 0.0195(12) 0.0205(14) 0.0209(11) 0.0042(10) 0.0018(9) 0.0015(11) C14 0.0234(13) 0.0268(15) 0.0178(11) 0.0056(11) 0.0048(10) -0.0009(12) C15 0.0213(12) 0.0239(15) 0.0201(11) 0.0050(11) 0.0086(10) -0.0014(12) C16 0.0223(12) 0.0268(16) 0.0214(11) -0.0003(11) 0.0086(10) -0.0038(12) C17 0.0265(13) 0.0242(15) 0.0300(13) -0.0025(11) 0.0119(11) 0.0022(13) C18 0.0198(12) 0.0258(15) 0.0303(13) 0.0039(11) 0.0088(10) 0.0043(12) C19 0.0171(11) 0.0215(14) 0.0226(11) 0.0028(10) 0.0089(9) -0.0026(11) C20 0.0239(12) 0.0199(14) 0.0200(11) 0.0033(10) 0.0091(10) 0.0002(12) C21 0.0180(12) 0.0220(14) 0.0239(12) 0.0038(11) 0.0077(10) 0.0015(12) C22 0.0154(11) 0.0194(14) 0.0206(11) 0.0006(10) 0.0028(9) -0.0031(11) C23 0.0174(12) 0.0205(14) 0.0269(12) 0.0017(11) 0.0072(10) 0.0001(12) C24 0.0219(12) 0.0266(15) 0.0296(13) 0.0110(11) 0.0074(10) 0.0063(12) C25 0.0206(12) 0.0235(14) 0.0228(11) 0.0056(11) 0.0060(10) -0.0003(12) C26 0.0162(11) 0.0189(14) 0.0206(11) -0.0005(10) 0.0024(9) -0.0027(11) C27 0.0173(11) 0.0176(13) 0.0211(11) 0.0021(10) 0.0019(9) 0.0007(11) C28 0.0200(12) 0.0249(15) 0.0198(11) 0.0034(10) 0.0063(10) 0.0030(12) C29 0.0263(13) 0.0248(15) 0.0270(12) 0.0035(11) 0.0072(10) 0.0042(13) C30 0.0441(17) 0.0295(17) 0.0416(16) 0.0097(13) 0.0084(14) 0.0109(15) C31 0.0275(14) 0.0300(16) 0.0296(13) 0.0110(12) 0.0060(11) -0.0013(13) C32 0.0397(17) 0.0357(19) 0.0516(18) 0.0208(15) 0.0014(14) 0.0028(16) C33 0.0238(13) 0.0248(15) 0.0280(12) 0.0060(11) 0.0073(10) -0.0004(12) C34 0.0342(15) 0.0323(18) 0.0369(15) 0.0023(13) 0.0053(12) -0.0073(15) C35 0.0249(13) 0.0246(15) 0.0283(13) -0.0001(11) 0.0064(11) 0.0023(13) C36 0.0361(16) 0.0297(18) 0.0423(16) -0.0024(14) 0.0005(13) -0.0016(15) O2S 0.0630(19) 0.188(4) 0.0634(19) -0.023(2) 0.0201(15) -0.034(2) C2S 0.044(2) 0.113(4) 0.101(4) 0.024(3) 0.009(2) 0.006(3) O1W 0.093(4) 0.072(4) 0.041(2) 0.009(2) -0.017(2) -0.029(3) O2W 0.046(2) 0.030(2) 0.0335(17) 0.0063(16) 0.0141(15) -0.0103(18) O3W 0.004(2) 0.009(3) 0.049(3) -0.017(3) -0.008(2) 0.000(3) O1S 0.0582(16) 0.073(2) 0.0777(19) 0.0096(16) 0.0138(14) -0.0132(16) C1S 0.063(3) 0.140(5) 0.062(3) 0.022(3) 0.020(2) -0.015(3) O9 0.0568(17) 0.0314(15) 0.093(2) 0.0042(14) 0.0143(15) 0.0029(14) O10 0.0683(16) 0.0340(13) 0.0527(13) 0.0049(11) 0.0001(12) 0.0068(13) C41 0.0534(19) 0.034(2) 0.0373(15) 0.0029(14) 0.0224(15) 0.0021(18) C42 0.056(2) 0.052(2) 0.0445(17) 0.0027(16) 0.0256(16) 0.0010(19) C43 0.052(2) 0.078(3) 0.059(2) -0.008(2) 0.0222(18) 0.016(2) Cl1 0.1061(9) 0.0840(8) 0.0758(7) 0.0136(6) 0.0230(6) 0.0559(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.384(3) . ? O2 C4 1.376(3) . ? O3 C9 1.390(3) . ? O4 C11 1.377(3) . ? O5 C16 1.383(3) . ? O6 C18 1.367(3) . ? O7 C23 1.389(3) . ? O8 C25 1.391(3) . ? C1 C6 1.388(3) . ? C1 C2 1.393(3) . ? C1 C28 1.520(3) . ? C2 C3 1.382(3) . ? C3 C4 1.386(3) . ? C4 C5 1.397(3) . ? C5 C6 1.397(3) . ? C5 C7 1.525(3) . ? C7 C29 1.534(4) . ? C7 C8 1.534(3) . ? C8 C9 1.389(4) . ? C8 C13 1.398(3) . ? C9 C10 1.384(3) . ? C10 C11 1.391(4) . ? C11 C12 1.391(4) . ? C12 C13 1.391(3) . ? C12 C14 1.533(3) . ? C14 C15 1.525(3) . ? C14 C31 1.531(4) . ? C15 C16 1.393(4) . ? C15 C20 1.401(3) . ? C16 C17 1.388(3) . ? C17 C18 1.386(4) . ? C18 C19 1.396(4) . ? C19 C20 1.395(3) . ? C19 C21 1.528(3) . ? C21 C33 1.530(4) . ? C21 C22 1.531(3) . ? C22 C27 1.395(3) . ? C22 C23 1.396(3) . ? C23 C24 1.381(3) . ? C24 C25 1.380(3) . ? C25 C26 1.396(3) . ? C26 C27 1.391(3) . ? C26 C28 1.531(3) . ? C28 C35 1.533(4) . ? C29 C30 1.522(3) . ? C31 C32 1.521(3) . ? C33 C34 1.528(4) . ? C35 C36 1.523(4) . ? O2S C2S 1.392(5) . ? O1S C1S 1.434(5) . ? O9 C41 1.300(4) . ? O10 C41 1.212(4) . ? C41 C42 1.483(5) . ? C42 C43 1.323(5) . ? C43 Cl1 1.716(5) . ? 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 C6 C1 C2 116.9(2) . . ? C6 C1 C28 123.0(2) . . ? C2 C1 C28 120.1(2) . . ? C3 C2 O1 120.9(2) . . ? C3 C2 C1 121.4(2) . . ? O1 C2 C1 117.7(2) . . ? C2 C3 C4 119.8(2) . . ? O2 C4 C3 115.3(2) . . ? O2 C4 C5 123.3(2) . . ? C3 C4 C5 121.4(2) . . ? C6 C5 C4 116.4(2) . . ? C6 C5 C7 122.1(2) . . ? C4 C5 C7 121.4(2) . . ? C1 C6 C5 124.1(2) . . ? C5 C7 C29 113.97(19) . . ? C5 C7 C8 110.51(18) . . ? C29 C7 C8 111.7(2) . . ? C9 C8 C13 116.9(2) . . ? C9 C8 C7 121.7(2) . . ? C13 C8 C7 121.4(2) . . ? C10 C9 C8 121.6(2) . . ? C10 C9 O3 120.9(2) . . ? C8 C9 O3 117.5(2) . . ? C9 C10 C11 119.6(2) . . ? O4 C11 C10 121.1(2) . . ? O4 C11 C12 117.8(2) . . ? C10 C11 C12 121.1(2) . . ? C13 C12 C11 117.3(2) . . ? C13 C12 C14 121.0(2) . . ? C11 C12 C14 121.7(2) . . ? C12 C13 C8 123.4(2) . . ? C15 C14 C31 114.6(2) . . ? C15 C14 C12 110.21(18) . . ? C31 C14 C12 112.1(2) . . ? C16 C15 C20 116.7(2) . . ? C16 C15 C14 121.1(2) . . ? C20 C15 C14 122.2(2) . . ? O5 C16 C17 115.3(2) . . ? O5 C16 C15 122.9(2) . . ? C17 C16 C15 121.8(2) . . ? C18 C17 C16 119.6(2) . . ? O6 C18 C17 121.7(2) . . ? O6 C18 C19 117.1(2) . . ? C17 C18 C19 121.2(2) . . ? C20 C19 C18 117.4(2) . . ? C20 C19 C21 123.5(2) . . ? C18 C19 C21 119.1(2) . . ? C19 C20 C15 123.3(2) . . ? C19 C21 C33 113.68(19) . . ? C19 C21 C22 111.03(19) . . ? C33 C21 C22 112.11(19) . . ? C27 C22 C23 116.5(2) . . ? C27 C22 C21 120.1(2) . . ? C23 C22 C21 123.3(2) . . ? C24 C23 O7 114.6(2) . . ? C24 C23 C22 121.2(2) . . ? O7 C23 C22 124.2(2) . . ? C25 C24 C23 120.2(2) . . ? C24 C25 O8 116.8(2) . . ? C24 C25 C26 121.3(2) . . ? O8 C25 C26 121.9(2) . . ? C27 C26 C25 116.5(2) . . ? C27 C26 C28 121.4(2) . . ? C25 C26 C28 122.0(2) . . ? C26 C27 C22 124.2(2) . . ? C1 C28 C26 110.81(18) . . ? C1 C28 C35 113.08(19) . . ? C26 C28 C35 112.6(2) . . ? C30 C29 C7 112.4(2) . . ? C32 C31 C14 112.3(2) . . ? C34 C33 C21 112.4(2) . . ? C36 C35 C28 112.7(2) . . ? O10 C41 O9 122.0(3) . . ? O10 C41 C42 121.2(3) . . ? O9 C41 C42 116.8(3) . . ? C43 C42 C41 129.2(4) . . ? C42 C43 Cl1 126.6(3) . . ? _diffrn_measured_fraction_theta_max 0.861 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.861 _refine_diff_density_max 0.611 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.051 #=======================================END data_CECR-Z-HClA-2MeOH-1.5H2O@90k-1h _database_code_depnum_ccdc_archive 'CCDC 629576' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CECR-Z-HClA-2MeOH-1.5H2O@90k-1h _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C41 H54 Cl O13.50' _chemical_formula_weight 798.29 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3657(3) _cell_length_b 13.3996(3) _cell_length_c 14.6514(4) _cell_angle_alpha 98.9111(8) _cell_angle_beta 110.2197(8) _cell_angle_gamma 95.1864(8) _cell_volume 2043.48(9) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 675 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.9689 _exptl_absorpt_correction_T_max 0.9812 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16516 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7178 _reflns_number_gt 5773 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+2.2830P] 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 7178 _refine_ls_number_parameters 550 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1695 _refine_ls_wR_factor_gt 0.1605 _refine_ls_goodness_of_fit_ref 1.169 _refine_ls_restrained_S_all 1.169 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.001 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 O1 O 0.80115(18) 0.60497(14) 0.58024(13) 0.0270(4) Uani 1 1 d . . . O2 O 0.41893(17) 0.60497(14) 0.31331(14) 0.0287(4) Uani 1 1 d . . . O3 O 0.31778(17) 0.65130(14) 0.12935(14) 0.0290(4) Uani 1 1 d . . . O4 O 0.54328(18) 0.61358(15) -0.09610(13) 0.0331(5) Uani 1 1 d . . . O5 O 0.77258(18) 0.54576(14) -0.03843(14) 0.0307(4) Uani 1 1 d . . . O6 O 1.14489(18) 0.54323(14) 0.23746(15) 0.0337(5) Uani 1 1 d . . . O7 O 1.29159(19) 0.59706(15) 0.44562(15) 0.0341(5) Uani 1 1 d . . . O8 O 1.05904(18) 0.63280(15) 0.65488(14) 0.0307(4) Uani 1 1 d . . . C1 C 0.7871(2) 0.74341(19) 0.49506(18) 0.0205(5) Uani 1 1 d . . . C2 C 0.7312(2) 0.65113(19) 0.50601(18) 0.0224(5) Uani 1 1 d . . . C3 C 0.6087(2) 0.60708(19) 0.44457(19) 0.0230(5) Uani 1 1 d . . . H3A H 0.5719 0.5445 0.4534 0.028 Uiso 1 1 calc R . . C4 C 0.5399(2) 0.65478(19) 0.37003(19) 0.0225(5) Uani 1 1 d . . . C5 C 0.5910(2) 0.74717(18) 0.35610(18) 0.0203(5) Uani 1 1 d . . . C6 C 0.7146(2) 0.78863(18) 0.41992(18) 0.0201(5) Uani 1 1 d . . . H6A H 0.7512 0.8515 0.4115 0.024 Uiso 1 1 calc R . . C7 C 0.5159(2) 0.79854(18) 0.27313(18) 0.0215(5) Uani 1 1 d . . . H7A H 0.4251 0.7855 0.2667 0.026 Uiso 1 1 calc R . . C8 C 0.5218(2) 0.74878(18) 0.17363(18) 0.0219(5) Uani 1 1 d . . . C9 C 0.4222(2) 0.6768(2) 0.10446(19) 0.0247(6) Uani 1 1 d . . . C10 C 0.4274(3) 0.6321(2) 0.01423(19) 0.0272(6) Uani 1 1 d . . . H10A H 0.3582 0.5838 -0.0323 0.033 Uiso 1 1 calc R . . C11 C 0.5338(3) 0.6579(2) -0.00787(19) 0.0268(6) Uani 1 1 d . . . C12 C 0.6370(2) 0.72894(19) 0.05935(18) 0.0234(6) Uani 1 1 d . . . C13 C 0.6273(2) 0.77166(18) 0.14887(18) 0.0217(5) Uani 1 1 d . . . H13A H 0.6969 0.8193 0.1958 0.026 Uiso 1 1 calc R . . C14 C 0.7548(2) 0.7577(2) 0.03568(18) 0.0244(6) Uani 1 1 d . . . H14A H 0.7312 0.7319 -0.0371 0.029 Uiso 1 1 calc R . . C15 C 0.8610(2) 0.70132(19) 0.08834(18) 0.0224(5) Uani 1 1 d . . . C16 C 0.8632(3) 0.5993(2) 0.05016(18) 0.0251(6) Uani 1 1 d . . . C17 C 0.9562(3) 0.5459(2) 0.0986(2) 0.0267(6) Uani 1 1 d . . . H17A H 0.9547 0.4765 0.0711 0.032 Uiso 1 1 calc R . . C18 C 1.0519(3) 0.5936(2) 0.1875(2) 0.0254(6) Uani 1 1 d . . . C19 C 1.0555(2) 0.69626(19) 0.22869(18) 0.0208(5) Uani 1 1 d . . . C20 C 0.9593(2) 0.74657(19) 0.17794(18) 0.0208(5) Uani 1 1 d . . . H20A H 0.9603 0.8157 0.2057 0.025 Uiso 1 1 calc R . . C21 C 1.1625(2) 0.74563(19) 0.32628(18) 0.0222(5) Uani 1 1 d . . . H21A H 1.2401 0.7168 0.3247 0.027 Uiso 1 1 calc R . . C22 C 1.1357(2) 0.71486(18) 0.41434(18) 0.0221(5) Uani 1 1 d . . . C23 C 1.1987(3) 0.64467(19) 0.4670(2) 0.0246(6) Uani 1 1 d . . . C24 C 1.1710(3) 0.6186(2) 0.5459(2) 0.0281(6) Uani 1 1 d . . . H24A H 1.2141 0.5701 0.5802 0.034 Uiso 1 1 calc R . . C25 C 1.0813(3) 0.66258(19) 0.57495(19) 0.0241(6) Uani 1 1 d . . . C26 C 1.0176(2) 0.73522(18) 0.52680(18) 0.0208(5) Uani 1 1 d . . . C27 C 1.0449(2) 0.75709(18) 0.44628(18) 0.0209(5) Uani 1 1 d . . . H27A H 0.9993 0.8036 0.4106 0.025 Uiso 1 1 calc R . . C28 C 0.9229(2) 0.78862(19) 0.56216(18) 0.0216(5) Uani 1 1 d . . . H28A H 0.9344 0.7729 0.6290 0.026 Uiso 1 1 calc R . . C29 C 0.5547(3) 0.91546(19) 0.2952(2) 0.0256(6) Uani 1 1 d . . . H29A H 0.5529 0.9444 0.3610 0.031 Uiso 1 1 calc R . . H29B H 0.6428 0.9314 0.2979 0.031 Uiso 1 1 calc R . . C30 C 0.4675(3) 0.9659(2) 0.2172(2) 0.0350(7) Uani 1 1 d . . . H30A H 0.4947 1.0401 0.2350 0.052 Uiso 1 1 calc R . . H30B H 0.3801 0.9504 0.2142 0.052 Uiso 1 1 calc R . . H30C H 0.4715 0.9395 0.1523 0.052 Uiso 1 1 calc R . . C31 C 0.7933(3) 0.8738(2) 0.0543(2) 0.0283(6) Uani 1 1 d . . . H31A H 0.8111 0.9034 0.1249 0.034 Uiso 1 1 calc R . . H31B H 0.8720 0.8890 0.0410 0.034 Uiso 1 1 calc R . . C32 C 0.6891(3) 0.9232(2) -0.0115(2) 0.0399(7) Uani 1 1 d . . . H32A H 0.7171 0.9971 0.0010 0.060 Uiso 1 1 calc R . . H32B H 0.6121 0.9106 0.0035 0.060 Uiso 1 1 calc R . . H32C H 0.6710 0.8938 -0.0813 0.060 Uiso 1 1 calc R . . C33 C 1.1946(3) 0.86212(19) 0.33985(19) 0.0245(6) Uani 1 1 d . . . H33A H 1.2090 0.8784 0.2805 0.029 Uiso 1 1 calc R . . H33B H 1.1213 0.8940 0.3451 0.029 Uiso 1 1 calc R . . C34 C 1.3118(3) 0.9077(2) 0.4318(2) 0.0309(6) Uani 1 1 d . . . H34A H 1.3284 0.9819 0.4373 0.046 Uiso 1 1 calc R . . H34B H 1.3850 0.8775 0.4263 0.046 Uiso 1 1 calc R . . H34C H 1.2973 0.8931 0.4909 0.046 Uiso 1 1 calc R . . C35 C 0.9502(2) 0.90523(19) 0.57673(19) 0.0247(6) Uani 1 1 d . . . H35A H 0.9470 0.9238 0.5132 0.030 Uiso 1 1 calc R . . H35B H 0.8833 0.9353 0.5953 0.030 Uiso 1 1 calc R . . C36 C 1.0791(3) 0.9506(2) 0.6564(2) 0.0336(7) Uani 1 1 d . . . H36A H 1.0925 1.0250 0.6624 0.050 Uiso 1 1 calc R . . H36B H 1.1458 0.9216 0.6381 0.050 Uiso 1 1 calc R . . H36C H 1.0819 0.9344 0.7201 0.050 Uiso 1 1 calc R . . O2S O 0.7755(4) 0.2673(5) 0.1696(3) 0.0697(15) Uani 0.768(10) 1 d PD A 1 H2S H 0.8181 0.3292 0.2225 0.105 Uiso 0.768(10) 1 d PR A 1 O2SB O 0.7949(12) 0.2108(16) 0.1728(11) 0.0697(15) Uani 0.232(10) 1 d PD A 2 H2SB H 0.8120 0.2757 0.1875 0.105 Uiso 0.232(10) 1 d PR A 2 C2S C 0.6747(4) 0.2012(4) 0.1779(3) 0.0684(12) Uani 1 1 d D . . H2S1 H 0.7042 0.1688 0.2357 0.103 Uiso 1 1 d R A . H2S2 H 0.6335 0.1483 0.1177 0.103 Uiso 1 1 d R . . H2S3 H 0.6138 0.2459 0.1860 0.103 Uiso 1 1 d R . . O1W O 0.3105(5) 0.5403(3) 0.7710(3) 0.0529(14) Uani 0.50 1 d P B 1 H1WA H 0.2447 0.4910 0.7207 0.079 Uiso 0.50 1 d PR B 1 H1WB H 0.2982 0.5739 0.8312 0.079 Uiso 0.50 1 d PR B 1 O2W O 0.2340(3) 0.4436(2) 0.7408(2) 0.0244(7) Uani 0.60 1 d P C 2 H2WA H 0.1871 0.3846 0.7209 0.037 Uiso 0.60 1 d PR C 2 H2WB H 0.2384 0.4618 0.6872 0.037 Uiso 0.60 1 d PR C 2 O3W O 0.3567(4) 0.4608(4) 0.8076(4) 0.0377(12) Uani 0.40 1 d P D 3 H3WA H 0.2776 0.4500 0.8113 0.057 Uiso 0.40 1 d PR D 3 H3WB H 0.3578 0.4866 0.7578 0.057 Uiso 0.40 1 d PR D 3 H1O H 0.7781 0.5524 0.5792 0.057 Uiso 1 1 d R . . H2O H 0.3918 0.6283 0.2613 0.057 Uiso 1 1 d R . . H3O H 0.2771 0.5990 0.0962 0.057 Uiso 1 1 d R . . H40 H 0.4751 0.5875 -0.1284 0.057 Uiso 1 1 d R . . H5O H 0.7085 0.5811 -0.0548 0.057 Uiso 1 1 d R . . H6O H 1.1315 0.4885 0.2179 0.057 Uiso 1 1 d R . . H7O H 1.3007 0.6072 0.4006 0.057 Uiso 1 1 d R . . H8O H 0.9979 0.6296 0.6510 0.057 Uiso 1 1 d R . . O1S O 0.9067(4) 0.1439(3) 0.0744(3) 0.0774(15) Uani 0.730(6) 1 d PD E 1 H1S H 0.8606 0.1854 0.1112 0.116 Uiso 0.730(6) 1 d PR E 1 C1S C 0.8702(9) 0.1865(6) -0.0246(5) 0.0669(19) Uani 0.730(6) 1 d PD E 1 H1S1 H 0.7861 0.2074 -0.0400 0.100 Uiso 0.730(6) 1 calc PR E 1 H1S2 H 0.8686 0.1330 -0.0790 0.100 Uiso 0.730(6) 1 calc PR E 1 H1S3 H 0.9330 0.2456 -0.0163 0.100 Uiso 0.730(6) 1 calc PR E 1 O9 O 1.150(2) 0.1801(10) 0.190(2) 0.094(2) Uani 0.603(3) 1 d PD F 1 H9O H 1.0556 0.1580 0.1431 0.141 Uiso 0.603(3) 1 d PR F 1 O10 O 1.1157(13) 0.3425(9) 0.1807(9) 0.0541(15) Uani 0.603(3) 1 d PD F 1 C41 C 1.1844(15) 0.2757(10) 0.2044(17) 0.0562(19) Uani 0.603(3) 1 d PD F 1 C42 C 1.3190(16) 0.3263(13) 0.265(2) 0.0710(13) Uani 0.603(3) 1 d PD F 1 H42A H 1.3369 0.3939 0.2563 0.085 Uiso 0.603(3) 1 calc PR F 1 C43 C 1.4210(6) 0.2954(5) 0.3311(5) 0.0544(14) Uani 0.603(3) 1 d PD F 1 H43A H 1.5003 0.3395 0.3600 0.065 Uiso 0.603(3) 1 calc PR F 1 Cl1 Cl 1.40570(18) 0.17569(13) 0.36159(13) 0.0651(6) Uani 0.603(3) 1 d PD F 1 O1SB O 0.884(2) 0.1612(11) -0.0083(13) 0.0774(15) Uani 0.270(6) 1 d PD E 2 H1SB H 0.8905 0.0990 -0.0471 0.116 Uiso 0.270(6) 1 d PR E 2 C1SB C 0.8974(16) 0.2738(11) 0.0564(11) 0.0669(19) Uani 0.270(6) 1 d PD E 2 H1S4 H 0.9825 0.2918 0.1080 0.100 Uiso 0.270(6) 1 calc PR E 2 H1S5 H 0.8337 0.2741 0.0874 0.100 Uiso 0.270(6) 1 calc PR E 2 H1S6 H 0.8846 0.3238 0.0129 0.100 Uiso 0.270(6) 1 calc PR E 2 O9B O 1.149(4) 0.1950(18) 0.186(3) 0.094(2) Uani 0.397(3) 1 d PD F 2 H9OB H 1.0608 0.1874 0.1455 0.141 Uiso 0.397(3) 1 d PR F 2 O10B O 1.094(2) 0.3349(15) 0.1625(15) 0.0541(15) Uani 0.397(3) 1 d PD F 2 C41B C 1.182(2) 0.2924(18) 0.210(3) 0.0562(19) Uani 0.397(3) 1 d PD F 2 C42B C 1.323(2) 0.324(2) 0.266(3) 0.0710(13) Uani 0.397(3) 1 d PD F 2 H42B H 1.3725 0.3892 0.2798 0.085 Uiso 0.397(3) 1 calc PR F 2 C43B C 1.3620(9) 0.2349(8) 0.2913(7) 0.0544(14) Uani 0.397(3) 1 d PD F 2 H43B H 1.3113 0.1693 0.2712 0.065 Uiso 0.397(3) 1 calc PR F 2 Cl1B Cl 1.5212(3) 0.2642(4) 0.3670(3) 0.127(2) Uani 0.397(3) 1 d PD F 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 O1 0.0305(10) 0.0261(9) 0.0252(9) 0.0104(8) 0.0082(8) 0.0070(8) O2 0.0209(10) 0.0276(10) 0.0317(10) 0.0078(8) 0.0031(8) -0.0026(8) O3 0.0237(10) 0.0294(10) 0.0277(10) -0.0031(8) 0.0077(8) -0.0049(8) O4 0.0316(11) 0.0409(11) 0.0180(9) -0.0037(8) 0.0058(8) -0.0086(9) O5 0.0303(10) 0.0294(10) 0.0236(9) -0.0070(8) 0.0061(8) -0.0037(8) O6 0.0301(11) 0.0213(9) 0.0425(12) -0.0010(8) 0.0069(9) 0.0072(8) O7 0.0406(12) 0.0312(10) 0.0449(12) 0.0148(9) 0.0281(10) 0.0151(9) O8 0.0351(11) 0.0366(11) 0.0289(10) 0.0135(8) 0.0174(9) 0.0130(9) C1 0.0212(13) 0.0213(12) 0.0183(12) -0.0001(10) 0.0077(10) 0.0055(10) C2 0.0277(14) 0.0234(13) 0.0198(12) 0.0052(10) 0.0117(11) 0.0090(11) C3 0.0223(13) 0.0230(13) 0.0255(13) 0.0051(10) 0.0113(11) 0.0017(11) C4 0.0189(13) 0.0236(13) 0.0243(13) 0.0016(10) 0.0085(11) 0.0024(10) C5 0.0217(13) 0.0188(12) 0.0201(12) 0.0002(10) 0.0083(10) 0.0055(10) C6 0.0234(13) 0.0176(12) 0.0186(12) 0.0007(9) 0.0079(10) 0.0030(10) C7 0.0195(13) 0.0191(12) 0.0235(13) 0.0030(10) 0.0052(10) 0.0031(10) C8 0.0243(13) 0.0173(12) 0.0197(12) 0.0037(10) 0.0027(11) 0.0033(10) C9 0.0228(13) 0.0249(13) 0.0243(13) 0.0057(11) 0.0060(11) 0.0020(11) C10 0.0261(14) 0.0268(14) 0.0203(13) -0.0005(11) 0.0023(11) -0.0046(11) C11 0.0321(15) 0.0276(14) 0.0172(12) 0.0033(10) 0.0061(11) -0.0001(12) C12 0.0243(14) 0.0230(13) 0.0183(12) 0.0059(10) 0.0022(11) 0.0006(11) C13 0.0230(13) 0.0178(12) 0.0188(12) 0.0042(10) 0.0010(10) 0.0015(10) C14 0.0274(14) 0.0264(14) 0.0161(12) 0.0044(10) 0.0049(11) -0.0004(11) C15 0.0252(13) 0.0231(13) 0.0197(12) 0.0030(10) 0.0111(11) -0.0016(11) C16 0.0264(14) 0.0271(14) 0.0183(12) -0.0032(10) 0.0093(11) -0.0051(11) C17 0.0278(14) 0.0218(13) 0.0287(14) -0.0040(11) 0.0128(12) 0.0006(11) C18 0.0246(14) 0.0231(13) 0.0287(14) 0.0019(11) 0.0116(11) 0.0027(11) C19 0.0223(13) 0.0209(12) 0.0196(12) 0.0013(10) 0.0102(10) 0.0000(10) C20 0.0251(13) 0.0189(12) 0.0179(12) 0.0010(10) 0.0098(11) -0.0016(10) C21 0.0223(13) 0.0208(13) 0.0225(13) 0.0029(10) 0.0073(11) 0.0038(10) C22 0.0237(13) 0.0184(12) 0.0216(13) 0.0016(10) 0.0067(11) 0.0013(10) C23 0.0264(14) 0.0205(13) 0.0288(14) 0.0032(11) 0.0128(12) 0.0058(11) C24 0.0313(15) 0.0256(14) 0.0302(14) 0.0103(11) 0.0114(12) 0.0093(12) C25 0.0273(14) 0.0234(13) 0.0212(13) 0.0043(10) 0.0085(11) 0.0029(11) C26 0.0208(13) 0.0178(12) 0.0188(12) -0.0012(10) 0.0039(10) 0.0006(10) C27 0.0193(13) 0.0186(12) 0.0199(12) 0.0023(10) 0.0020(10) 0.0023(10) C28 0.0241(13) 0.0213(13) 0.0172(12) 0.0023(10) 0.0049(10) 0.0056(10) C29 0.0259(14) 0.0208(13) 0.0264(13) 0.0025(10) 0.0056(11) 0.0046(11) C30 0.0347(16) 0.0242(14) 0.0399(17) 0.0099(12) 0.0039(14) 0.0073(12) C31 0.0288(15) 0.0274(14) 0.0261(14) 0.0090(11) 0.0064(12) 0.0001(12) C32 0.0419(18) 0.0333(16) 0.0397(17) 0.0165(13) 0.0057(14) 0.0033(14) C33 0.0254(14) 0.0222(13) 0.0230(13) 0.0037(10) 0.0066(11) 0.0004(11) C34 0.0286(15) 0.0274(14) 0.0302(15) 0.0014(12) 0.0065(12) -0.0028(12) C35 0.0229(13) 0.0226(13) 0.0237(13) 0.0001(10) 0.0040(11) 0.0043(11) C36 0.0321(16) 0.0253(14) 0.0310(15) -0.0028(12) 0.0007(13) 0.0012(12) O2S 0.061(2) 0.086(4) 0.0490(18) 0.015(2) 0.0091(16) -0.016(3) O2SB 0.061(2) 0.086(4) 0.0490(18) 0.015(2) 0.0091(16) -0.016(3) C2S 0.043(2) 0.084(3) 0.068(3) 0.017(2) 0.008(2) 0.001(2) O1W 0.077(3) 0.032(2) 0.0162(19) 0.0048(17) -0.016(2) -0.025(2) O2W 0.0300(17) 0.0228(15) 0.0198(14) 0.0053(12) 0.0090(13) -0.0011(13) O3W 0.025(3) 0.035(3) 0.041(3) -0.001(2) 0.002(2) 0.006(2) O1S 0.104(3) 0.062(2) 0.059(2) 0.0036(19) 0.036(2) -0.030(2) C1S 0.076(4) 0.076(5) 0.052(3) 0.019(3) 0.026(3) 0.001(4) O9 0.133(3) 0.038(4) 0.129(4) 0.025(4) 0.061(3) 0.035(4) O10 0.072(5) 0.030(2) 0.034(4) 0.001(2) -0.008(3) -0.001(2) C41 0.097(3) 0.031(5) 0.057(3) -0.002(4) 0.052(3) 0.015(3) C42 0.083(3) 0.099(3) 0.051(2) 0.019(2) 0.041(2) 0.040(3) C43 0.050(4) 0.062(4) 0.045(3) -0.007(2) 0.014(3) 0.020(3) Cl1 0.0826(13) 0.0554(10) 0.0661(11) 0.0108(8) 0.0328(9) 0.0340(9) O1SB 0.104(3) 0.062(2) 0.059(2) 0.0036(19) 0.036(2) -0.030(2) C1SB 0.076(4) 0.076(5) 0.052(3) 0.019(3) 0.026(3) 0.001(4) O9B 0.133(3) 0.038(4) 0.129(4) 0.025(4) 0.061(3) 0.035(4) O10B 0.072(5) 0.030(2) 0.034(4) 0.001(2) -0.008(3) -0.001(2) C41B 0.097(3) 0.031(5) 0.057(3) -0.002(4) 0.052(3) 0.015(3) C42B 0.083(3) 0.099(3) 0.051(2) 0.019(2) 0.041(2) 0.040(3) C43B 0.050(4) 0.062(4) 0.045(3) -0.007(2) 0.014(3) 0.020(3) Cl1B 0.058(2) 0.172(4) 0.102(3) -0.049(3) -0.0036(18) 0.037(2) _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 O1 C2 1.377(3) . ? O2 C4 1.378(3) . ? O3 C9 1.386(3) . ? O4 C11 1.380(3) . ? O5 C16 1.383(3) . ? O6 C18 1.362(3) . ? O7 C23 1.381(3) . ? O8 C25 1.388(3) . ? C1 C6 1.389(3) . ? C1 C2 1.396(4) . ? C1 C28 1.521(4) . ? C2 C3 1.385(4) . ? C3 C4 1.389(4) . ? C4 C5 1.393(4) . ? C5 C6 1.395(4) . ? C5 C7 1.526(3) . ? C7 C8 1.533(3) . ? C7 C29 1.541(3) . ? C8 C13 1.390(4) . ? C8 C9 1.395(4) . ? C9 C10 1.388(4) . ? C10 C11 1.384(4) . ? C11 C12 1.401(4) . ? C12 C13 1.393(4) . ? C12 C14 1.526(4) . ? C14 C15 1.524(4) . ? C14 C31 1.534(4) . ? C15 C20 1.399(4) . ? C15 C16 1.401(4) . ? C16 C17 1.381(4) . ? C17 C18 1.388(4) . ? C18 C19 1.405(4) . ? C19 C20 1.389(4) . ? C19 C21 1.523(3) . ? C21 C22 1.530(4) . ? C21 C33 1.536(3) . ? C22 C23 1.399(4) . ? C22 C27 1.400(4) . ? C23 C24 1.384(4) . ? C24 C25 1.378(4) . ? C25 C26 1.399(4) . ? C26 C27 1.385(4) . ? C26 C28 1.533(3) . ? C28 C35 1.532(3) . ? C29 C30 1.524(4) . ? C31 C32 1.524(4) . ? C33 C34 1.523(4) . ? C35 C36 1.521(4) . ? O2S C2S 1.436(6) . ? O2SB C2S 1.390(13) . ? O1S C1S 1.576(8) . ? O9 C41 1.268(14) . ? O10 C41 1.252(10) . ? C41 C42 1.509(11) . ? C42 C43 1.372(12) . ? C43 Cl1 1.741(7) . ? O1SB C1SB 1.615(16) . ? O9B C41B 1.28(2) . ? O10B C41B 1.249(14) . ? C41B C42B 1.508(14) . ? C42B C43B 1.369(17) . ? C43B Cl1B 1.734(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 117.0(2) . . ? C6 C1 C28 123.0(2) . . ? C2 C1 C28 120.0(2) . . ? O1 C2 C3 120.6(2) . . ? O1 C2 C1 118.1(2) . . ? C3 C2 C1 121.2(2) . . ? C2 C3 C4 119.7(2) . . ? O2 C4 C3 115.2(2) . . ? O2 C4 C5 123.4(2) . . ? C3 C4 C5 121.4(2) . . ? C4 C5 C6 116.8(2) . . ? C4 C5 C7 121.3(2) . . ? C6 C5 C7 122.0(2) . . ? C1 C6 C5 123.8(2) . . ? C5 C7 C8 110.74(19) . . ? C5 C7 C29 113.7(2) . . ? C8 C7 C29 111.5(2) . . ? C13 C8 C9 116.9(2) . . ? C13 C8 C7 121.7(2) . . ? C9 C8 C7 121.3(2) . . ? O3 C9 C10 121.2(2) . . ? O3 C9 C8 117.5(2) . . ? C10 C9 C8 121.3(2) . . ? C11 C10 C9 119.9(2) . . ? O4 C11 C10 121.5(2) . . ? O4 C11 C12 117.4(2) . . ? C10 C11 C12 121.2(2) . . ? C13 C12 C11 116.8(2) . . ? C13 C12 C14 121.7(2) . . ? C11 C12 C14 121.5(2) . . ? C8 C13 C12 123.9(2) . . ? C15 C14 C12 110.3(2) . . ? C15 C14 C31 114.3(2) . . ? C12 C14 C31 112.1(2) . . ? C20 C15 C16 116.1(2) . . ? C20 C15 C14 122.6(2) . . ? C16 C15 C14 121.2(2) . . ? C17 C16 O5 115.9(2) . . ? C17 C16 C15 122.0(2) . . ? O5 C16 C15 122.1(2) . . ? C16 C17 C18 120.0(2) . . ? O6 C18 C17 121.6(2) . . ? O6 C18 C19 117.9(2) . . ? C17 C18 C19 120.5(2) . . ? C20 C19 C18 117.5(2) . . ? C20 C19 C21 123.8(2) . . ? C18 C19 C21 118.7(2) . . ? C19 C20 C15 123.8(2) . . ? C19 C21 C22 110.9(2) . . ? C19 C21 C33 113.6(2) . . ? C22 C21 C33 112.0(2) . . ? C23 C22 C27 116.5(2) . . ? C23 C22 C21 122.9(2) . . ? C27 C22 C21 120.5(2) . . ? O7 C23 C24 115.2(2) . . ? O7 C23 C22 123.7(2) . . ? C24 C23 C22 121.1(2) . . ? C25 C24 C23 120.3(2) . . ? C24 C25 O8 116.9(2) . . ? C24 C25 C26 121.2(2) . . ? O8 C25 C26 121.9(2) . . ? C27 C26 C25 116.9(2) . . ? C27 C26 C28 121.7(2) . . ? C25 C26 C28 121.5(2) . . ? C26 C27 C22 124.0(2) . . ? C1 C28 C35 113.4(2) . . ? C1 C28 C26 110.79(19) . . ? C35 C28 C26 112.6(2) . . ? C30 C29 C7 112.4(2) . . ? C32 C31 C14 111.4(2) . . ? C34 C33 C21 112.5(2) . . ? C36 C35 C28 112.6(2) . . ? O2SB C2S O2S 33.3(7) . . ? O10 C41 O9 127.9(18) . . ? O10 C41 C42 109.7(12) . . ? O9 C41 C42 122.0(16) . . ? C43 C42 C41 133.7(13) . . ? C42 C43 Cl1 120.2(9) . . ? O10B C41B O9B 110(3) . . ? O10B C41B C42B 135(2) . . ? O9B C41B C42B 113(3) . . ? C43B C42B C41B 103.1(18) . . ? C42B C43B Cl1B 107.3(13) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.840 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.063 #=======================================END data_CECR-Z-HClA-2MeOH-1.5H2O@90k-2h _database_code_depnum_ccdc_archive 'CCDC 629577' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CECR-Z-HClA-2MeOH-1.5H2O@90k-2h _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C41 H54 Cl O13.50' _chemical_formula_weight 798.29 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3736(4) _cell_length_b 13.3966(4) _cell_length_c 14.6486(5) _cell_angle_alpha 98.9479(10) _cell_angle_beta 110.1919(10) _cell_angle_gamma 95.1444(10) _cell_volume 2044.42(12) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 675 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.9690 _exptl_absorpt_correction_T_max 0.9812 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14724 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7186 _reflns_number_gt 5561 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+2.2830P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7186 _refine_ls_number_parameters 550 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1800 _refine_ls_wR_factor_gt 0.1693 _refine_ls_goodness_of_fit_ref 1.209 _refine_ls_restrained_S_all 1.209 _refine_ls_shift/su_max 0.003 _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 O1 O 0.80101(19) 0.60517(15) 0.58036(14) 0.0283(5) Uani 1 1 d . . . O2 O 0.41913(18) 0.60518(15) 0.31355(15) 0.0297(5) Uani 1 1 d . . . O3 O 0.31813(19) 0.65147(15) 0.12965(15) 0.0300(5) Uani 1 1 d . . . O4 O 0.5432(2) 0.61371(17) -0.09604(14) 0.0344(5) Uani 1 1 d . . . O5 O 0.7720(2) 0.54576(16) -0.03858(15) 0.0328(5) Uani 1 1 d . . . O6 O 1.1443(2) 0.54316(15) 0.23714(16) 0.0348(5) Uani 1 1 d . . . O7 O 1.2909(2) 0.59676(16) 0.44524(16) 0.0353(5) Uani 1 1 d . . . O8 O 1.0589(2) 0.63276(16) 0.65489(15) 0.0321(5) Uani 1 1 d . . . C1 C 0.7867(3) 0.7438(2) 0.49517(19) 0.0209(6) Uani 1 1 d . . . C2 C 0.7310(3) 0.6514(2) 0.50620(19) 0.0227(6) Uani 1 1 d . . . C3 C 0.6087(3) 0.6076(2) 0.4449(2) 0.0243(6) Uani 1 1 d . . . H3A H 0.5719 0.5451 0.4539 0.029 Uiso 1 1 calc R . . C4 C 0.5397(3) 0.6550(2) 0.3700(2) 0.0234(6) Uani 1 1 d . . . C5 C 0.5907(3) 0.7474(2) 0.35612(19) 0.0207(6) Uani 1 1 d . . . C6 C 0.7141(3) 0.7887(2) 0.42002(19) 0.0211(6) Uani 1 1 d . . . H6A H 0.7507 0.8516 0.4115 0.025 Uiso 1 1 calc R . . C7 C 0.5159(3) 0.7986(2) 0.2735(2) 0.0226(6) Uani 1 1 d . . . H7A H 0.4251 0.7857 0.2671 0.027 Uiso 1 1 calc R . . C8 C 0.5219(3) 0.7489(2) 0.17388(19) 0.0227(6) Uani 1 1 d . . . C9 C 0.4222(3) 0.6772(2) 0.1048(2) 0.0252(6) Uani 1 1 d . . . C10 C 0.4275(3) 0.6321(2) 0.0143(2) 0.0287(7) Uani 1 1 d . . . H10A H 0.3585 0.5836 -0.0320 0.034 Uiso 1 1 calc R . . C11 C 0.5334(3) 0.6583(2) -0.0078(2) 0.0272(7) Uani 1 1 d . . . C12 C 0.6364(3) 0.7288(2) 0.0593(2) 0.0246(6) Uani 1 1 d . . . C13 C 0.6272(3) 0.7720(2) 0.14927(19) 0.0225(6) Uani 1 1 d . . . H13A H 0.6967 0.8197 0.1961 0.027 Uiso 1 1 calc R . . C14 C 0.7548(3) 0.7574(2) 0.0360(2) 0.0263(6) Uani 1 1 d . . . H14A H 0.7314 0.7315 -0.0368 0.032 Uiso 1 1 calc R . . C15 C 0.8609(3) 0.7015(2) 0.08838(19) 0.0233(6) Uani 1 1 d . . . C16 C 0.8626(3) 0.5993(2) 0.0499(2) 0.0265(6) Uani 1 1 d . . . C17 C 0.9556(3) 0.5459(2) 0.0984(2) 0.0279(7) Uani 1 1 d . . . H17A H 0.9541 0.4765 0.0708 0.033 Uiso 1 1 calc R . . C18 C 1.0510(3) 0.5934(2) 0.1870(2) 0.0263(6) Uani 1 1 d . . . C19 C 1.0551(3) 0.6960(2) 0.2283(2) 0.0217(6) Uani 1 1 d . . . C20 C 0.9588(3) 0.7464(2) 0.17751(19) 0.0214(6) Uani 1 1 d . . . H20A H 0.9599 0.8156 0.2053 0.026 Uiso 1 1 calc R . . C21 C 1.1615(3) 0.7454(2) 0.3260(2) 0.0223(6) Uani 1 1 d . . . H21A H 1.2390 0.7164 0.3245 0.027 Uiso 1 1 calc R . . C22 C 1.1347(3) 0.7145(2) 0.4139(2) 0.0227(6) Uani 1 1 d . . . C23 C 1.1978(3) 0.6446(2) 0.4664(2) 0.0263(6) Uani 1 1 d . . . C24 C 1.1703(3) 0.6185(2) 0.5456(2) 0.0284(7) Uani 1 1 d . . . H24A H 1.2135 0.5700 0.5799 0.034 Uiso 1 1 calc R . . C25 C 1.0807(3) 0.6624(2) 0.5747(2) 0.0251(6) Uani 1 1 d . . . C26 C 1.0173(3) 0.7350(2) 0.52684(19) 0.0217(6) Uani 1 1 d . . . C27 C 1.0445(3) 0.7568(2) 0.44586(19) 0.0215(6) Uani 1 1 d . . . H27A H 0.9989 0.8032 0.4101 0.026 Uiso 1 1 calc R . . C28 C 0.9225(3) 0.7887(2) 0.56230(19) 0.0221(6) Uani 1 1 d . . . H28A H 0.9340 0.7731 0.6291 0.027 Uiso 1 1 calc R . . C29 C 0.5550(3) 0.9155(2) 0.2955(2) 0.0265(6) Uani 1 1 d . . . H29A H 0.5537 0.9445 0.3615 0.032 Uiso 1 1 calc R . . H29B H 0.6428 0.9311 0.2979 0.032 Uiso 1 1 calc R . . C30 C 0.4677(3) 0.9660(2) 0.2178(2) 0.0358(8) Uani 1 1 d . . . H30A H 0.4949 1.0402 0.2356 0.054 Uiso 1 1 calc R . . H30B H 0.3805 0.9507 0.2151 0.054 Uiso 1 1 calc R . . H30C H 0.4714 0.9397 0.1528 0.054 Uiso 1 1 calc R . . C31 C 0.7931(3) 0.8739(2) 0.0542(2) 0.0296(7) Uani 1 1 d . . . H31A H 0.8114 0.9037 0.1248 0.036 Uiso 1 1 calc R . . H31B H 0.8715 0.8889 0.0405 0.036 Uiso 1 1 calc R . . C32 C 0.6886(3) 0.9236(3) -0.0114(3) 0.0420(8) Uani 1 1 d . . . H32A H 0.7166 0.9974 0.0011 0.063 Uiso 1 1 calc R . . H32B H 0.6118 0.9111 0.0039 0.063 Uiso 1 1 calc R . . H32C H 0.6702 0.8942 -0.0814 0.063 Uiso 1 1 calc R . . C33 C 1.1941(3) 0.8618(2) 0.3398(2) 0.0260(6) Uani 1 1 d . . . H33A H 1.2085 0.8779 0.2804 0.031 Uiso 1 1 calc R . . H33B H 1.1210 0.8939 0.3450 0.031 Uiso 1 1 calc R . . C34 C 1.3113(3) 0.9076(2) 0.4317(2) 0.0318(7) Uani 1 1 d . . . H34A H 1.3277 0.9818 0.4371 0.048 Uiso 1 1 calc R . . H34B H 1.3845 0.8774 0.4261 0.048 Uiso 1 1 calc R . . H34C H 1.2970 0.8931 0.4909 0.048 Uiso 1 1 calc R . . C35 C 0.9502(3) 0.9053(2) 0.5768(2) 0.0265(6) Uani 1 1 d . . . H35A H 0.9470 0.9236 0.5131 0.032 Uiso 1 1 calc R . . H35B H 0.8835 0.9357 0.5954 0.032 Uiso 1 1 calc R . . C36 C 1.0787(3) 0.9502(2) 0.6561(2) 0.0337(7) Uani 1 1 d . . . H36A H 1.0923 1.0246 0.6622 0.051 Uiso 1 1 calc R . . H36B H 1.1453 0.9211 0.6377 0.051 Uiso 1 1 calc R . . H36C H 1.0815 0.9341 0.7198 0.051 Uiso 1 1 calc R . . O2S O 0.7759(4) 0.2665(5) 0.1689(3) 0.0724(17) Uani 0.785(11) 1 d PD A 1 H2S H 0.8185 0.3283 0.2217 0.109 Uiso 0.785(11) 1 d PR A 1 O2SB O 0.7975(13) 0.2088(19) 0.1745(13) 0.0724(17) Uani 0.215(11) 1 d PD A 2 H2SB H 0.8147 0.2737 0.1892 0.109 Uiso 0.215(11) 1 d PR A 2 C2S C 0.6751(4) 0.2017(4) 0.1777(4) 0.0699(13) Uani 1 1 d D . . H2S1 H 0.7046 0.1693 0.2355 0.105 Uiso 1 1 d R A . H2S2 H 0.6339 0.1489 0.1175 0.105 Uiso 1 1 d R . . H2S3 H 0.6142 0.2464 0.1857 0.105 Uiso 1 1 d R . . O1W O 0.3099(6) 0.5403(4) 0.7709(3) 0.0581(16) Uani 0.50 1 d P B 1 H1WA H 0.2441 0.4910 0.7206 0.087 Uiso 0.50 1 d PR B 1 H1WB H 0.2976 0.5739 0.8311 0.087 Uiso 0.50 1 d PR B 1 O2W O 0.2340(3) 0.4439(2) 0.7409(2) 0.0258(7) Uani 0.60 1 d P C 2 H2WA H 0.1871 0.3849 0.7210 0.039 Uiso 0.60 1 d PR C 2 H2WB H 0.2384 0.4622 0.6872 0.039 Uiso 0.60 1 d PR C 2 O3W O 0.3565(5) 0.4609(4) 0.8071(4) 0.0365(13) Uani 0.40 1 d P D 3 H3WA H 0.2774 0.4502 0.8108 0.055 Uiso 0.40 1 d PR D 3 H3WB H 0.3576 0.4868 0.7573 0.055 Uiso 0.40 1 d PR D 3 H1O H 0.7779 0.5525 0.5787 0.055 Uiso 1 1 d R . . H2O H 0.3916 0.6284 0.2608 0.055 Uiso 1 1 d R . . H3O H 0.2769 0.5991 0.0958 0.055 Uiso 1 1 d R . . H40 H 0.4749 0.5876 -0.1288 0.055 Uiso 1 1 d R . . H5O H 0.7083 0.5812 -0.0553 0.055 Uiso 1 1 d R . . H6O H 1.1313 0.4886 0.2175 0.055 Uiso 1 1 d R . . H7O H 1.3005 0.6074 0.4002 0.055 Uiso 1 1 d R . . H8O H 0.9977 0.6297 0.6505 0.055 Uiso 1 1 d R . . O1S O 0.9053(5) 0.1440(3) 0.0736(3) 0.0807(16) Uani 0.754(6) 1 d PD E 1 H1S H 0.8592 0.1856 0.1105 0.121 Uiso 0.754(6) 1 d PR E 1 C1S C 0.8704(10) 0.1844(7) -0.0257(5) 0.072(2) Uani 0.754(6) 1 d PD E 1 H1S1 H 0.7865 0.2056 -0.0422 0.108 Uiso 0.754(6) 1 calc PR E 1 H1S2 H 0.8692 0.1299 -0.0792 0.108 Uiso 0.754(6) 1 calc PR E 1 H1S3 H 0.9336 0.2430 -0.0180 0.108 Uiso 0.754(6) 1 calc PR E 1 O9 O 1.145(3) 0.1763(11) 0.186(2) 0.096(2) Uani 0.557(3) 1 d PD F 1 H9O H 1.0505 0.1542 0.1388 0.145 Uiso 0.557(3) 1 d PR F 1 O10 O 1.1111(14) 0.3296(7) 0.1744(11) 0.0541(15) Uani 0.557(3) 1 d PD F 1 C41 C 1.1848(14) 0.2715(9) 0.2049(15) 0.0562(19) Uani 0.557(3) 1 d PD F 1 C42 C 1.3194(17) 0.3278(15) 0.266(2) 0.0769(17) Uani 0.557(3) 1 d PD F 1 H42A H 1.3348 0.3960 0.2576 0.092 Uiso 0.557(3) 1 calc PR F 1 C43 C 1.4203(8) 0.2963(6) 0.3302(5) 0.0589(17) Uani 0.557(3) 1 d PD F 1 H43A H 1.4999 0.3399 0.3586 0.071 Uiso 0.557(3) 1 calc PR F 1 Cl1 Cl 1.4048(2) 0.17561(15) 0.36113(15) 0.0680(7) Uani 0.557(3) 1 d PD F 1 O1SB O 0.884(2) 0.1631(13) -0.0059(15) 0.0807(16) Uani 0.246(6) 1 d PD E 2 H1SB H 0.8906 0.1009 -0.0447 0.121 Uiso 0.246(6) 1 d PR E 2 C1SB C 0.897(2) 0.2746(13) 0.0571(13) 0.072(2) Uani 0.246(6) 1 d PD E 2 H1S4 H 0.9824 0.2927 0.1088 0.108 Uiso 0.246(6) 1 calc PR E 2 H1S5 H 0.8337 0.2754 0.0882 0.108 Uiso 0.246(6) 1 calc PR E 2 H1S6 H 0.8848 0.3241 0.0133 0.108 Uiso 0.246(6) 1 calc PR E 2 O9B O 1.149(4) 0.1961(15) 0.188(3) 0.096(2) Uani 0.443(3) 1 d PD F 2 H9OB H 1.0603 0.1885 0.1470 0.145 Uiso 0.443(3) 1 d PR F 2 O10B O 1.0981(19) 0.3525(10) 0.1716(15) 0.0541(15) Uani 0.443(3) 1 d PD F 2 C41B C 1.175(2) 0.2959(14) 0.205(2) 0.0562(19) Uani 0.443(3) 1 d PD F 2 C42B C 1.318(2) 0.3206(19) 0.263(3) 0.0769(17) Uani 0.443(3) 1 d PD F 2 H42B H 1.3686 0.3857 0.2775 0.092 Uiso 0.443(3) 1 calc PR F 2 C43B C 1.3619(9) 0.2347(8) 0.2911(7) 0.0589(17) Uani 0.443(3) 1 d PD F 2 H43B H 1.3129 0.1686 0.2722 0.071 Uiso 0.443(3) 1 calc PR F 2 Cl1B Cl 1.5212(3) 0.2646(4) 0.3665(3) 0.1241(19) Uani 0.443(3) 1 d PD F 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 O1 0.0332(11) 0.0272(11) 0.0253(10) 0.0097(8) 0.0092(9) 0.0077(9) O2 0.0232(11) 0.0286(11) 0.0315(11) 0.0073(9) 0.0033(9) -0.0009(9) O3 0.0263(11) 0.0297(11) 0.0274(11) -0.0047(9) 0.0082(9) -0.0042(9) O4 0.0346(12) 0.0423(13) 0.0172(10) -0.0049(9) 0.0063(9) -0.0076(10) O5 0.0339(12) 0.0303(11) 0.0240(10) -0.0098(9) 0.0067(9) -0.0038(9) O6 0.0326(12) 0.0215(10) 0.0424(13) -0.0030(9) 0.0069(10) 0.0089(9) O7 0.0442(13) 0.0321(12) 0.0456(13) 0.0154(10) 0.0305(11) 0.0168(10) O8 0.0386(12) 0.0384(12) 0.0283(11) 0.0139(9) 0.0179(10) 0.0156(10) C1 0.0237(14) 0.0220(14) 0.0177(13) -0.0003(10) 0.0096(11) 0.0063(11) C2 0.0301(15) 0.0221(14) 0.0190(13) 0.0028(11) 0.0120(12) 0.0100(12) C3 0.0271(15) 0.0211(14) 0.0268(14) 0.0037(11) 0.0132(12) 0.0022(12) C4 0.0219(14) 0.0238(14) 0.0238(14) 0.0002(11) 0.0092(12) 0.0036(12) C5 0.0233(14) 0.0195(13) 0.0193(13) -0.0013(10) 0.0094(11) 0.0059(11) C6 0.0261(15) 0.0175(13) 0.0197(13) -0.0001(10) 0.0099(12) 0.0036(11) C7 0.0214(14) 0.0201(14) 0.0234(14) 0.0013(11) 0.0059(12) 0.0040(11) C8 0.0270(15) 0.0184(13) 0.0187(13) 0.0039(11) 0.0032(12) 0.0046(11) C9 0.0260(15) 0.0238(14) 0.0228(14) 0.0041(11) 0.0060(12) 0.0020(12) C10 0.0285(16) 0.0287(15) 0.0193(14) -0.0014(12) 0.0018(12) -0.0049(13) C11 0.0336(16) 0.0281(15) 0.0163(13) 0.0019(11) 0.0066(12) 0.0005(13) C12 0.0273(15) 0.0233(14) 0.0185(13) 0.0056(11) 0.0024(12) 0.0022(12) C13 0.0247(15) 0.0186(13) 0.0186(13) 0.0038(11) 0.0012(11) 0.0027(11) C14 0.0312(16) 0.0271(15) 0.0169(13) 0.0021(11) 0.0066(12) -0.0015(13) C15 0.0281(15) 0.0235(14) 0.0189(13) 0.0031(11) 0.0108(12) -0.0011(12) C16 0.0291(16) 0.0271(15) 0.0195(13) -0.0043(11) 0.0104(12) -0.0054(13) C17 0.0315(16) 0.0212(14) 0.0296(15) -0.0043(12) 0.0141(13) 0.0021(12) C18 0.0275(15) 0.0243(15) 0.0280(15) 0.0019(12) 0.0128(13) 0.0037(12) C19 0.0242(14) 0.0213(14) 0.0210(13) 0.0002(11) 0.0124(12) 0.0003(11) C20 0.0280(15) 0.0184(13) 0.0175(13) -0.0001(10) 0.0106(12) -0.0014(11) C21 0.0237(14) 0.0217(14) 0.0220(14) 0.0033(11) 0.0091(12) 0.0050(11) C22 0.0250(15) 0.0193(13) 0.0215(14) 0.0002(11) 0.0076(12) 0.0016(11) C23 0.0285(15) 0.0228(14) 0.0304(15) 0.0035(12) 0.0141(13) 0.0074(12) C24 0.0329(16) 0.0253(15) 0.0311(15) 0.0101(12) 0.0130(13) 0.0111(13) C25 0.0303(16) 0.0231(14) 0.0218(14) 0.0030(11) 0.0103(12) 0.0036(12) C26 0.0231(14) 0.0200(13) 0.0183(13) -0.0012(11) 0.0054(11) 0.0021(11) C27 0.0222(14) 0.0184(13) 0.0190(13) 0.0005(10) 0.0028(11) 0.0032(11) C28 0.0260(15) 0.0219(14) 0.0163(13) 0.0012(11) 0.0057(11) 0.0058(12) C29 0.0292(16) 0.0199(14) 0.0270(15) 0.0018(11) 0.0069(13) 0.0053(12) C30 0.0369(18) 0.0252(16) 0.0402(18) 0.0098(13) 0.0056(15) 0.0081(14) C31 0.0331(17) 0.0275(15) 0.0242(14) 0.0070(12) 0.0061(13) -0.0008(13) C32 0.047(2) 0.0341(18) 0.0401(19) 0.0143(15) 0.0070(16) 0.0047(16) C33 0.0279(15) 0.0235(15) 0.0241(14) 0.0026(11) 0.0078(12) 0.0020(12) C34 0.0324(17) 0.0278(16) 0.0286(16) 0.0007(12) 0.0070(14) -0.0028(13) C35 0.0274(15) 0.0217(14) 0.0243(14) -0.0028(11) 0.0048(12) 0.0053(12) C36 0.0332(17) 0.0243(15) 0.0316(16) -0.0038(13) 0.0012(14) 0.0036(13) O2S 0.064(2) 0.091(4) 0.0489(19) 0.014(3) 0.0104(18) -0.013(3) O2SB 0.064(2) 0.091(4) 0.0489(19) 0.014(3) 0.0104(18) -0.013(3) C2S 0.045(2) 0.089(3) 0.067(3) 0.019(3) 0.010(2) 0.004(2) O1W 0.087(4) 0.034(3) 0.018(2) 0.0058(19) -0.016(2) -0.027(3) O2W 0.0321(19) 0.0236(17) 0.0210(16) 0.0055(13) 0.0093(14) 0.0000(14) O3W 0.025(3) 0.035(3) 0.039(3) -0.003(2) 0.002(2) 0.006(2) O1S 0.116(4) 0.063(3) 0.059(3) 0.003(2) 0.040(3) -0.030(2) C1S 0.081(4) 0.088(5) 0.050(4) 0.021(3) 0.028(4) 0.001(4) O9 0.151(4) 0.032(5) 0.128(3) 0.022(5) 0.070(3) 0.037(5) O10 0.072(5) 0.030(2) 0.034(4) 0.001(2) -0.008(3) -0.001(2) C41 0.097(3) 0.031(5) 0.057(3) -0.002(4) 0.052(3) 0.015(3) C42 0.091(4) 0.115(5) 0.048(3) 0.020(3) 0.044(3) 0.051(3) C43 0.057(4) 0.065(4) 0.045(4) -0.011(3) 0.012(3) 0.025(3) Cl1 0.0888(16) 0.0569(12) 0.0669(13) 0.0088(9) 0.0344(11) 0.0355(11) O1SB 0.116(4) 0.063(3) 0.059(3) 0.003(2) 0.040(3) -0.030(2) C1SB 0.081(4) 0.088(5) 0.050(4) 0.021(3) 0.028(4) 0.001(4) O9B 0.151(4) 0.032(5) 0.128(3) 0.022(5) 0.070(3) 0.037(5) O10B 0.072(5) 0.030(2) 0.034(4) 0.001(2) -0.008(3) -0.001(2) C41B 0.097(3) 0.031(5) 0.057(3) -0.002(4) 0.052(3) 0.015(3) C42B 0.091(4) 0.115(5) 0.048(3) 0.020(3) 0.044(3) 0.051(3) C43B 0.057(4) 0.065(4) 0.045(4) -0.011(3) 0.012(3) 0.025(3) Cl1B 0.061(2) 0.165(4) 0.099(3) -0.046(2) -0.0028(18) 0.035(2) _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 O1 C2 1.377(3) . ? O2 C4 1.375(3) . ? O3 C9 1.384(4) . ? O4 C11 1.382(3) . ? O5 C16 1.383(3) . ? O6 C18 1.366(4) . ? O7 C23 1.384(3) . ? O8 C25 1.388(3) . ? C1 C6 1.387(4) . ? C1 C2 1.399(4) . ? C1 C28 1.521(4) . ? C2 C3 1.383(4) . ? C3 C4 1.391(4) . ? C4 C5 1.393(4) . ? C5 C6 1.395(4) . ? C5 C7 1.521(4) . ? C7 C8 1.533(4) . ? C7 C29 1.540(4) . ? C8 C13 1.388(4) . ? C8 C9 1.394(4) . ? C9 C10 1.392(4) . ? C10 C11 1.381(4) . ? C11 C12 1.396(4) . ? C12 C13 1.397(4) . ? C12 C14 1.531(4) . ? C14 C15 1.519(4) . ? C14 C31 1.538(4) . ? C15 C20 1.392(4) . ? C15 C16 1.401(4) . ? C16 C17 1.382(4) . ? C17 C18 1.384(4) . ? C18 C19 1.402(4) . ? C19 C20 1.391(4) . ? C19 C21 1.523(4) . ? C21 C22 1.528(4) . ? C21 C33 1.535(4) . ? C22 C27 1.394(4) . ? C22 C23 1.395(4) . ? C23 C24 1.387(4) . ? C24 C25 1.377(4) . ? C25 C26 1.396(4) . ? C26 C27 1.390(4) . ? C26 C28 1.536(4) . ? C28 C35 1.531(4) . ? C29 C30 1.523(4) . ? C31 C32 1.527(4) . ? C33 C34 1.525(4) . ? C35 C36 1.517(4) . ? O2S C2S 1.429(6) . ? O2SB C2S 1.405(14) . ? O1S C1S 1.566(8) . ? O9 C41 1.267(15) . ? O10 C41 1.214(10) . ? C41 C42 1.534(12) . ? C42 C43 1.358(12) . ? C43 Cl1 1.755(8) . ? O1SB C1SB 1.592(17) . ? O9B C41B 1.309(19) . ? O10B C41B 1.228(12) . ? C41B C42B 1.535(14) . ? C42B C43B 1.359(16) . ? C43B Cl1B 1.736(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 117.0(2) . . ? C6 C1 C28 123.2(2) . . ? C2 C1 C28 119.8(2) . . ? O1 C2 C3 120.8(2) . . ? O1 C2 C1 118.1(2) . . ? C3 C2 C1 121.1(3) . . ? C2 C3 C4 120.0(3) . . ? O2 C4 C3 115.2(2) . . ? O2 C4 C5 123.6(2) . . ? C3 C4 C5 121.2(3) . . ? C4 C5 C6 116.7(2) . . ? C4 C5 C7 121.2(2) . . ? C6 C5 C7 122.1(2) . . ? C1 C6 C5 124.1(3) . . ? C5 C7 C8 110.8(2) . . ? C5 C7 C29 113.6(2) . . ? C8 C7 C29 111.4(2) . . ? C13 C8 C9 117.2(3) . . ? C13 C8 C7 121.6(2) . . ? C9 C8 C7 121.2(3) . . ? O3 C9 C10 121.0(2) . . ? O3 C9 C8 117.7(2) . . ? C10 C9 C8 121.2(3) . . ? C11 C10 C9 119.7(3) . . ? C10 C11 O4 121.4(3) . . ? C10 C11 C12 121.3(3) . . ? O4 C11 C12 117.3(3) . . ? C11 C12 C13 117.1(3) . . ? C11 C12 C14 121.7(2) . . ? C13 C12 C14 121.2(2) . . ? C8 C13 C12 123.5(3) . . ? C15 C14 C12 110.7(2) . . ? C15 C14 C31 114.3(2) . . ? C12 C14 C31 112.0(2) . . ? C20 C15 C16 116.3(3) . . ? C20 C15 C14 122.8(2) . . ? C16 C15 C14 120.9(2) . . ? C17 C16 O5 115.9(2) . . ? C17 C16 C15 121.8(3) . . ? O5 C16 C15 122.3(3) . . ? C16 C17 C18 120.0(3) . . ? O6 C18 C17 121.7(3) . . ? O6 C18 C19 117.6(2) . . ? C17 C18 C19 120.7(3) . . ? C20 C19 C18 117.3(2) . . ? C20 C19 C21 123.7(2) . . ? C18 C19 C21 119.0(2) . . ? C19 C20 C15 123.9(3) . . ? C19 C21 C22 111.1(2) . . ? C19 C21 C33 113.7(2) . . ? C22 C21 C33 112.2(2) . . ? C27 C22 C23 116.6(3) . . ? C27 C22 C21 120.5(2) . . ? C23 C22 C21 122.9(2) . . ? O7 C23 C24 115.0(3) . . ? O7 C23 C22 123.9(3) . . ? C24 C23 C22 121.1(3) . . ? C25 C24 C23 120.3(3) . . ? C24 C25 O8 116.9(2) . . ? C24 C25 C26 121.1(3) . . ? O8 C25 C26 121.9(2) . . ? C27 C26 C25 116.8(3) . . ? C27 C26 C28 121.6(2) . . ? C25 C26 C28 121.5(2) . . ? C26 C27 C22 124.0(3) . . ? C1 C28 C35 113.3(2) . . ? C1 C28 C26 110.9(2) . . ? C35 C28 C26 112.4(2) . . ? C30 C29 C7 112.4(2) . . ? C32 C31 C14 111.6(2) . . ? C34 C33 C21 112.7(2) . . ? C36 C35 C28 112.5(2) . . ? O2SB C2S O2S 34.4(9) . . ? O10 C41 O9 119.8(18) . . ? O10 C41 C42 112.3(12) . . ? O9 C41 C42 127.9(17) . . ? C43 C42 C41 130.7(15) . . ? C42 C43 Cl1 120.5(11) . . ? O10B C41B O9B 125(2) . . ? O10B C41B C42B 130.2(18) . . ? O9B C41B C42B 105(2) . . ? C43B C42B C41B 109.3(17) . . ? C42B C43B Cl1B 109.5(12) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.941 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.066 #=======================================END data_CECR-Z-HClA-2MeOH-1.5H2O@90k-4h _database_code_depnum_ccdc_archive 'CCDC 629578' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CECR-Z-HClA-2MeOH-1.5H2O@90k-4h _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C41 H54 Cl O13.50' _chemical_formula_weight 798.29 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3794(4) _cell_length_b 13.3976(5) _cell_length_c 14.6461(5) _cell_angle_alpha 99.0222(10) _cell_angle_beta 110.2090(10) _cell_angle_gamma 95.0382(11) _cell_volume 2045.08(13) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 675 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.9690 _exptl_absorpt_correction_T_max 0.9812 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14949 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7180 _reflns_number_gt 5458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+2.2830P] 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 7180 _refine_ls_number_parameters 550 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0874 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1825 _refine_ls_wR_factor_gt 0.1704 _refine_ls_goodness_of_fit_ref 1.217 _refine_ls_restrained_S_all 1.216 _refine_ls_shift/su_max 0.078 _refine_ls_shift/su_mean 0.001 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 O1 O 0.80156(19) 0.60583(15) 0.58077(15) 0.0296(5) Uani 1 1 d . . . O2 O 0.41931(19) 0.60561(15) 0.31438(15) 0.0306(5) Uani 1 1 d . . . O3 O 0.31814(19) 0.65156(15) 0.13010(15) 0.0313(5) Uani 1 1 d . . . O4 O 0.5422(2) 0.61414(17) -0.09602(15) 0.0372(5) Uani 1 1 d . . . O5 O 0.7711(2) 0.54582(16) -0.03894(15) 0.0343(5) Uani 1 1 d . . . O6 O 1.1431(2) 0.54283(15) 0.23678(17) 0.0368(5) Uani 1 1 d . . . O7 O 1.2906(2) 0.59612(16) 0.44534(17) 0.0367(5) Uani 1 1 d . . . O8 O 1.0597(2) 0.63291(16) 0.65520(15) 0.0330(5) Uani 1 1 d . . . C1 C 0.7869(3) 0.7439(2) 0.49536(19) 0.0225(6) Uani 1 1 d . . . C2 C 0.7315(3) 0.6513(2) 0.5067(2) 0.0242(6) Uani 1 1 d . . . C3 C 0.6091(3) 0.6079(2) 0.4456(2) 0.0259(6) Uani 1 1 d . . . H3A H 0.5722 0.5456 0.4547 0.031 Uiso 1 1 calc R . . C4 C 0.5400(3) 0.6553(2) 0.3707(2) 0.0239(6) Uani 1 1 d . . . C5 C 0.5905(3) 0.7473(2) 0.35679(19) 0.0221(6) Uani 1 1 d . . . C6 C 0.7146(3) 0.7887(2) 0.42060(19) 0.0217(6) Uani 1 1 d . . . H6A H 0.7512 0.8513 0.4119 0.026 Uiso 1 1 calc R . . C7 C 0.5160(3) 0.7988(2) 0.2742(2) 0.0231(6) Uani 1 1 d . . . H7A H 0.4253 0.7858 0.2678 0.028 Uiso 1 1 calc R . . C8 C 0.5214(3) 0.7490(2) 0.1743(2) 0.0236(6) Uani 1 1 d . . . C9 C 0.4220(3) 0.6775(2) 0.1052(2) 0.0262(6) Uani 1 1 d . . . C10 C 0.4265(3) 0.6326(2) 0.0147(2) 0.0299(7) Uani 1 1 d . . . H10A H 0.3574 0.5844 -0.0317 0.036 Uiso 1 1 calc R . . C11 C 0.5327(3) 0.6587(2) -0.0076(2) 0.0289(7) Uani 1 1 d . . . C12 C 0.6357(3) 0.7291(2) 0.0593(2) 0.0252(6) Uani 1 1 d . . . C13 C 0.6266(3) 0.7720(2) 0.1493(2) 0.0234(6) Uani 1 1 d . . . H13A H 0.6961 0.8196 0.1962 0.028 Uiso 1 1 calc R . . C14 C 0.7536(3) 0.7578(2) 0.0358(2) 0.0282(7) Uani 1 1 d . . . H14A H 0.7300 0.7321 -0.0371 0.034 Uiso 1 1 calc R . . C15 C 0.8598(3) 0.7013(2) 0.0880(2) 0.0249(6) Uani 1 1 d . . . C16 C 0.8616(3) 0.5991(2) 0.0496(2) 0.0276(7) Uani 1 1 d . . . C17 C 0.9543(3) 0.5457(2) 0.0978(2) 0.0296(7) Uani 1 1 d . . . H17A H 0.9526 0.4763 0.0702 0.035 Uiso 1 1 calc R . . C18 C 1.0501(3) 0.5931(2) 0.1866(2) 0.0283(7) Uani 1 1 d . . . C19 C 1.0540(3) 0.6958(2) 0.2279(2) 0.0232(6) Uani 1 1 d . . . C20 C 0.9579(3) 0.7463(2) 0.17737(19) 0.0229(6) Uani 1 1 d . . . H20A H 0.9590 0.8155 0.2053 0.027 Uiso 1 1 calc R . . C21 C 1.1609(3) 0.7446(2) 0.3255(2) 0.0237(6) Uani 1 1 d . . . H21A H 1.2382 0.7155 0.3236 0.028 Uiso 1 1 calc R . . C22 C 1.1343(3) 0.7139(2) 0.4137(2) 0.0233(6) Uani 1 1 d . . . C23 C 1.1975(3) 0.6439(2) 0.4661(2) 0.0275(6) Uani 1 1 d . . . C24 C 1.1703(3) 0.6181(2) 0.5457(2) 0.0300(7) Uani 1 1 d . . . H24A H 1.2135 0.5697 0.5801 0.036 Uiso 1 1 calc R . . C25 C 1.0810(3) 0.6624(2) 0.5748(2) 0.0268(6) Uani 1 1 d . . . C26 C 1.0173(3) 0.7345(2) 0.5268(2) 0.0230(6) Uani 1 1 d . . . C27 C 1.0441(3) 0.7563(2) 0.44576(19) 0.0221(6) Uani 1 1 d . . . H27A H 0.9983 0.8028 0.4101 0.027 Uiso 1 1 calc R . . C28 C 0.9228(3) 0.7886(2) 0.5622(2) 0.0230(6) Uani 1 1 d . . . H28A H 0.9344 0.7733 0.6292 0.028 Uiso 1 1 calc R . . C29 C 0.5540(3) 0.9157(2) 0.2962(2) 0.0280(7) Uani 1 1 d . . . H29A H 0.5524 0.9446 0.3622 0.034 Uiso 1 1 calc R . . H29B H 0.6419 0.9317 0.2989 0.034 Uiso 1 1 calc R . . C30 C 0.4671(3) 0.9663(2) 0.2189(3) 0.0381(8) Uani 1 1 d . . . H30A H 0.4945 1.0405 0.2368 0.057 Uiso 1 1 calc R . . H30B H 0.3800 0.9512 0.2162 0.057 Uiso 1 1 calc R . . H30C H 0.4708 0.9400 0.1538 0.057 Uiso 1 1 calc R . . C31 C 0.7918(3) 0.8741(2) 0.0545(2) 0.0316(7) Uani 1 1 d . . . H31A H 0.8100 0.9037 0.1251 0.038 Uiso 1 1 calc R . . H31B H 0.8700 0.8892 0.0407 0.038 Uiso 1 1 calc R . . C32 C 0.6873(3) 0.9235(3) -0.0109(3) 0.0425(8) Uani 1 1 d . . . H32A H 0.7152 0.9974 0.0016 0.064 Uiso 1 1 calc R . . H32B H 0.6108 0.9111 0.0046 0.064 Uiso 1 1 calc R . . H32C H 0.6687 0.8940 -0.0809 0.064 Uiso 1 1 calc R . . C33 C 1.1931(3) 0.8611(2) 0.3393(2) 0.0268(6) Uani 1 1 d . . . H33A H 1.2074 0.8773 0.2800 0.032 Uiso 1 1 calc R . . H33B H 1.1200 0.8932 0.3449 0.032 Uiso 1 1 calc R . . C34 C 1.3106(3) 0.9065(2) 0.4315(2) 0.0335(7) Uani 1 1 d . . . H34A H 1.3273 0.9807 0.4371 0.050 Uiso 1 1 calc R . . H34B H 1.3836 0.8760 0.4258 0.050 Uiso 1 1 calc R . . H34C H 1.2962 0.8920 0.4907 0.050 Uiso 1 1 calc R . . C35 C 0.9507(3) 0.9054(2) 0.5767(2) 0.0269(6) Uani 1 1 d . . . H35A H 0.9473 0.9237 0.5130 0.032 Uiso 1 1 calc R . . H35B H 0.8843 0.9360 0.5956 0.032 Uiso 1 1 calc R . . C36 C 1.0794(3) 0.9501(2) 0.6559(2) 0.0355(8) Uani 1 1 d . . . H36A H 1.0931 1.0245 0.6621 0.053 Uiso 1 1 calc R . . H36B H 1.1457 0.9207 0.6372 0.053 Uiso 1 1 calc R . . H36C H 1.0825 0.9340 0.7196 0.053 Uiso 1 1 calc R . . O2S O 0.7771(4) 0.2638(6) 0.1670(3) 0.0775(18) Uani 0.790(11) 1 d PD A 1 H2S H 0.8198 0.3257 0.2199 0.116 Uiso 0.790(11) 1 d PR A 1 O2SB O 0.7990(14) 0.204(2) 0.1769(14) 0.0775(18) Uani 0.210(11) 1 d PD A 2 H2SB H 0.8162 0.2691 0.1916 0.116 Uiso 0.210(11) 1 d PR A 2 C2S C 0.6753(4) 0.2025(4) 0.1782(4) 0.0749(14) Uani 1 1 d D . . H2S1 H 0.7048 0.1701 0.2359 0.112 Uiso 1 1 d R A . H2S2 H 0.6341 0.1496 0.1179 0.112 Uiso 1 1 d R . . H2S3 H 0.6145 0.2472 0.1862 0.112 Uiso 1 1 d R . . O1W O 0.3075(7) 0.5401(4) 0.7707(4) 0.077(2) Uani 0.50 1 d P B 1 H1WA H 0.2417 0.4908 0.7205 0.116 Uiso 0.50 1 d PR B 1 H1WB H 0.2951 0.5737 0.8310 0.116 Uiso 0.50 1 d PR B 1 O2W O 0.2346(3) 0.4438(2) 0.7413(2) 0.0271(7) Uani 0.60 1 d P C 2 H2WA H 0.1877 0.3848 0.7214 0.041 Uiso 0.60 1 d PR C 2 H2WB H 0.2391 0.4621 0.6877 0.041 Uiso 0.60 1 d PR C 2 O3W O 0.3566(4) 0.4606(4) 0.8080(4) 0.0317(12) Uani 0.40 1 d P D 3 H3WA H 0.2775 0.4498 0.8117 0.048 Uiso 0.40 1 d PR D 3 H3WB H 0.3577 0.4864 0.7582 0.048 Uiso 0.40 1 d PR D 3 H1O H 0.7780 0.5522 0.5796 0.048 Uiso 1 1 d R . . H2O H 0.3917 0.6281 0.2617 0.048 Uiso 1 1 d R . . H3O H 0.2770 0.5988 0.0966 0.048 Uiso 1 1 d R . . H40 H 0.4750 0.5873 -0.1280 0.048 Uiso 1 1 d R . . H5O H 0.7084 0.5809 -0.0544 0.048 Uiso 1 1 d R . . H6O H 1.1314 0.4883 0.2183 0.048 Uiso 1 1 d R . . H7O H 1.3006 0.6070 0.4010 0.048 Uiso 1 1 d R . . H8O H 0.9978 0.6294 0.6514 0.048 Uiso 1 1 d R . . O1S O 0.9046(5) 0.1430(3) 0.0715(3) 0.0838(16) Uani 0.783(7) 1 d PD E 1 H1S H 0.8585 0.1845 0.1083 0.126 Uiso 0.783(7) 1 d PR E 1 C1S C 0.8700(10) 0.1821(7) -0.0266(5) 0.079(3) Uani 0.783(7) 1 d PD E 1 H1S1 H 0.7861 0.2034 -0.0431 0.119 Uiso 0.783(7) 1 calc PR E 1 H1S2 H 0.8688 0.1273 -0.0799 0.119 Uiso 0.783(7) 1 calc PR E 1 H1S3 H 0.9331 0.2406 -0.0191 0.119 Uiso 0.783(7) 1 calc PR E 1 O9 O 1.144(3) 0.1771(15) 0.186(3) 0.101(2) Uani 0.511(3) 1 d PD F 1 H9O H 1.0495 0.1550 0.1388 0.152 Uiso 0.511(3) 1 d PR F 1 O10 O 1.109(2) 0.3355(15) 0.1745(18) 0.0623(13) Uani 0.511(3) 1 d PD F 1 C41 C 1.180(2) 0.2748(14) 0.202(3) 0.0593(18) Uani 0.511(3) 1 d PD F 1 C42 C 1.315(2) 0.3239(19) 0.263(3) 0.0842(17) Uani 0.511(3) 1 d PD F 1 H42A H 1.3329 0.3909 0.2528 0.101 Uiso 0.511(3) 1 calc PR F 1 C43 C 1.4192(9) 0.2962(7) 0.3303(6) 0.0630(19) Uani 0.511(3) 1 d PD F 1 H43A H 1.4976 0.3413 0.3595 0.076 Uiso 0.511(3) 1 calc PR F 1 Cl1 Cl 1.4032(2) 0.17533(17) 0.36034(18) 0.0710(8) Uani 0.511(3) 1 d PD F 1 O1SB O 0.886(3) 0.1630(16) -0.0054(18) 0.0838(16) Uani 0.217(7) 1 d PD E 2 H1SB H 0.8931 0.1008 -0.0442 0.126 Uiso 0.217(7) 1 d PR E 2 C1SB C 0.899(2) 0.2720(16) 0.0548(15) 0.079(3) Uani 0.217(7) 1 d PD E 2 H1S4 H 0.9837 0.2907 0.1066 0.119 Uiso 0.217(7) 1 calc PR E 2 H1S5 H 0.8350 0.2734 0.0857 0.119 Uiso 0.217(7) 1 calc PR E 2 H1S6 H 0.8862 0.3209 0.0103 0.119 Uiso 0.217(7) 1 calc PR E 2 O9B O 1.143(4) 0.1911(16) 0.181(3) 0.101(2) Uani 0.489(3) 1 d PD F 2 H9OB H 1.0550 0.1835 0.1404 0.152 Uiso 0.489(3) 1 d PR F 2 O10B O 1.099(2) 0.3430(16) 0.171(2) 0.0623(13) Uani 0.489(3) 1 d PD F 2 C41B C 1.177(2) 0.2893(16) 0.204(3) 0.0593(18) Uani 0.489(3) 1 d PD F 2 C42B C 1.317(2) 0.321(2) 0.263(3) 0.0842(17) Uani 0.489(3) 1 d PD F 2 H42B H 1.3647 0.3871 0.2783 0.101 Uiso 0.489(3) 1 calc PR F 2 C43B C 1.3629(8) 0.2342(8) 0.2912(6) 0.0630(19) Uani 0.489(3) 1 d PD F 2 H43B H 1.3146 0.1677 0.2719 0.076 Uiso 0.489(3) 1 calc PR F 2 Cl1B Cl 1.5211(3) 0.2647(3) 0.3665(2) 0.1167(16) Uani 0.489(3) 1 d PD F 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 O1 0.0343(12) 0.0286(11) 0.0279(10) 0.0108(9) 0.0104(9) 0.0089(9) O2 0.0239(11) 0.0313(11) 0.0327(11) 0.0085(9) 0.0053(9) 0.0010(9) O3 0.0267(11) 0.0310(11) 0.0296(11) -0.0043(9) 0.0085(9) -0.0034(9) O4 0.0371(12) 0.0457(13) 0.0198(10) -0.0051(9) 0.0080(9) -0.0087(10) O5 0.0331(12) 0.0327(12) 0.0276(11) -0.0098(9) 0.0082(9) -0.0027(9) O6 0.0344(12) 0.0222(11) 0.0471(13) -0.0030(9) 0.0097(10) 0.0099(9) O7 0.0453(13) 0.0351(12) 0.0469(13) 0.0172(10) 0.0310(11) 0.0201(10) O8 0.0381(12) 0.0403(12) 0.0302(11) 0.0148(9) 0.0184(10) 0.0165(10) C1 0.0256(14) 0.0236(14) 0.0185(13) -0.0020(11) 0.0100(12) 0.0080(12) C2 0.0311(16) 0.0254(14) 0.0195(13) 0.0037(11) 0.0122(12) 0.0100(12) C3 0.0290(16) 0.0239(14) 0.0286(15) 0.0051(12) 0.0152(13) 0.0045(12) C4 0.0223(14) 0.0254(15) 0.0239(14) 0.0000(11) 0.0101(12) 0.0045(12) C5 0.0239(14) 0.0224(14) 0.0200(13) -0.0017(11) 0.0097(12) 0.0071(12) C6 0.0264(15) 0.0187(13) 0.0212(13) 0.0006(10) 0.0112(12) 0.0055(11) C7 0.0225(14) 0.0212(14) 0.0240(14) 0.0014(11) 0.0070(12) 0.0063(11) C8 0.0276(15) 0.0199(14) 0.0204(13) 0.0052(11) 0.0041(12) 0.0058(12) C9 0.0252(15) 0.0250(15) 0.0252(14) 0.0049(12) 0.0058(12) 0.0021(12) C10 0.0296(16) 0.0310(16) 0.0205(14) -0.0012(12) 0.0030(12) -0.0030(13) C11 0.0339(17) 0.0312(16) 0.0178(13) 0.0020(12) 0.0069(13) 0.0007(13) C12 0.0282(15) 0.0241(14) 0.0197(13) 0.0056(11) 0.0040(12) 0.0034(12) C13 0.0252(15) 0.0201(14) 0.0201(13) 0.0045(11) 0.0022(12) 0.0034(12) C14 0.0333(16) 0.0296(16) 0.0183(13) 0.0036(12) 0.0073(12) -0.0014(13) C15 0.0291(15) 0.0262(15) 0.0202(13) 0.0031(11) 0.0119(12) -0.0013(12) C16 0.0300(16) 0.0283(15) 0.0202(14) -0.0058(12) 0.0108(12) -0.0059(13) C17 0.0319(16) 0.0234(15) 0.0316(16) -0.0050(12) 0.0143(13) 0.0019(13) C18 0.0287(16) 0.0254(15) 0.0312(16) 0.0010(12) 0.0135(13) 0.0042(13) C19 0.0263(15) 0.0223(14) 0.0222(13) 0.0004(11) 0.0125(12) 0.0018(12) C20 0.0307(15) 0.0195(14) 0.0184(13) 0.0000(11) 0.0115(12) 0.0001(12) C21 0.0231(14) 0.0224(14) 0.0249(14) 0.0023(11) 0.0090(12) 0.0045(12) C22 0.0257(15) 0.0202(14) 0.0220(14) 0.0000(11) 0.0084(12) 0.0017(12) C23 0.0298(16) 0.0249(15) 0.0312(15) 0.0035(12) 0.0154(13) 0.0086(13) C24 0.0349(17) 0.0281(15) 0.0327(16) 0.0113(13) 0.0150(14) 0.0132(13) C25 0.0319(16) 0.0264(15) 0.0224(14) 0.0039(12) 0.0102(12) 0.0066(13) C26 0.0240(14) 0.0216(14) 0.0195(13) -0.0011(11) 0.0058(11) 0.0027(12) C27 0.0229(14) 0.0185(13) 0.0202(13) 0.0001(10) 0.0036(11) 0.0034(11) C28 0.0267(15) 0.0236(14) 0.0178(13) 0.0007(11) 0.0075(12) 0.0078(12) C29 0.0284(16) 0.0229(15) 0.0285(15) 0.0010(12) 0.0066(13) 0.0053(12) C30 0.0384(19) 0.0263(16) 0.0438(19) 0.0087(14) 0.0061(15) 0.0090(14) C31 0.0337(17) 0.0303(16) 0.0275(15) 0.0085(12) 0.0073(13) -0.0004(13) C32 0.048(2) 0.0359(18) 0.0402(19) 0.0154(15) 0.0081(16) 0.0061(16) C33 0.0302(16) 0.0235(15) 0.0263(15) 0.0034(12) 0.0104(13) 0.0043(12) C34 0.0335(17) 0.0293(16) 0.0310(16) 0.0005(13) 0.0072(14) -0.0008(14) C35 0.0275(15) 0.0232(14) 0.0254(14) -0.0009(12) 0.0057(12) 0.0074(12) C36 0.0342(18) 0.0281(16) 0.0318(16) -0.0037(13) 0.0012(14) 0.0033(14) O2S 0.063(2) 0.110(5) 0.048(2) 0.017(3) 0.0124(18) -0.013(3) O2SB 0.063(2) 0.110(5) 0.048(2) 0.017(3) 0.0124(18) -0.013(3) C2S 0.045(2) 0.100(4) 0.070(3) 0.018(3) 0.011(2) 0.003(3) O1W 0.117(5) 0.046(3) 0.024(2) 0.011(2) -0.019(3) -0.034(3) O2W 0.0342(19) 0.0248(17) 0.0216(16) 0.0039(13) 0.0108(15) 0.0001(15) O3W 0.023(3) 0.030(3) 0.032(3) -0.003(2) 0.002(2) 0.008(2) O1S 0.120(4) 0.065(3) 0.064(3) 0.002(2) 0.044(3) -0.028(2) C1S 0.083(5) 0.104(6) 0.053(4) 0.019(3) 0.030(4) 0.001(4) O9 0.161(4) 0.045(4) 0.126(4) 0.028(4) 0.075(3) 0.045(4) O10 0.090(3) 0.034(2) 0.051(2) 0.0074(18) 0.010(2) 0.013(2) C41 0.100(4) 0.037(5) 0.058(3) 0.005(4) 0.049(3) 0.024(3) C42 0.098(4) 0.131(5) 0.052(3) 0.027(3) 0.049(3) 0.062(4) C43 0.060(5) 0.075(5) 0.046(4) -0.007(3) 0.013(3) 0.029(4) Cl1 0.0883(18) 0.0628(14) 0.0696(14) 0.0093(11) 0.0339(13) 0.0373(12) O1SB 0.120(4) 0.065(3) 0.064(3) 0.002(2) 0.044(3) -0.028(2) C1SB 0.083(5) 0.104(6) 0.053(4) 0.019(3) 0.030(4) 0.001(4) O9B 0.161(4) 0.045(4) 0.126(4) 0.028(4) 0.075(3) 0.045(4) O10B 0.090(3) 0.034(2) 0.051(2) 0.0074(18) 0.010(2) 0.013(2) C41B 0.100(4) 0.037(5) 0.058(3) 0.005(4) 0.049(3) 0.024(3) C42B 0.098(4) 0.131(5) 0.052(3) 0.027(3) 0.049(3) 0.062(4) C43B 0.060(5) 0.075(5) 0.046(4) -0.007(3) 0.013(3) 0.029(4) Cl1B 0.0603(18) 0.154(3) 0.095(2) -0.041(2) 0.0016(15) 0.0339(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.370(3) . ? O2 C4 1.376(3) . ? O3 C9 1.384(4) . ? O4 C11 1.382(4) . ? O5 C16 1.382(3) . ? O6 C18 1.363(4) . ? O7 C23 1.381(4) . ? O8 C25 1.388(3) . ? C1 C6 1.380(4) . ? C1 C2 1.401(4) . ? C1 C28 1.522(4) . ? C2 C3 1.383(4) . ? C3 C4 1.392(4) . ? C4 C5 1.387(4) . ? C5 C6 1.402(4) . ? C5 C7 1.521(4) . ? C7 C8 1.534(4) . ? C7 C29 1.540(4) . ? C8 C13 1.390(4) . ? C8 C9 1.392(4) . ? C9 C10 1.386(4) . ? C10 C11 1.387(4) . ? C11 C12 1.395(4) . ? C12 C13 1.395(4) . ? C12 C14 1.529(4) . ? C14 C15 1.523(4) . ? C14 C31 1.535(4) . ? C15 C20 1.396(4) . ? C15 C16 1.401(4) . ? C16 C17 1.378(4) . ? C17 C18 1.386(4) . ? C18 C19 1.404(4) . ? C19 C20 1.389(4) . ? C19 C21 1.522(4) . ? C21 C22 1.531(4) . ? C21 C33 1.536(4) . ? C22 C23 1.395(4) . ? C22 C27 1.397(4) . ? C23 C24 1.391(4) . ? C24 C25 1.376(4) . ? C25 C26 1.392(4) . ? C26 C27 1.389(4) . ? C26 C28 1.535(4) . ? C28 C35 1.534(4) . ? C29 C30 1.518(4) . ? C31 C32 1.523(4) . ? C33 C34 1.527(4) . ? C35 C36 1.518(4) . ? O2S C2S 1.431(6) . ? O2SB C2S 1.412(14) . ? O1S C1S 1.541(9) . ? O9 C41 1.295(18) . ? O10 C41 1.212(11) . ? C41 C42 1.518(13) . ? C42 C43 1.373(14) . ? C43 Cl1 1.754(9) . ? O1SB C1SB 1.550(19) . ? O9B C41B 1.294(19) . ? O10B C41B 1.211(12) . ? C41B C42B 1.517(13) . ? C42B C43B 1.373(16) . ? C43B Cl1B 1.728(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 117.2(3) . . ? C6 C1 C28 123.2(3) . . ? C2 C1 C28 119.6(2) . . ? O1 C2 C3 121.1(3) . . ? O1 C2 C1 118.1(2) . . ? C3 C2 C1 120.8(3) . . ? C2 C3 C4 120.0(3) . . ? O2 C4 C5 123.5(2) . . ? O2 C4 C3 115.2(2) . . ? C5 C4 C3 121.3(3) . . ? C4 C5 C6 116.7(3) . . ? C4 C5 C7 121.5(2) . . ? C6 C5 C7 121.7(2) . . ? C1 C6 C5 123.9(3) . . ? C5 C7 C8 110.9(2) . . ? C5 C7 C29 114.0(2) . . ? C8 C7 C29 111.5(2) . . ? C13 C8 C9 117.0(3) . . ? C13 C8 C7 121.6(2) . . ? C9 C8 C7 121.4(3) . . ? O3 C9 C10 120.8(3) . . ? O3 C9 C8 117.7(3) . . ? C10 C9 C8 121.5(3) . . ? C9 C10 C11 119.5(3) . . ? O4 C11 C10 121.4(3) . . ? O4 C11 C12 117.2(3) . . ? C10 C11 C12 121.4(3) . . ? C11 C12 C13 116.8(3) . . ? C11 C12 C14 121.8(3) . . ? C13 C12 C14 121.3(2) . . ? C8 C13 C12 123.7(3) . . ? C15 C14 C12 110.5(2) . . ? C15 C14 C31 114.4(2) . . ? C12 C14 C31 112.1(3) . . ? C20 C15 C16 116.2(3) . . ? C20 C15 C14 122.6(3) . . ? C16 C15 C14 121.2(2) . . ? C17 C16 O5 115.9(3) . . ? C17 C16 C15 121.9(3) . . ? O5 C16 C15 122.2(3) . . ? C16 C17 C18 120.2(3) . . ? O6 C18 C17 121.9(3) . . ? O6 C18 C19 117.6(3) . . ? C17 C18 C19 120.4(3) . . ? C20 C19 C18 117.5(3) . . ? C20 C19 C21 124.0(2) . . ? C18 C19 C21 118.6(3) . . ? C19 C20 C15 123.8(3) . . ? C19 C21 C22 111.1(2) . . ? C19 C21 C33 113.5(2) . . ? C22 C21 C33 112.0(2) . . ? C23 C22 C27 116.7(3) . . ? C23 C22 C21 122.9(3) . . ? C27 C22 C21 120.4(2) . . ? O7 C23 C24 114.8(3) . . ? O7 C23 C22 124.2(3) . . ? C24 C23 C22 121.0(3) . . ? C25 C24 C23 120.1(3) . . ? C24 C25 O8 116.6(3) . . ? C24 C25 C26 121.3(3) . . ? O8 C25 C26 122.0(3) . . ? C27 C26 C25 117.0(3) . . ? C27 C26 C28 121.3(2) . . ? C25 C26 C28 121.7(2) . . ? C26 C27 C22 123.8(3) . . ? C1 C28 C35 113.4(2) . . ? C1 C28 C26 110.9(2) . . ? C35 C28 C26 112.5(2) . . ? C30 C29 C7 112.7(2) . . ? C32 C31 C14 111.4(3) . . ? C34 C33 C21 112.5(2) . . ? C36 C35 C28 112.5(2) . . ? O2SB C2S O2S 35.8(9) . . ? O10 C41 O9 124(2) . . ? O10 C41 C42 113.9(18) . . ? O9 C41 C42 122(2) . . ? C43 C42 C41 136(2) . . ? C42 C43 Cl1 118.1(13) . . ? O10B C41B O9B 119(3) . . ? O10B C41B C42B 128(2) . . ? O9B C41B C42B 113(3) . . ? C43B C42B C41B 106.4(18) . . ? C42B C43B Cl1B 109.6(12) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.979 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.071 #=======================================END data_CECR-Z-HClA-2MeOH-1.5H2O@90k-8h _database_code_depnum_ccdc_archive 'CCDC 629579' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CECR-Z-HClA-2MeOH-1.5H2O@90k-8h _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C41 H54 Cl O13.50' _chemical_formula_weight 798.29 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3833(4) _cell_length_b 13.4042(5) _cell_length_c 14.6333(5) _cell_angle_alpha 99.0088(11) _cell_angle_beta 110.2459(11) _cell_angle_gamma 94.9955(11) _cell_volume 2044.83(13) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 675 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.9690 _exptl_absorpt_correction_T_max 0.9812 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15027 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7182 _reflns_number_gt 5254 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+2.2830P] 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 7182 _refine_ls_number_parameters 550 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1814 _refine_ls_wR_factor_gt 0.1675 _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_restrained_S_all 1.196 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.001 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 O1 O 0.8024(2) 0.60572(15) 0.58113(15) 0.0301(5) Uani 1 1 d . . . O2 O 0.41936(19) 0.60558(16) 0.31466(15) 0.0304(5) Uani 1 1 d . . . O3 O 0.31763(19) 0.65173(16) 0.13031(15) 0.0313(5) Uani 1 1 d . . . O4 O 0.5411(2) 0.61445(17) -0.09654(15) 0.0364(6) Uani 1 1 d . . . O5 O 0.7703(2) 0.54607(16) -0.03906(15) 0.0350(5) Uani 1 1 d . . . O6 O 1.1430(2) 0.54307(16) 0.23671(17) 0.0364(6) Uani 1 1 d . . . O7 O 1.2908(2) 0.59609(16) 0.44549(17) 0.0361(5) Uani 1 1 d . . . O8 O 1.0608(2) 0.63299(17) 0.65587(15) 0.0337(5) Uani 1 1 d . . . C1 C 0.7869(3) 0.7437(2) 0.4958(2) 0.0228(6) Uani 1 1 d . . . C2 C 0.7319(3) 0.6515(2) 0.5071(2) 0.0244(6) Uani 1 1 d . . . C3 C 0.6096(3) 0.6077(2) 0.4458(2) 0.0262(7) Uani 1 1 d . . . H3A H 0.5731 0.5453 0.4548 0.031 Uiso 1 1 calc R . . C4 C 0.5402(3) 0.6552(2) 0.3712(2) 0.0239(6) Uani 1 1 d . . . C5 C 0.5904(3) 0.7471(2) 0.3571(2) 0.0227(6) Uani 1 1 d . . . C6 C 0.7147(3) 0.7886(2) 0.4209(2) 0.0223(6) Uani 1 1 d . . . H6A H 0.7513 0.8511 0.4121 0.027 Uiso 1 1 calc R . . C7 C 0.5159(3) 0.7989(2) 0.2745(2) 0.0235(6) Uani 1 1 d . . . H7A H 0.4252 0.7860 0.2681 0.028 Uiso 1 1 calc R . . C8 C 0.5211(3) 0.7493(2) 0.1744(2) 0.0235(6) Uani 1 1 d . . . C9 C 0.4215(3) 0.6775(2) 0.1053(2) 0.0263(7) Uani 1 1 d . . . C10 C 0.4262(3) 0.6331(2) 0.0146(2) 0.0303(7) Uani 1 1 d . . . H10A H 0.3569 0.5850 -0.0320 0.036 Uiso 1 1 calc R . . C11 C 0.5320(3) 0.6590(2) -0.0079(2) 0.0276(7) Uani 1 1 d . . . C12 C 0.6348(3) 0.7292(2) 0.0592(2) 0.0254(7) Uani 1 1 d . . . C13 C 0.6259(3) 0.7720(2) 0.1492(2) 0.0241(6) Uani 1 1 d . . . H13A H 0.6955 0.8195 0.1961 0.029 Uiso 1 1 calc R . . C14 C 0.7530(3) 0.7579(2) 0.0356(2) 0.0277(7) Uani 1 1 d . . . H14A H 0.7293 0.7322 -0.0374 0.033 Uiso 1 1 calc R . . C15 C 0.8591(3) 0.7012(2) 0.0880(2) 0.0246(6) Uani 1 1 d . . . C16 C 0.8610(3) 0.5993(2) 0.0494(2) 0.0272(7) Uani 1 1 d . . . C17 C 0.9538(3) 0.5458(2) 0.0979(2) 0.0297(7) Uani 1 1 d . . . H17A H 0.9519 0.4764 0.0703 0.036 Uiso 1 1 calc R . . C18 C 1.0500(3) 0.5932(2) 0.1865(2) 0.0284(7) Uani 1 1 d . . . C19 C 1.0538(3) 0.6957(2) 0.2277(2) 0.0234(6) Uani 1 1 d . . . C20 C 0.9573(3) 0.7465(2) 0.1770(2) 0.0230(6) Uani 1 1 d . . . H20A H 0.9585 0.8157 0.2047 0.028 Uiso 1 1 calc R . . C21 C 1.1603(3) 0.7447(2) 0.3253(2) 0.0239(6) Uani 1 1 d . . . H21A H 1.2377 0.7157 0.3236 0.029 Uiso 1 1 calc R . . C22 C 1.1341(3) 0.7142(2) 0.4136(2) 0.0237(6) Uani 1 1 d . . . C23 C 1.1981(3) 0.6442(2) 0.4665(2) 0.0272(7) Uani 1 1 d . . . C24 C 1.1707(3) 0.6182(2) 0.5457(2) 0.0305(7) Uani 1 1 d . . . H24A H 1.2136 0.5696 0.5799 0.037 Uiso 1 1 calc R . . C25 C 1.0815(3) 0.6625(2) 0.5752(2) 0.0271(7) Uani 1 1 d . . . C26 C 1.0176(3) 0.7347(2) 0.5272(2) 0.0226(6) Uani 1 1 d . . . C27 C 1.0441(3) 0.7562(2) 0.4460(2) 0.0219(6) Uani 1 1 d . . . H27A H 0.9980 0.8024 0.4101 0.026 Uiso 1 1 calc R . . C28 C 0.9229(3) 0.7886(2) 0.5628(2) 0.0240(6) Uani 1 1 d . . . H28A H 0.9347 0.7733 0.6298 0.029 Uiso 1 1 calc R . . C29 C 0.5539(3) 0.9156(2) 0.2964(2) 0.0276(7) Uani 1 1 d . . . H29A H 0.5529 0.9444 0.3627 0.033 Uiso 1 1 calc R . . H29B H 0.6416 0.9314 0.2987 0.033 Uiso 1 1 calc R . . C30 C 0.4667(3) 0.9665(2) 0.2194(3) 0.0384(8) Uani 1 1 d . . . H30A H 0.4942 1.0405 0.2374 0.058 Uiso 1 1 calc R . . H30B H 0.3797 0.9515 0.2170 0.058 Uiso 1 1 calc R . . H30C H 0.4697 0.9402 0.1540 0.058 Uiso 1 1 calc R . . C31 C 0.7908(3) 0.8739(2) 0.0540(2) 0.0311(7) Uani 1 1 d . . . H31A H 0.8092 0.9036 0.1248 0.037 Uiso 1 1 calc R . . H31B H 0.8689 0.8890 0.0401 0.037 Uiso 1 1 calc R . . C32 C 0.6861(4) 0.9233(3) -0.0113(3) 0.0423(9) Uani 1 1 d . . . H32A H 0.7139 0.9971 0.0011 0.064 Uiso 1 1 calc R . . H32B H 0.6098 0.9109 0.0044 0.064 Uiso 1 1 calc R . . H32C H 0.6673 0.8938 -0.0814 0.064 Uiso 1 1 calc R . . C33 C 1.1927(3) 0.8612(2) 0.3397(2) 0.0263(7) Uani 1 1 d . . . H33A H 1.2069 0.8777 0.2803 0.032 Uiso 1 1 calc R . . H33B H 1.1198 0.8933 0.3454 0.032 Uiso 1 1 calc R . . C34 C 1.3097(3) 0.9064(2) 0.4315(2) 0.0335(7) Uani 1 1 d . . . H34A H 1.3264 0.9805 0.4371 0.050 Uiso 1 1 calc R . . H34B H 1.3827 0.8758 0.4258 0.050 Uiso 1 1 calc R . . H34C H 1.2955 0.8919 0.4908 0.050 Uiso 1 1 calc R . . C35 C 0.9506(3) 0.9050(2) 0.5770(2) 0.0274(7) Uani 1 1 d . . . H35A H 0.9466 0.9231 0.5131 0.033 Uiso 1 1 calc R . . H35B H 0.8843 0.9356 0.5961 0.033 Uiso 1 1 calc R . . C36 C 1.0795(3) 0.9500(2) 0.6559(2) 0.0358(8) Uani 1 1 d . . . H36A H 1.0929 1.0244 0.6619 0.054 Uiso 1 1 calc R . . H36B H 1.1457 0.9208 0.6370 0.054 Uiso 1 1 calc R . . H36C H 1.0832 0.9341 0.7199 0.054 Uiso 1 1 calc R . . O2S O 0.7789(5) 0.2606(6) 0.1654(3) 0.0769(19) Uani 0.796(13) 1 d PD A 1 H2S H 0.8215 0.3225 0.2183 0.115 Uiso 0.796(13) 1 d PR A 1 O2SB O 0.7987(14) 0.204(2) 0.1754(15) 0.0769(19) Uani 0.204(13) 1 d PD A 2 H2SB H 0.8159 0.2685 0.1901 0.115 Uiso 0.204(13) 1 d PR A 2 C2S C 0.6751(4) 0.2021(4) 0.1781(4) 0.0766(15) Uani 1 1 d D . . H2S1 H 0.7046 0.1697 0.2358 0.115 Uiso 1 1 d R A . H2S2 H 0.6339 0.1492 0.1178 0.115 Uiso 1 1 d R . . H2S3 H 0.6142 0.2468 0.1861 0.115 Uiso 1 1 d R . . O1W O 0.3026(8) 0.5407(4) 0.7710(4) 0.065(2) Uani 0.40 1 d P B 1 H1WA H 0.2368 0.4913 0.7207 0.098 Uiso 0.40 1 d PR B 1 H1WB H 0.2902 0.5743 0.8312 0.098 Uiso 0.40 1 d PR B 1 O2W O 0.2338(3) 0.4438(2) 0.7411(2) 0.0271(8) Uani 0.60 1 d P C 2 H2WA H 0.1869 0.3848 0.7212 0.041 Uiso 0.60 1 d PR C 2 H2WB H 0.2382 0.4621 0.6875 0.041 Uiso 0.60 1 d PR C 2 O3W O 0.3568(4) 0.4609(3) 0.8079(3) 0.0392(11) Uani 0.50 1 d P D 3 H3WA H 0.2777 0.4501 0.8116 0.059 Uiso 0.50 1 d PR D 3 H3WB H 0.3579 0.4867 0.7582 0.059 Uiso 0.50 1 d PR D 3 H1O H 0.7782 0.5525 0.5796 0.059 Uiso 1 1 d R . . H2O H 0.3918 0.6284 0.2617 0.059 Uiso 1 1 d R . . H3O H 0.2772 0.5991 0.0966 0.059 Uiso 1 1 d R . . H40 H 0.4751 0.5876 -0.1280 0.059 Uiso 1 1 d R . . H5O H 0.7085 0.5812 -0.0545 0.059 Uiso 1 1 d R . . H6O H 1.1315 0.4886 0.2183 0.059 Uiso 1 1 d R . . H7O H 1.3007 0.6073 0.4010 0.059 Uiso 1 1 d R . . H8O H 0.9979 0.6297 0.6514 0.059 Uiso 1 1 d R . . O1S O 0.9057(4) 0.1423(3) 0.0712(3) 0.0798(15) Uani 0.842(7) 1 d PD E 1 H1S H 0.8596 0.1838 0.1080 0.120 Uiso 0.842(7) 1 d PR E 1 C1S C 0.8798(9) 0.1751(10) -0.0219(7) 0.092(3) Uani 0.842(7) 1 d PD E 1 H1S1 H 0.7964 0.1975 -0.0424 0.138 Uiso 0.842(7) 1 calc PR E 1 H1S2 H 0.8804 0.1182 -0.0727 0.138 Uiso 0.842(7) 1 calc PR E 1 H1S3 H 0.9449 0.2321 -0.0142 0.138 Uiso 0.842(7) 1 calc PR E 1 O9 O 1.147(3) 0.1783(16) 0.186(3) 0.091(2) Uani 0.495(3) 1 d PD F 1 H9O H 1.0519 0.1562 0.1382 0.137 Uiso 0.495(3) 1 d PR F 1 O10 O 1.107(2) 0.3387(16) 0.1748(19) 0.0590(11) Uani 0.495(3) 1 d PD F 1 C41 C 1.178(2) 0.2774(16) 0.201(3) 0.0571(15) Uani 0.495(3) 1 d PD F 1 C42 C 1.312(2) 0.324(2) 0.263(3) 0.0808(17) Uani 0.495(3) 1 d PD F 1 H42A H 1.3303 0.3910 0.2524 0.097 Uiso 0.495(3) 1 calc PR F 1 C43 C 1.4171(9) 0.2971(7) 0.3291(6) 0.0634(19) Uani 0.495(3) 1 d PD F 1 H43A H 1.4953 0.3422 0.3581 0.076 Uiso 0.495(3) 1 calc PR F 1 Cl1 Cl 1.4011(2) 0.17530(18) 0.35894(17) 0.0669(8) Uani 0.495(3) 1 d PD F 1 O1SB O 0.853(4) 0.176(3) -0.021(3) 0.0798(15) Uani 0.158(7) 1 d PD E 2 H1SB H 0.8603 0.1139 -0.0602 0.120 Uiso 0.158(7) 1 d PR E 2 C1SB C 0.900(3) 0.271(3) 0.051(2) 0.092(3) Uani 0.158(7) 1 d PD E 2 H1S4 H 0.9873 0.2709 0.0942 0.138 Uiso 0.158(7) 1 calc PR E 2 H1S5 H 0.8466 0.2781 0.0915 0.138 Uiso 0.158(7) 1 calc PR E 2 H1S6 H 0.8960 0.3285 0.0167 0.138 Uiso 0.158(7) 1 calc PR E 2 O9B O 1.138(3) 0.1890(15) 0.178(3) 0.091(2) Uani 0.505(3) 1 d PD F 2 H9OB H 1.0500 0.1814 0.1372 0.137 Uiso 0.505(3) 1 d PR F 2 O10B O 1.098(2) 0.3409(16) 0.1704(19) 0.0590(11) Uani 0.505(3) 1 d PD F 2 C41B C 1.177(2) 0.2873(16) 0.203(3) 0.0571(15) Uani 0.505(3) 1 d PD F 2 C42B C 1.315(2) 0.319(2) 0.262(3) 0.0808(17) Uani 0.505(3) 1 d PD F 2 H42B H 1.3611 0.3863 0.2772 0.097 Uiso 0.505(3) 1 calc PR F 2 C43B C 1.3628(8) 0.2343(8) 0.2906(6) 0.0634(19) Uani 0.505(3) 1 d PD F 2 H43B H 1.3153 0.1676 0.2714 0.076 Uiso 0.505(3) 1 calc PR F 2 Cl1B Cl 1.5211(3) 0.2640(3) 0.3664(2) 0.1106(14) Uani 0.505(3) 1 d PD F 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 O1 0.0336(12) 0.0299(11) 0.0280(11) 0.0113(9) 0.0095(9) 0.0084(10) O2 0.0238(11) 0.0310(11) 0.0319(11) 0.0072(9) 0.0052(9) 0.0006(9) O3 0.0258(11) 0.0321(12) 0.0292(11) -0.0038(9) 0.0079(9) -0.0037(9) O4 0.0365(13) 0.0440(13) 0.0197(10) -0.0044(9) 0.0075(10) -0.0087(11) O5 0.0335(12) 0.0344(12) 0.0273(11) -0.0088(9) 0.0075(10) -0.0026(10) O6 0.0318(12) 0.0235(11) 0.0460(13) -0.0022(10) 0.0070(11) 0.0093(10) O7 0.0441(13) 0.0348(12) 0.0457(13) 0.0177(10) 0.0295(11) 0.0188(11) O8 0.0380(13) 0.0419(13) 0.0306(11) 0.0159(10) 0.0177(10) 0.0177(10) C1 0.0246(15) 0.0246(15) 0.0206(14) 0.0000(11) 0.0111(12) 0.0075(12) C2 0.0292(16) 0.0275(15) 0.0199(14) 0.0041(12) 0.0119(13) 0.0112(13) C3 0.0303(16) 0.0247(15) 0.0269(15) 0.0044(12) 0.0147(13) 0.0038(13) C4 0.0228(15) 0.0253(15) 0.0231(14) 0.0004(12) 0.0097(12) 0.0042(12) C5 0.0238(15) 0.0231(15) 0.0211(14) -0.0009(11) 0.0097(12) 0.0075(12) C6 0.0258(15) 0.0202(14) 0.0210(14) 0.0013(11) 0.0094(12) 0.0048(12) C7 0.0215(15) 0.0218(15) 0.0235(14) 0.0006(11) 0.0053(12) 0.0040(12) C8 0.0253(15) 0.0215(14) 0.0203(14) 0.0059(11) 0.0029(12) 0.0059(12) C9 0.0250(16) 0.0252(15) 0.0264(15) 0.0057(12) 0.0065(13) 0.0024(13) C10 0.0301(17) 0.0320(17) 0.0193(14) -0.0007(12) 0.0017(13) -0.0035(14) C11 0.0320(17) 0.0301(16) 0.0169(14) 0.0031(12) 0.0060(13) 0.0004(13) C12 0.0277(16) 0.0246(15) 0.0199(14) 0.0062(12) 0.0034(12) 0.0027(13) C13 0.0258(16) 0.0203(14) 0.0203(14) 0.0043(11) 0.0012(12) 0.0027(12) C14 0.0310(17) 0.0298(16) 0.0180(14) 0.0031(12) 0.0056(13) -0.0012(13) C15 0.0272(16) 0.0269(15) 0.0202(14) 0.0040(12) 0.0109(12) -0.0013(13) C16 0.0277(16) 0.0292(16) 0.0204(14) -0.0049(12) 0.0101(13) -0.0065(13) C17 0.0327(17) 0.0243(15) 0.0312(16) -0.0037(13) 0.0151(14) 0.0015(13) C18 0.0278(16) 0.0259(16) 0.0316(16) 0.0021(13) 0.0130(14) 0.0032(13) C19 0.0259(15) 0.0237(15) 0.0224(14) 0.0018(11) 0.0128(12) 0.0013(12) C20 0.0301(16) 0.0201(14) 0.0193(13) 0.0020(11) 0.0113(12) 0.0002(12) C21 0.0236(15) 0.0226(15) 0.0251(15) 0.0033(12) 0.0090(12) 0.0045(12) C22 0.0263(16) 0.0214(14) 0.0209(14) 0.0003(11) 0.0074(12) 0.0023(12) C23 0.0291(16) 0.0261(15) 0.0304(16) 0.0041(13) 0.0152(14) 0.0091(13) C24 0.0347(18) 0.0285(16) 0.0334(17) 0.0122(13) 0.0142(14) 0.0136(14) C25 0.0313(17) 0.0277(16) 0.0234(15) 0.0053(12) 0.0112(13) 0.0055(13) C26 0.0235(15) 0.0207(14) 0.0203(14) -0.0003(11) 0.0057(12) 0.0035(12) C27 0.0222(15) 0.0187(14) 0.0197(14) 0.0008(11) 0.0025(12) 0.0035(12) C28 0.0275(16) 0.0246(15) 0.0182(13) 0.0028(11) 0.0060(12) 0.0082(13) C29 0.0278(16) 0.0231(15) 0.0280(15) 0.0023(12) 0.0064(13) 0.0050(13) C30 0.0386(19) 0.0273(17) 0.0424(19) 0.0088(14) 0.0045(16) 0.0091(15) C31 0.0323(17) 0.0318(17) 0.0257(15) 0.0085(13) 0.0061(14) -0.0002(14) C32 0.046(2) 0.0346(19) 0.0406(19) 0.0147(15) 0.0066(17) 0.0031(16) C33 0.0272(16) 0.0240(15) 0.0262(15) 0.0033(12) 0.0086(13) 0.0032(13) C34 0.0336(18) 0.0294(17) 0.0318(17) 0.0007(13) 0.0086(14) -0.0015(14) C35 0.0267(16) 0.0241(15) 0.0248(15) -0.0017(12) 0.0040(13) 0.0049(13) C36 0.0340(18) 0.0291(17) 0.0318(17) -0.0046(13) 0.0020(15) 0.0021(14) O2S 0.062(2) 0.111(5) 0.046(2) 0.010(3) 0.0137(19) -0.009(3) O2SB 0.062(2) 0.111(5) 0.046(2) 0.010(3) 0.0137(19) -0.009(3) C2S 0.042(3) 0.109(4) 0.070(3) 0.022(3) 0.010(2) 0.003(3) O1W 0.104(6) 0.031(3) 0.019(3) 0.010(2) -0.023(3) -0.029(4) O2W 0.0321(19) 0.0272(18) 0.0194(16) 0.0050(14) 0.0069(15) 0.0008(15) O3W 0.025(2) 0.039(3) 0.042(3) -0.002(2) 0.003(2) 0.005(2) O1S 0.116(3) 0.057(2) 0.064(2) 0.0014(18) 0.043(2) -0.026(2) C1S 0.071(5) 0.135(7) 0.070(4) 0.001(4) 0.041(4) -0.013(5) O9 0.151(5) 0.046(4) 0.098(4) 0.024(3) 0.061(4) 0.044(4) O10 0.081(3) 0.0346(15) 0.049(2) 0.0067(14) 0.010(2) 0.0108(18) C41 0.096(4) 0.040(4) 0.051(2) 0.009(3) 0.043(3) 0.026(3) C42 0.088(4) 0.130(5) 0.049(3) 0.026(3) 0.042(3) 0.060(4) C43 0.061(5) 0.075(5) 0.045(4) -0.008(3) 0.011(3) 0.027(4) Cl1 0.0823(18) 0.0603(14) 0.0634(14) 0.0094(11) 0.0286(12) 0.0353(12) O1SB 0.116(3) 0.057(2) 0.064(2) 0.0014(18) 0.043(2) -0.026(2) C1SB 0.071(5) 0.135(7) 0.070(4) 0.001(4) 0.041(4) -0.013(5) O9B 0.151(5) 0.046(4) 0.098(4) 0.024(3) 0.061(4) 0.044(4) O10B 0.081(3) 0.0346(15) 0.049(2) 0.0067(14) 0.010(2) 0.0108(18) C41B 0.096(4) 0.040(4) 0.051(2) 0.009(3) 0.043(3) 0.026(3) C42B 0.088(4) 0.130(5) 0.049(3) 0.026(3) 0.042(3) 0.060(4) C43B 0.061(5) 0.075(5) 0.045(4) -0.008(3) 0.011(3) 0.027(4) Cl1B 0.0556(16) 0.144(3) 0.092(2) -0.0360(19) 0.0005(14) 0.0296(18) _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 O1 C2 1.373(3) . ? O2 C4 1.378(3) . ? O3 C9 1.386(4) . ? O4 C11 1.383(4) . ? O5 C16 1.382(3) . ? O6 C18 1.361(4) . ? O7 C23 1.380(4) . ? O8 C25 1.389(4) . ? C1 C6 1.381(4) . ? C1 C2 1.396(4) . ? C1 C28 1.524(4) . ? C2 C3 1.385(4) . ? C3 C4 1.389(4) . ? C4 C5 1.388(4) . ? C5 C6 1.404(4) . ? C5 C7 1.522(4) . ? C7 C8 1.534(4) . ? C7 C29 1.538(4) . ? C8 C13 1.389(4) . ? C8 C9 1.394(4) . ? C9 C10 1.389(4) . ? C10 C11 1.384(4) . ? C11 C12 1.394(4) . ? C12 C13 1.393(4) . ? C12 C14 1.533(4) . ? C14 C15 1.526(4) . ? C14 C31 1.532(4) . ? C15 C20 1.393(4) . ? C15 C16 1.399(4) . ? C16 C17 1.380(4) . ? C17 C18 1.386(4) . ? C18 C19 1.402(4) . ? C19 C20 1.394(4) . ? C19 C21 1.521(4) . ? C21 C22 1.529(4) . ? C21 C33 1.536(4) . ? C22 C27 1.394(4) . ? C22 C23 1.403(4) . ? C23 C24 1.386(4) . ? C24 C25 1.377(4) . ? C25 C26 1.394(4) . ? C26 C27 1.388(4) . ? C26 C28 1.537(4) . ? C28 C35 1.531(4) . ? C29 C30 1.519(4) . ? C31 C32 1.523(5) . ? C33 C34 1.520(4) . ? C35 C36 1.519(4) . ? O2S C2S 1.443(6) . ? O2SB C2S 1.419(15) . ? O1S C1S 1.439(13) . ? O9 C41 1.308(19) . ? O10 C41 1.212(11) . ? C41 C42 1.499(13) . ? C42 C43 1.370(14) . ? C43 Cl1 1.765(10) . ? O1SB C1SB 1.45(2) . ? O9B C41B 1.304(19) . ? O10B C41B 1.212(11) . ? C41B C42B 1.498(13) . ? C42B C43B 1.369(16) . ? C43B Cl1B 1.728(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 117.3(3) . . ? C6 C1 C28 123.0(3) . . ? C2 C1 C28 119.7(3) . . ? O1 C2 C3 121.0(3) . . ? O1 C2 C1 118.1(3) . . ? C3 C2 C1 120.9(3) . . ? C2 C3 C4 120.0(3) . . ? O2 C4 C5 123.3(3) . . ? O2 C4 C3 115.4(3) . . ? C5 C4 C3 121.3(3) . . ? C4 C5 C6 116.7(3) . . ? C4 C5 C7 121.7(3) . . ? C6 C5 C7 121.6(3) . . ? C1 C6 C5 123.7(3) . . ? C5 C7 C8 110.9(2) . . ? C5 C7 C29 114.1(2) . . ? C8 C7 C29 111.4(2) . . ? C13 C8 C9 117.0(3) . . ? C13 C8 C7 121.7(2) . . ? C9 C8 C7 121.3(3) . . ? O3 C9 C10 120.9(3) . . ? O3 C9 C8 117.8(3) . . ? C10 C9 C8 121.3(3) . . ? C11 C10 C9 119.8(3) . . ? O4 C11 C10 121.3(3) . . ? O4 C11 C12 117.5(3) . . ? C10 C11 C12 121.2(3) . . ? C13 C12 C11 117.0(3) . . ? C13 C12 C14 121.3(3) . . ? C11 C12 C14 121.7(3) . . ? C8 C13 C12 123.7(3) . . ? C15 C14 C31 114.6(2) . . ? C15 C14 C12 110.4(2) . . ? C31 C14 C12 112.0(3) . . ? C20 C15 C16 116.4(3) . . ? C20 C15 C14 122.4(3) . . ? C16 C15 C14 121.2(3) . . ? C17 C16 O5 116.0(3) . . ? C17 C16 C15 121.8(3) . . ? O5 C16 C15 122.2(3) . . ? C16 C17 C18 120.2(3) . . ? O6 C18 C17 122.0(3) . . ? O6 C18 C19 117.7(3) . . ? C17 C18 C19 120.3(3) . . ? C20 C19 C18 117.6(3) . . ? C20 C19 C21 123.7(3) . . ? C18 C19 C21 118.7(3) . . ? C15 C20 C19 123.6(3) . . ? C19 C21 C22 111.2(2) . . ? C19 C21 C33 113.9(2) . . ? C22 C21 C33 111.7(2) . . ? C27 C22 C23 116.5(3) . . ? C27 C22 C21 120.7(3) . . ? C23 C22 C21 122.8(3) . . ? O7 C23 C24 114.9(3) . . ? O7 C23 C22 124.3(3) . . ? C24 C23 C22 120.8(3) . . ? C25 C24 C23 120.4(3) . . ? C24 C25 O8 116.7(3) . . ? C24 C25 C26 121.2(3) . . ? O8 C25 C26 122.1(3) . . ? C27 C26 C25 116.8(3) . . ? C27 C26 C28 121.5(3) . . ? C25 C26 C28 121.6(3) . . ? C26 C27 C22 124.1(3) . . ? C1 C28 C35 113.4(2) . . ? C1 C28 C26 111.0(2) . . ? C35 C28 C26 112.3(2) . . ? C30 C29 C7 112.8(2) . . ? C32 C31 C14 111.5(3) . . ? C34 C33 C21 112.7(2) . . ? C36 C35 C28 112.7(2) . . ? O2SB C2S O2S 34.0(11) . . ? O10 C41 O9 127(3) . . ? O10 C41 C42 114.5(19) . . ? O9 C41 C42 119(2) . . ? C43 C42 C41 138(2) . . ? C42 C43 Cl1 117.4(14) . . ? O10B C41B O9B 116(2) . . ? O10B C41B C42B 128.1(19) . . ? O9B C41B C42B 115(2) . . ? C43B C42B C41B 107.0(19) . . ? C42B C43B Cl1B 111.1(12) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.735 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.070 #=======================================END data_CECR-Z-HClA-2MeOH-1.5H2O@90k-12h _database_code_depnum_ccdc_archive 'CCDC 629580' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CECR-Z-HClA-2MeOH-1.5H2O@90k _chemical_melting_point 'not measured' _chemical_formula_moiety ? _chemical_formula_sum 'C41 H54 Cl O13.50' _chemical_formula_weight 798.29 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3796(7) _cell_length_b 13.4055(8) _cell_length_c 14.6244(8) _cell_angle_alpha 98.9840(17) _cell_angle_beta 110.2775(16) _cell_angle_gamma 94.9880(18) _cell_volume 2042.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 675 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.9689 _exptl_absorpt_correction_T_max 0.9812 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15802 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7179 _reflns_number_gt 4400 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+2.2830P] 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 7179 _refine_ls_number_parameters 550 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1159 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.1852 _refine_ls_wR_factor_gt 0.1608 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.013 _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 O1 O 0.8025(2) 0.60574(18) 0.58121(17) 0.0303(6) Uani 1 1 d . . . O2 O 0.4195(2) 0.60534(19) 0.31442(18) 0.0311(6) Uani 1 1 d . . . O3 O 0.3177(2) 0.65190(18) 0.13029(18) 0.0313(6) Uani 1 1 d . . . O4 O 0.5409(2) 0.6145(2) -0.09665(17) 0.0362(7) Uani 1 1 d . . . O5 O 0.7702(2) 0.54583(19) -0.03926(18) 0.0345(6) Uani 1 1 d . . . O6 O 1.1431(2) 0.54330(18) 0.2364(2) 0.0371(7) Uani 1 1 d . . . O7 O 1.2906(2) 0.59629(19) 0.4452(2) 0.0370(7) Uani 1 1 d . . . O8 O 1.0608(2) 0.6331(2) 0.65586(18) 0.0339(6) Uani 1 1 d . . . C1 C 0.7867(3) 0.7435(3) 0.4959(2) 0.0218(8) Uani 1 1 d . . . C2 C 0.7321(3) 0.6514(3) 0.5069(2) 0.0242(8) Uani 1 1 d . . . C3 C 0.6091(3) 0.6076(3) 0.4453(2) 0.0251(8) Uani 1 1 d . . . H3A H 0.5726 0.5452 0.4543 0.030 Uiso 1 1 calc R . . C4 C 0.5400(3) 0.6549(3) 0.3709(3) 0.0248(8) Uani 1 1 d . . . C5 C 0.5908(3) 0.7473(2) 0.3570(2) 0.0218(8) Uani 1 1 d . . . C6 C 0.7150(3) 0.7885(2) 0.4209(2) 0.0223(8) Uani 1 1 d . . . H6A H 0.7519 0.8509 0.4120 0.027 Uiso 1 1 calc R . . C7 C 0.5161(3) 0.7989(2) 0.2745(2) 0.0236(8) Uani 1 1 d . . . H7A H 0.4255 0.7860 0.2684 0.028 Uiso 1 1 calc R . . C8 C 0.5206(3) 0.7490(2) 0.1743(2) 0.0222(8) Uani 1 1 d . . . C9 C 0.4213(3) 0.6779(3) 0.1050(2) 0.0246(8) Uani 1 1 d . . . C10 C 0.4253(4) 0.6332(3) 0.0140(3) 0.0285(8) Uani 1 1 d . . . H10A H 0.3557 0.5857 -0.0328 0.034 Uiso 1 1 calc R . . C11 C 0.5317(3) 0.6587(3) -0.0079(2) 0.0274(8) Uani 1 1 d . . . C12 C 0.6347(3) 0.7290(3) 0.0589(2) 0.0231(8) Uani 1 1 d . . . C13 C 0.6260(3) 0.7721(2) 0.1490(2) 0.0237(8) Uani 1 1 d . . . H13A H 0.6955 0.8198 0.1957 0.028 Uiso 1 1 calc R . . C14 C 0.7528(3) 0.7578(3) 0.0354(2) 0.0275(8) Uani 1 1 d . . . H14A H 0.7291 0.7321 -0.0376 0.033 Uiso 1 1 calc R . . C15 C 0.8590(3) 0.7012(3) 0.0877(2) 0.0239(8) Uani 1 1 d . . . C16 C 0.8611(3) 0.5994(3) 0.0492(2) 0.0265(8) Uani 1 1 d . . . C17 C 0.9539(3) 0.5460(3) 0.0974(3) 0.0293(9) Uani 1 1 d . . . H17A H 0.9523 0.4767 0.0698 0.035 Uiso 1 1 calc R . . C18 C 1.0497(3) 0.5936(3) 0.1863(3) 0.0275(8) Uani 1 1 d . . . C19 C 1.0539(3) 0.6961(2) 0.2278(2) 0.0218(8) Uani 1 1 d . . . C20 C 0.9577(3) 0.7468(3) 0.1771(2) 0.0223(8) Uani 1 1 d . . . H20A H 0.9591 0.8161 0.2047 0.027 Uiso 1 1 calc R . . C21 C 1.1602(3) 0.7450(2) 0.3254(2) 0.0227(8) Uani 1 1 d . . . H21A H 1.2375 0.7159 0.3235 0.027 Uiso 1 1 calc R . . C22 C 1.1344(3) 0.7139(2) 0.4137(2) 0.0231(8) Uani 1 1 d . . . C23 C 1.1971(3) 0.6444(3) 0.4661(3) 0.0285(8) Uani 1 1 d . . . C24 C 1.1706(4) 0.6183(3) 0.5457(3) 0.0317(9) Uani 1 1 d . . . H24A H 1.2139 0.5698 0.5800 0.038 Uiso 1 1 calc R . . C25 C 1.0811(3) 0.6628(3) 0.5753(2) 0.0261(8) Uani 1 1 d . . . C26 C 1.0176(3) 0.7350(2) 0.5272(2) 0.0223(8) Uani 1 1 d . . . C27 C 1.0443(3) 0.7564(2) 0.4462(2) 0.0213(7) Uani 1 1 d . . . H27A H 0.9986 0.8029 0.4104 0.026 Uiso 1 1 calc R . . C28 C 0.9229(3) 0.7888(3) 0.5631(2) 0.0232(8) Uani 1 1 d . . . H28A H 0.9349 0.7735 0.6302 0.028 Uiso 1 1 calc R . . C29 C 0.5538(3) 0.9156(3) 0.2964(3) 0.0279(8) Uani 1 1 d . . . H29A H 0.5529 0.9442 0.3628 0.033 Uiso 1 1 calc R . . H29B H 0.6414 0.9315 0.2986 0.033 Uiso 1 1 calc R . . C30 C 0.4666(4) 0.9665(3) 0.2198(3) 0.0401(10) Uani 1 1 d . . . H30A H 0.4942 1.0406 0.2379 0.060 Uiso 1 1 calc R . . H30B H 0.3797 0.9515 0.2176 0.060 Uiso 1 1 calc R . . H30C H 0.4694 0.9404 0.1543 0.060 Uiso 1 1 calc R . . C31 C 0.7904(4) 0.8734(3) 0.0537(3) 0.0306(9) Uani 1 1 d . . . H31A H 0.8687 0.8884 0.0399 0.037 Uiso 1 1 calc R . . H31B H 0.8087 0.9030 0.1244 0.037 Uiso 1 1 calc R . . C32 C 0.6855(4) 0.9229(3) -0.0121(3) 0.0432(11) Uani 1 1 d . . . H32A H 0.7133 0.9966 0.0003 0.065 Uiso 1 1 calc R . . H32B H 0.6090 0.9105 0.0033 0.065 Uiso 1 1 calc R . . H32C H 0.6670 0.8933 -0.0822 0.065 Uiso 1 1 calc R . . C33 C 1.1929(3) 0.8610(3) 0.3392(3) 0.0261(8) Uani 1 1 d . . . H33A H 1.2078 0.8770 0.2799 0.031 Uiso 1 1 calc R . . H33B H 1.1197 0.8933 0.3441 0.031 Uiso 1 1 calc R . . C34 C 1.3094(4) 0.9066(3) 0.4314(3) 0.0323(9) Uani 1 1 d . . . H34A H 1.3259 0.9807 0.4368 0.048 Uiso 1 1 calc R . . H34B H 1.3827 0.8763 0.4263 0.048 Uiso 1 1 calc R . . H34C H 1.2947 0.8922 0.4906 0.048 Uiso 1 1 calc R . . C35 C 0.9511(3) 0.9049(3) 0.5772(3) 0.0274(8) Uani 1 1 d . . . H35A H 0.9476 0.9227 0.5132 0.033 Uiso 1 1 calc R . . H35B H 0.8845 0.9357 0.5957 0.033 Uiso 1 1 calc R . . C36 C 1.0793(4) 0.9502(3) 0.6563(3) 0.0349(9) Uani 1 1 d . . . H36A H 1.0924 1.0245 0.6620 0.052 Uiso 1 1 calc R . . H36B H 1.1459 0.9211 0.6377 0.052 Uiso 1 1 calc R . . H36C H 1.0827 0.9343 0.7202 0.052 Uiso 1 1 calc R . . O2S O 0.7796(5) 0.2602(7) 0.1655(4) 0.077(2) Uani 0.809(14) 1 d PD A 1 H2S H 0.8222 0.3221 0.2184 0.115 Uiso 0.809(14) 1 d PR A 1 O2SB O 0.7989(16) 0.199(3) 0.1733(18) 0.077(2) Uani 0.191(14) 1 d PD A 2 H2SB H 0.8161 0.2643 0.1880 0.115 Uiso 0.191(14) 1 d PR A 2 C2S C 0.6753(5) 0.2028(5) 0.1786(4) 0.0798(18) Uani 1 1 d D . . H2S1 H 0.7049 0.1704 0.2363 0.120 Uiso 1 1 d R A . H2S2 H 0.6341 0.1500 0.1184 0.120 Uiso 1 1 d R . . H2S3 H 0.6145 0.2475 0.1866 0.120 Uiso 1 1 d R . . O1W O 0.2986(8) 0.5413(5) 0.7712(5) 0.062(3) Uani 0.40 1 d P B 1 H1WA H 0.2329 0.4919 0.7209 0.093 Uiso 0.40 1 d PR B 1 H1WB H 0.2863 0.5748 0.8315 0.093 Uiso 0.40 1 d PR B 1 O2W O 0.2330(4) 0.4438(3) 0.7408(3) 0.0269(9) Uani 0.60 1 d P C 2 H2WA H 0.1861 0.3848 0.7209 0.040 Uiso 0.60 1 d PR C 2 H2WB H 0.2374 0.4621 0.6872 0.040 Uiso 0.60 1 d PR C 2 O3W O 0.3568(4) 0.4609(4) 0.8074(4) 0.0351(13) Uani 0.50 1 d P D 3 H3WA H 0.2777 0.4502 0.8111 0.053 Uiso 0.50 1 d PR D 3 H3WB H 0.3578 0.4868 0.7576 0.053 Uiso 0.50 1 d PR D 3 H1O H 0.7781 0.5525 0.5790 0.053 Uiso 1 1 d R . . H2O H 0.3918 0.6284 0.2611 0.053 Uiso 1 1 d R . . H3O H 0.2772 0.5992 0.0960 0.053 Uiso 1 1 d R . . H40 H 0.4751 0.5877 -0.1285 0.053 Uiso 1 1 d R . . H5O H 0.7085 0.5812 -0.0550 0.053 Uiso 1 1 d R . . H6O H 1.1315 0.4886 0.2177 0.053 Uiso 1 1 d R . . H7O H 1.3007 0.6074 0.4005 0.053 Uiso 1 1 d R . . H8O H 0.9979 0.6297 0.6508 0.053 Uiso 1 1 d R . . O1S O 0.9051(5) 0.1429(3) 0.0714(3) 0.0787(17) Uani 0.857(7) 1 d PD E 1 H1S H 0.8590 0.1844 0.1082 0.118 Uiso 0.857(7) 1 d PR E 1 C1S C 0.8786(9) 0.1753(10) -0.0223(7) 0.084(3) Uani 0.857(7) 1 d PD E 1 H1S1 H 0.7952 0.1976 -0.0427 0.126 Uiso 0.857(7) 1 calc PR E 1 H1S2 H 0.8791 0.1182 -0.0729 0.126 Uiso 0.857(7) 1 calc PR E 1 H1S3 H 0.9436 0.2322 -0.0149 0.126 Uiso 0.857(7) 1 calc PR E 1 O9 O 1.145(4) 0.1773(17) 0.184(3) 0.088(2) Uani 0.486(3) 1 d PD F 1 H9O H 1.0505 0.1552 0.1369 0.131 Uiso 0.486(3) 1 d PR F 1 O10 O 1.106(3) 0.3405(18) 0.174(2) 0.0575(11) Uani 0.486(3) 1 d PD F 1 C41 C 1.174(2) 0.2769(17) 0.200(3) 0.0563(17) Uani 0.486(3) 1 d PD F 1 C42 C 1.311(2) 0.321(2) 0.261(3) 0.080(2) Uani 0.486(3) 1 d PD F 1 H42A H 1.3294 0.3864 0.2487 0.096 Uiso 0.486(3) 1 calc PR F 1 C43 C 1.4178(11) 0.2972(8) 0.3297(7) 0.061(2) Uani 0.486(3) 1 d PD F 1 H43A H 1.4950 0.3435 0.3594 0.073 Uiso 0.486(3) 1 calc PR F 1 Cl1 Cl 1.4007(3) 0.1754(2) 0.3581(2) 0.0666(10) Uani 0.486(3) 1 d PD F 1 O1SB O 0.848(5) 0.178(3) -0.020(3) 0.0787(17) Uani 0.143(7) 1 d PD E 2 H1SB H 0.8548 0.1162 -0.0589 0.118 Uiso 0.143(7) 1 d PR E 2 C1SB C 0.907(4) 0.270(3) 0.056(3) 0.084(3) Uani 0.143(7) 1 d PD E 2 H1S4 H 0.9933 0.2622 0.0955 0.126 Uiso 0.143(7) 1 calc PR E 2 H1S5 H 0.8575 0.2803 0.0988 0.126 Uiso 0.143(7) 1 calc PR E 2 H1S6 H 0.9088 0.3288 0.0240 0.126 Uiso 0.143(7) 1 calc PR E 2 O9B O 1.138(4) 0.1899(16) 0.179(3) 0.088(2) Uani 0.514(3) 1 d PD F 2 H9OB H 1.0499 0.1823 0.1384 0.131 Uiso 0.514(3) 1 d PR F 2 O10B O 1.098(2) 0.3396(18) 0.171(2) 0.0575(11) Uani 0.514(3) 1 d PD F 2 C41B C 1.179(2) 0.2881(17) 0.204(3) 0.0563(17) Uani 0.514(3) 1 d PD F 2 C42B C 1.319(2) 0.324(2) 0.264(3) 0.080(2) Uani 0.514(3) 1 d PD F 2 H42B H 1.3643 0.3915 0.2807 0.096 Uiso 0.514(3) 1 calc PR F 2 C43B C 1.3638(9) 0.2362(9) 0.2898(7) 0.061(2) Uani 0.514(3) 1 d PD F 2 H43B H 1.3153 0.1698 0.2682 0.073 Uiso 0.514(3) 1 calc PR F 2 Cl1B Cl 1.5212(3) 0.2650(3) 0.3668(3) 0.1111(16) Uani 0.514(3) 1 d PD F 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 O1 0.0331(14) 0.0315(14) 0.0292(13) 0.0109(11) 0.0120(12) 0.0087(12) O2 0.0219(13) 0.0344(14) 0.0320(14) 0.0064(11) 0.0053(11) -0.0018(11) O3 0.0256(14) 0.0323(14) 0.0302(14) -0.0052(11) 0.0100(11) -0.0040(11) O4 0.0347(15) 0.0457(16) 0.0197(13) -0.0052(11) 0.0083(12) -0.0093(13) O5 0.0316(15) 0.0356(15) 0.0275(13) -0.0092(11) 0.0084(12) -0.0026(12) O6 0.0309(15) 0.0230(14) 0.0501(17) -0.0045(12) 0.0099(13) 0.0090(12) O7 0.0453(16) 0.0360(15) 0.0497(16) 0.0181(12) 0.0351(14) 0.0192(13) O8 0.0389(15) 0.0441(16) 0.0299(14) 0.0159(12) 0.0199(12) 0.0173(13) C1 0.0215(18) 0.0245(18) 0.0188(17) -0.0020(14) 0.0086(15) 0.0063(15) C2 0.028(2) 0.0268(19) 0.0215(17) 0.0053(15) 0.0119(16) 0.0108(16) C3 0.027(2) 0.0243(19) 0.0271(19) 0.0043(15) 0.0145(16) 0.0007(16) C4 0.0223(19) 0.0266(19) 0.0259(18) 0.0011(15) 0.0115(16) 0.0026(16) C5 0.0232(18) 0.0237(18) 0.0194(17) -0.0015(14) 0.0104(15) 0.0071(15) C6 0.0286(19) 0.0189(17) 0.0214(17) 0.0007(14) 0.0128(15) 0.0043(15) C7 0.0210(18) 0.0237(18) 0.0257(18) 0.0018(14) 0.0090(15) 0.0046(15) C8 0.0233(19) 0.0199(17) 0.0211(17) 0.0048(14) 0.0045(15) 0.0052(15) C9 0.0219(19) 0.0237(18) 0.0250(18) 0.0037(15) 0.0060(16) -0.0004(15) C10 0.029(2) 0.030(2) 0.0209(18) -0.0005(15) 0.0053(16) -0.0025(16) C11 0.033(2) 0.030(2) 0.0174(17) 0.0030(15) 0.0086(16) 0.0013(17) C12 0.0229(19) 0.0249(19) 0.0186(17) 0.0047(14) 0.0041(15) 0.0021(15) C13 0.0258(19) 0.0198(18) 0.0204(17) 0.0045(14) 0.0023(15) 0.0020(15) C14 0.030(2) 0.030(2) 0.0189(17) 0.0020(15) 0.0089(16) -0.0037(17) C15 0.0253(19) 0.0285(19) 0.0196(17) 0.0040(14) 0.0124(15) -0.0026(16) C16 0.028(2) 0.0267(19) 0.0207(18) -0.0057(15) 0.0120(16) -0.0092(16) C17 0.033(2) 0.0218(19) 0.033(2) -0.0055(15) 0.0165(17) 0.0015(16) C18 0.027(2) 0.0243(19) 0.031(2) -0.0007(15) 0.0127(17) 0.0026(16) C19 0.0217(18) 0.0233(18) 0.0213(17) 0.0008(14) 0.0113(15) 0.0005(15) C20 0.029(2) 0.0222(18) 0.0174(16) 0.0015(14) 0.0122(15) 0.0003(15) C21 0.0212(18) 0.0224(18) 0.0251(18) 0.0016(14) 0.0103(15) 0.0039(15) C22 0.0269(19) 0.0207(18) 0.0210(17) -0.0002(14) 0.0099(15) 0.0022(15) C23 0.029(2) 0.0264(19) 0.034(2) 0.0024(16) 0.0172(17) 0.0082(16) C24 0.037(2) 0.029(2) 0.034(2) 0.0109(16) 0.0150(18) 0.0124(17) C25 0.031(2) 0.0286(19) 0.0207(18) 0.0043(15) 0.0122(16) 0.0050(16) C26 0.0230(18) 0.0213(18) 0.0215(17) -0.0009(14) 0.0090(15) 0.0037(15) C27 0.0218(18) 0.0182(17) 0.0182(17) -0.0011(13) 0.0025(14) 0.0013(14) C28 0.0266(19) 0.0242(18) 0.0186(17) 0.0021(14) 0.0079(15) 0.0080(15) C29 0.028(2) 0.0229(19) 0.0303(19) 0.0025(15) 0.0085(16) 0.0063(16) C30 0.040(2) 0.027(2) 0.045(2) 0.0083(18) 0.005(2) 0.0080(19) C31 0.032(2) 0.030(2) 0.0264(19) 0.0069(16) 0.0077(17) -0.0018(17) C32 0.046(3) 0.036(2) 0.044(2) 0.0177(19) 0.008(2) 0.003(2) C33 0.0264(19) 0.0236(19) 0.0275(19) 0.0024(15) 0.0103(16) 0.0021(16) C34 0.035(2) 0.027(2) 0.031(2) 0.0019(16) 0.0105(18) -0.0009(17) C35 0.025(2) 0.0259(19) 0.0253(18) -0.0043(15) 0.0061(16) 0.0051(16) C36 0.032(2) 0.028(2) 0.033(2) -0.0044(16) 0.0024(18) 0.0031(17) O2S 0.061(3) 0.111(6) 0.051(2) 0.009(3) 0.021(2) -0.007(3) O2SB 0.061(3) 0.111(6) 0.051(2) 0.009(3) 0.021(2) -0.007(3) C2S 0.045(3) 0.122(5) 0.070(4) 0.025(4) 0.016(3) 0.006(3) O1W 0.106(7) 0.023(4) 0.019(3) 0.007(3) -0.017(4) -0.025(4) O2W 0.030(2) 0.029(2) 0.019(2) 0.0039(17) 0.0074(18) -0.0001(19) O3W 0.021(3) 0.037(3) 0.037(3) -0.002(2) 0.004(2) 0.001(2) O1S 0.111(4) 0.060(3) 0.061(3) 0.000(2) 0.040(3) -0.030(2) C1S 0.066(6) 0.122(7) 0.066(5) 0.005(4) 0.038(4) -0.012(5) O9 0.141(5) 0.046(4) 0.094(4) 0.019(4) 0.057(3) 0.040(4) O10 0.078(3) 0.0352(18) 0.049(2) 0.0051(15) 0.011(2) 0.012(2) C41 0.096(4) 0.036(4) 0.051(4) 0.008(4) 0.042(3) 0.021(3) C42 0.086(5) 0.128(5) 0.052(4) 0.028(3) 0.043(4) 0.061(4) C43 0.059(6) 0.077(7) 0.040(5) -0.004(4) 0.012(4) 0.032(5) Cl1 0.080(2) 0.0596(17) 0.0656(18) 0.0065(13) 0.0300(15) 0.0321(15) O1SB 0.111(4) 0.060(3) 0.061(3) 0.000(2) 0.040(3) -0.030(2) C1SB 0.066(6) 0.122(7) 0.066(5) 0.005(4) 0.038(4) -0.012(5) O9B 0.141(5) 0.046(4) 0.094(4) 0.019(4) 0.057(3) 0.040(4) O10B 0.078(3) 0.0352(18) 0.049(2) 0.0051(15) 0.011(2) 0.012(2) C41B 0.096(4) 0.036(4) 0.051(4) 0.008(4) 0.042(3) 0.021(3) C42B 0.086(5) 0.128(5) 0.052(4) 0.028(3) 0.043(4) 0.061(4) C43B 0.059(6) 0.077(7) 0.040(5) -0.004(4) 0.012(4) 0.032(5) Cl1B 0.0547(19) 0.145(3) 0.097(2) -0.034(2) 0.0044(17) 0.029(2) _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 O1 C2 1.373(4) . ? O2 C4 1.374(4) . ? O3 C9 1.385(4) . ? O4 C11 1.382(4) . ? O5 C16 1.382(4) . ? O6 C18 1.364(4) . ? O7 C23 1.386(4) . ? O8 C25 1.385(4) . ? C1 C6 1.380(5) . ? C1 C2 1.392(5) . ? C1 C28 1.527(5) . ? C2 C3 1.390(5) . ? C3 C4 1.383(5) . ? C4 C5 1.394(5) . ? C5 C6 1.401(5) . ? C5 C7 1.521(5) . ? C7 C8 1.532(5) . ? C7 C29 1.537(5) . ? C8 C9 1.389(5) . ? C8 C13 1.397(5) . ? C9 C10 1.389(5) . ? C10 C11 1.384(5) . ? C11 C12 1.394(5) . ? C12 C13 1.394(5) . ? C12 C14 1.532(5) . ? C14 C15 1.524(5) . ? C14 C31 1.526(5) . ? C15 C20 1.399(5) . ? C15 C16 1.399(5) . ? C16 C17 1.378(5) . ? C17 C18 1.387(5) . ? C18 C19 1.402(5) . ? C19 C20 1.391(5) . ? C19 C21 1.517(5) . ? C21 C22 1.530(5) . ? C21 C33 1.533(5) . ? C22 C23 1.387(5) . ? C22 C27 1.398(5) . ? C23 C24 1.387(5) . ? C24 C25 1.382(5) . ? C25 C26 1.391(5) . ? C26 C27 1.386(5) . ? C26 C28 1.538(5) . ? C28 C35 1.527(5) . ? C29 C30 1.514(5) . ? C31 C32 1.527(5) . ? C33 C34 1.521(5) . ? C35 C36 1.514(5) . ? O2S C2S 1.442(7) . ? O2SB C2S 1.439(16) . ? O1S C1S 1.442(13) . ? O9 C41 1.31(2) . ? O10 C41 1.213(12) . ? C41 C42 1.514(13) . ? C42 C43 1.379(15) . ? C43 Cl1 1.757(11) . ? O1SB C1SB 1.45(2) . ? O9B C41B 1.309(19) . ? O10B C41B 1.213(12) . ? C41B C42B 1.514(13) . ? C42B C43B 1.381(17) . ? C43B Cl1B 1.724(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 117.5(3) . . ? C6 C1 C28 122.6(3) . . ? C2 C1 C28 119.8(3) . . ? O1 C2 C3 121.1(3) . . ? O1 C2 C1 118.1(3) . . ? C3 C2 C1 120.8(3) . . ? C4 C3 C2 120.1(3) . . ? O2 C4 C3 115.3(3) . . ? O2 C4 C5 123.5(3) . . ? C3 C4 C5 121.1(3) . . ? C4 C5 C6 116.8(3) . . ? C4 C5 C7 121.4(3) . . ? C6 C5 C7 121.7(3) . . ? C1 C6 C5 123.6(3) . . ? C5 C7 C8 110.9(3) . . ? C5 C7 C29 114.1(3) . . ? C8 C7 C29 111.8(3) . . ? C9 C8 C13 116.8(3) . . ? C9 C8 C7 121.9(3) . . ? C13 C8 C7 121.3(3) . . ? O3 C9 C8 117.5(3) . . ? O3 C9 C10 120.8(3) . . ? C8 C9 C10 121.7(3) . . ? C11 C10 C9 119.4(3) . . ? O4 C11 C10 121.3(3) . . ? O4 C11 C12 117.2(3) . . ? C10 C11 C12 121.5(3) . . ? C13 C12 C11 117.0(3) . . ? C13 C12 C14 121.1(3) . . ? C11 C12 C14 121.9(3) . . ? C12 C13 C8 123.6(3) . . ? C15 C14 C31 114.5(3) . . ? C15 C14 C12 110.5(3) . . ? C31 C14 C12 112.1(3) . . ? C20 C15 C16 116.4(3) . . ? C20 C15 C14 122.4(3) . . ? C16 C15 C14 121.2(3) . . ? C17 C16 O5 115.8(3) . . ? C17 C16 C15 121.9(3) . . ? O5 C16 C15 122.3(3) . . ? C16 C17 C18 120.0(3) . . ? O6 C18 C17 121.7(3) . . ? O6 C18 C19 117.5(3) . . ? C17 C18 C19 120.7(3) . . ? C20 C19 C18 117.4(3) . . ? C20 C19 C21 123.6(3) . . ? C18 C19 C21 119.0(3) . . ? C19 C20 C15 123.6(3) . . ? C19 C21 C22 111.3(3) . . ? C19 C21 C33 113.8(3) . . ? C22 C21 C33 112.3(3) . . ? C23 C22 C27 116.4(3) . . ? C23 C22 C21 123.3(3) . . ? C27 C22 C21 120.2(3) . . ? O7 C23 C24 114.5(3) . . ? O7 C23 C22 124.1(3) . . ? C24 C23 C22 121.4(3) . . ? C25 C24 C23 120.0(3) . . ? C24 C25 O8 116.4(3) . . ? C24 C25 C26 121.1(3) . . ? O8 C25 C26 122.5(3) . . ? C27 C26 C25 116.9(3) . . ? C27 C26 C28 121.7(3) . . ? C25 C26 C28 121.4(3) . . ? C26 C27 C22 124.1(3) . . ? C1 C28 C35 113.8(3) . . ? C1 C28 C26 110.8(3) . . ? C35 C28 C26 112.0(3) . . ? C30 C29 C7 113.0(3) . . ? C14 C31 C32 111.5(3) . . ? C34 C33 C21 112.8(3) . . ? C36 C35 C28 113.0(3) . . ? O2SB C2S O2S 35.4(12) . . ? O10 C41 O9 130(3) . . ? O10 C41 C42 114(2) . . ? O9 C41 C42 116(3) . . ? C43 C42 C41 141(2) . . ? C42 C43 Cl1 115.1(15) . . ? O10B C41B O9B 113(3) . . ? O10B C41B C42B 128(2) . . ? O9B C41B C42B 119(3) . . ? C43B C42B C41B 103.4(19) . . ? C42B C43B Cl1B 109.7(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.555 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.068 #_eof #End of Crystallographic Information File