# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Richard Gandour' _publ_contact_author_address ; Department of Chemistry (MC 0212) Virginia Tech Blacksburg Virginia 24061 USA ; _publ_contact_author_email GANDOUR@VT.EDU _publ_section_title ; Homologous, Long-chain Alkyl Dendrons Form Homologous Thin Films on Silver Oxide Surfaces. ; loop_ _publ_author_name 'Richard Gandour' 'B. Scott Day' 'Brett L. Kite' 'Melinda K. McPherson' 'John R. Morris' ; C.Slebodnik ; 'Andre A. Williams' data_cs359 _database_code_depnum_ccdc_archive 'CCDC 271916' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H71 N O7' _chemical_formula_sum 'C38 H71 N O7' _chemical_formula_weight 653.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.6653(9) _cell_length_b 9.9138(10) _cell_length_c 35.868(3) _cell_angle_alpha 82.928(8) _cell_angle_beta 89.815(10) _cell_angle_gamma 81.801(10) _cell_volume 1978.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3026 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 21.3 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.011 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.098 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Crysalis (Oxford Diffraction)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur2' _diffrn_detector CCD _diffrn_detector_type 'Oxford Diffraction Sapphire 2 CCD' _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 13578 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.1085 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 25.05 _reflns_number_total 7015 _reflns_number_gt 4338 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis (Oxford Diffraction)' _computing_cell_refinement 'Crysalis (Oxford Diffraction)' _computing_data_reduction 'Crysalis (Oxford Diffraction)' _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^)+(0.0520P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7015 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1205 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1215 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.8027(3) 0.9471(2) 0.27357(5) 0.0266(5) Uani 1 1 d . . . O2 O 0.6152(3) 0.80543(18) 0.11988(5) 0.0226(5) Uani 1 1 d . . . O3 O 0.3819(3) 0.66450(18) 0.15167(5) 0.0207(4) Uani 1 1 d . . . O4 O 0.1396(3) 1.1361(2) 0.10497(5) 0.0345(6) Uani 1 1 d . . . O5 O 0.4111(3) 1.20985(18) 0.06395(5) 0.0211(4) Uani 1 1 d . . . O6 O 1.1591(3) 1.28017(18) 0.22635(5) 0.0218(4) Uani 1 1 d . . . O7 O 0.8685(3) 1.42738(17) 0.24853(5) 0.0187(4) Uani 1 1 d . . . N1 N 0.5039(4) 1.0231(2) 0.23073(6) 0.0160(5) Uani 1 1 d . . . H1 H 0.3516 1.0429 0.2283 0.019 Uiso 1 1 calc R . . C1 C -0.7371(6) -0.2196(4) 0.63796(9) 0.0407(9) Uani 1 1 d . . . H1C H -0.7683 -0.1503 0.6545 0.061 Uiso 1 1 calc R . . H1D H -0.6888 -0.3072 0.6524 0.061 Uiso 1 1 calc R . . H1E H -0.8791 -0.2229 0.6238 0.061 Uiso 1 1 calc R . . C2 C -0.5378(5) -0.1851(3) 0.61104(9) 0.0333(8) Uani 1 1 d . . . H2A H -0.3912 -0.1906 0.6254 0.040 Uiso 1 1 calc R . . H2B H -0.5125 -0.2534 0.5937 0.040 Uiso 1 1 calc R . . C3 C -0.5904(5) -0.0441(3) 0.58877(8) 0.0244(7) Uani 1 1 d . . . H3A H -0.6120 0.0242 0.6062 0.029 Uiso 1 1 calc R . . H3B H -0.7391 -0.0380 0.5749 0.029 Uiso 1 1 calc R . . C4 C -0.3963(5) -0.0099(3) 0.56125(8) 0.0235(7) Uani 1 1 d . . . H4A H -0.2465 -0.0196 0.5750 0.028 Uiso 1 1 calc R . . H4B H -0.3788 -0.0765 0.5434 0.028 Uiso 1 1 calc R . . C5 C -0.4425(5) 0.1330(3) 0.53974(8) 0.0241(7) Uani 1 1 d . . . H5A H -0.4595 0.1996 0.5576 0.029 Uiso 1 1 calc R . . H5B H -0.5924 0.1428 0.5260 0.029 Uiso 1 1 calc R . . C6 C -0.2478(5) 0.1662(3) 0.51221(7) 0.0225(7) Uani 1 1 d . . . H6A H -0.0971 0.1536 0.5259 0.027 Uiso 1 1 calc R . . H6B H -0.2340 0.1011 0.4939 0.027 Uiso 1 1 calc R . . C7 C -0.2894(5) 0.3108(3) 0.49134(8) 0.0247(7) Uani 1 1 d . . . H7A H -0.3059 0.3761 0.5096 0.030 Uiso 1 1 calc R . . H7B H -0.4383 0.3229 0.4772 0.030 Uiso 1 1 calc R . . C8 C -0.0910(5) 0.3435(3) 0.46444(8) 0.0247(7) Uani 1 1 d . . . H8A H -0.0762 0.2791 0.4460 0.030 Uiso 1 1 calc R . . H8B H 0.0583 0.3299 0.4785 0.030 Uiso 1 1 calc R . . C9 C -0.1299(5) 0.4889(3) 0.44390(8) 0.0259(7) Uani 1 1 d . . . H9A H -0.1460 0.5535 0.4623 0.031 Uiso 1 1 calc R . . H9B H -0.2782 0.5024 0.4296 0.031 Uiso 1 1 calc R . . C10 C 0.0712(5) 0.5205(3) 0.41739(8) 0.0250(7) Uani 1 1 d . . . H10A H 0.2200 0.5035 0.4316 0.030 Uiso 1 1 calc R . . H10B H 0.0835 0.4574 0.3986 0.030 Uiso 1 1 calc R . . C11 C 0.0410(5) 0.6663(3) 0.39751(8) 0.0224(7) Uani 1 1 d . . . H11A H 0.0301 0.7299 0.4162 0.027 Uiso 1 1 calc R . . H11B H -0.1075 0.6838 0.3832 0.027 Uiso 1 1 calc R . . C12 C 0.2460(5) 0.6934(3) 0.37110(7) 0.0212(6) Uani 1 1 d . . . H12A H 0.3927 0.6793 0.3858 0.025 Uiso 1 1 calc R . . H12B H 0.2615 0.6260 0.3535 0.025 Uiso 1 1 calc R . . C13 C 0.2202(5) 0.8363(3) 0.34884(7) 0.0208(6) Uani 1 1 d . . . H13A H 0.0653 0.8562 0.3364 0.025 Uiso 1 1 calc R . . H13B H 0.2283 0.9039 0.3660 0.025 Uiso 1 1 calc R . . C14 C 0.4144(5) 0.8478(3) 0.31961(7) 0.0214(6) Uani 1 1 d . . . H14A H 0.5685 0.8252 0.3323 0.026 Uiso 1 1 calc R . . H14B H 0.4041 0.7801 0.3025 0.026 Uiso 1 1 calc R . . C15 C 0.4031(5) 0.9882(3) 0.29668(7) 0.0203(6) Uani 1 1 d . . . H15A H 0.2461 1.0151 0.2852 0.024 Uiso 1 1 calc R . . H15B H 0.4293 1.0557 0.3131 0.024 Uiso 1 1 calc R . . C16 C 0.5907(5) 0.9851(3) 0.26635(8) 0.0199(6) Uani 1 1 d . . . C17 C 0.6423(4) 1.0344(3) 0.19592(7) 0.0149(6) Uani 1 1 d . . . C18 C 0.7682(4) 0.8905(2) 0.18955(7) 0.0162(6) Uani 1 1 d . . . H18A H 0.8557 0.8991 0.1663 0.019 Uiso 1 1 calc R . . H18B H 0.8836 0.8584 0.2097 0.019 Uiso 1 1 calc R . . C19 C 0.6047(5) 0.7815(3) 0.18759(7) 0.0199(6) Uani 1 1 d . . . H19A H 0.6823 0.6957 0.2010 0.024 Uiso 1 1 calc R . . H19B H 0.4592 0.8085 0.2008 0.024 Uiso 1 1 calc R . . C20 C 0.5383(5) 0.7558(3) 0.14903(8) 0.0189(6) Uani 1 1 d . . . C21 C 0.3078(5) 0.6063(3) 0.11828(7) 0.0191(6) Uani 1 1 d . . . C22 C 0.1428(5) 0.5075(3) 0.13529(8) 0.0255(7) Uani 1 1 d . . . H22A H 0.2269 0.4433 0.1547 0.038 Uiso 1 1 calc R . . H22B H 0.0903 0.4586 0.1161 0.038 Uiso 1 1 calc R . . H22C H 0.0070 0.5582 0.1458 0.038 Uiso 1 1 calc R . . C23 C 0.5246(5) 0.5293(3) 0.10127(8) 0.0247(7) Uani 1 1 d . . . H23A H 0.6286 0.5931 0.0914 0.037 Uiso 1 1 calc R . . H23B H 0.4742 0.4831 0.0813 0.037 Uiso 1 1 calc R . . H23C H 0.6080 0.4631 0.1203 0.037 Uiso 1 1 calc R . . C24 C 0.1757(5) 0.7180(3) 0.08998(8) 0.0259(7) Uani 1 1 d . . . H24A H 0.0474 0.7688 0.1022 0.039 Uiso 1 1 calc R . . H24B H 0.1126 0.6769 0.0700 0.039 Uiso 1 1 calc R . . H24C H 0.2837 0.7789 0.0798 0.039 Uiso 1 1 calc R . . C25 C 0.4558(4) 1.0934(3) 0.16509(7) 0.0165(6) Uani 1 1 d . . . H25A H 0.3441 1.0282 0.1642 0.020 Uiso 1 1 calc R . . H25B H 0.3672 1.1767 0.1726 0.020 Uiso 1 1 calc R . . C26 C 0.5453(5) 1.1271(3) 0.12557(7) 0.0185(6) Uani 1 1 d . . . H26A H 0.6290 1.2063 0.1246 0.022 Uiso 1 1 calc R . . H26B H 0.6564 1.0502 0.1190 0.022 Uiso 1 1 calc R . . C27 C 0.3408(5) 1.1572(3) 0.09794(7) 0.0190(6) Uani 1 1 d . . . C28 C 0.2447(5) 1.2367(3) 0.03152(7) 0.0233(7) Uani 1 1 d . . . C29 C 0.1638(6) 1.1029(3) 0.02351(8) 0.0362(8) Uani 1 1 d . . . H29A H 0.3007 1.0345 0.0221 0.054 Uiso 1 1 calc R . . H29B H 0.0775 1.1178 0.0000 0.054 Uiso 1 1 calc R . . H29C H 0.0623 1.0721 0.0433 0.054 Uiso 1 1 calc R . . C30 C 0.3986(6) 1.2903(3) -0.00005(8) 0.0383(8) Uani 1 1 d . . . H30A H 0.4529 1.3727 0.0059 0.057 Uiso 1 1 calc R . . H30B H 0.3068 1.3100 -0.0230 0.057 Uiso 1 1 calc R . . H30C H 0.5337 1.2222 -0.0030 0.057 Uiso 1 1 calc R . . C31 C 0.0358(5) 1.3439(3) 0.03818(8) 0.0337(8) Uani 1 1 d . . . H31A H -0.0598 1.3074 0.0580 0.051 Uiso 1 1 calc R . . H31B H -0.0593 1.3685 0.0156 0.051 Uiso 1 1 calc R . . H31C H 0.0938 1.4239 0.0451 0.051 Uiso 1 1 calc R . . C32 C 0.8347(4) 1.1277(3) 0.19893(7) 0.0167(6) Uani 1 1 d . . . H32A H 0.9582 1.0791 0.2163 0.020 Uiso 1 1 calc R . . H32B H 0.9071 1.1429 0.1745 0.020 Uiso 1 1 calc R . . C33 C 0.7500(5) 1.2669(3) 0.21189(8) 0.0187(6) Uani 1 1 d . . . H33A H 0.6840 1.3308 0.1906 0.022 Uiso 1 1 calc R . . H33B H 0.6245 1.2577 0.2301 0.022 Uiso 1 1 calc R . . C34 C 0.9503(5) 1.3235(3) 0.22933(7) 0.0168(6) Uani 1 1 d . . . C35 C 1.0367(5) 1.4937(3) 0.26966(7) 0.0188(6) Uani 1 1 d . . . C36 C 1.1784(5) 1.3890(3) 0.29820(8) 0.0254(7) Uani 1 1 d . . . H36A H 1.0728 1.3342 0.3120 0.038 Uiso 1 1 calc R . . H36B H 1.2586 1.4353 0.3153 0.038 Uiso 1 1 calc R . . H36C H 1.2941 1.3309 0.2855 0.038 Uiso 1 1 calc R . . C37 C 0.8657(5) 1.5956(3) 0.28859(8) 0.0246(7) Uani 1 1 d . . . H37A H 0.7739 1.6587 0.2698 0.037 Uiso 1 1 calc R . . H37B H 0.9546 1.6454 0.3035 0.037 Uiso 1 1 calc R . . H37C H 0.7604 1.5471 0.3044 0.037 Uiso 1 1 calc R . . C38 C 1.1954(5) 1.5678(3) 0.24234(8) 0.0231(7) Uani 1 1 d . . . H38A H 1.3031 1.5016 0.2309 0.035 Uiso 1 1 calc R . . H38B H 1.2850 1.6224 0.2556 0.035 Uiso 1 1 calc R . . H38C H 1.0983 1.6263 0.2232 0.035 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 0.0215(11) 0.0306(12) 0.0249(11) 0.0026(9) -0.0051(9) 0.0005(9) O2 0.0295(11) 0.0215(11) 0.0188(11) -0.0044(9) 0.0040(9) -0.0088(9) O3 0.0254(10) 0.0193(10) 0.0200(10) -0.0056(8) -0.0010(8) -0.0090(9) O4 0.0211(11) 0.0609(16) 0.0205(11) 0.0066(10) -0.0029(9) -0.0129(11) O5 0.0254(11) 0.0228(11) 0.0141(10) 0.0030(8) -0.0031(8) -0.0047(9) O6 0.0148(10) 0.0232(11) 0.0290(11) -0.0112(9) 0.0012(9) -0.0008(9) O7 0.0185(10) 0.0176(10) 0.0218(10) -0.0081(8) -0.0001(8) -0.0042(8) N1 0.0139(11) 0.0172(12) 0.0163(12) -0.0007(10) -0.0033(10) -0.0013(10) C1 0.0381(19) 0.046(2) 0.036(2) 0.0106(16) -0.0009(16) -0.0153(17) C2 0.0298(18) 0.0346(19) 0.0341(18) 0.0044(15) -0.0020(15) -0.0069(15) C3 0.0246(16) 0.0256(17) 0.0222(16) -0.0016(13) 0.0004(13) -0.0021(13) C4 0.0237(16) 0.0265(17) 0.0203(15) -0.0051(13) -0.0018(13) -0.0017(13) C5 0.0250(16) 0.0258(17) 0.0210(15) -0.0012(13) -0.0013(13) -0.0035(13) C6 0.0213(15) 0.0264(17) 0.0185(15) -0.0004(12) -0.0026(12) -0.0014(13) C7 0.0215(15) 0.0285(17) 0.0236(16) 0.0001(13) 0.0014(13) -0.0049(13) C8 0.0246(16) 0.0238(16) 0.0241(16) 0.0017(13) 0.0003(13) -0.0017(13) C9 0.0222(16) 0.0284(17) 0.0252(17) 0.0028(13) -0.0016(13) -0.0021(13) C10 0.0242(16) 0.0283(17) 0.0220(16) -0.0003(13) 0.0012(13) -0.0048(14) C11 0.0226(16) 0.0228(16) 0.0210(15) 0.0005(12) -0.0002(13) -0.0030(13) C12 0.0199(15) 0.0252(16) 0.0175(15) -0.0014(12) -0.0017(12) -0.0009(13) C13 0.0233(15) 0.0228(16) 0.0172(15) -0.0047(12) -0.0008(12) -0.0043(13) C14 0.0244(16) 0.0231(16) 0.0166(15) -0.0031(12) 0.0012(12) -0.0022(13) C15 0.0237(15) 0.0196(15) 0.0172(15) -0.0028(12) -0.0013(12) -0.0018(13) C16 0.0199(16) 0.0188(15) 0.0218(16) -0.0038(12) -0.0030(13) -0.0039(13) C17 0.0141(14) 0.0148(14) 0.0150(14) 0.0007(11) 0.0013(11) -0.0019(11) C18 0.0155(14) 0.0139(14) 0.0185(14) -0.0024(11) -0.0011(12) 0.0005(12) C19 0.0215(15) 0.0167(15) 0.0215(15) -0.0024(12) 0.0030(12) -0.0030(12) C20 0.0180(15) 0.0139(15) 0.0248(17) -0.0052(13) -0.0012(13) 0.0003(12) C21 0.0235(15) 0.0182(15) 0.0180(15) -0.0064(12) -0.0024(12) -0.0078(13) C22 0.0285(17) 0.0263(17) 0.0236(16) -0.0054(13) -0.0032(13) -0.0082(14) C23 0.0311(17) 0.0178(16) 0.0261(17) -0.0049(13) -0.0030(14) -0.0044(13) C24 0.0250(16) 0.0278(17) 0.0244(16) -0.0041(13) -0.0051(13) -0.0017(14) C25 0.0161(14) 0.0149(14) 0.0192(14) -0.0035(11) -0.0004(12) -0.0033(12) C26 0.0200(15) 0.0168(15) 0.0191(15) -0.0035(12) 0.0026(12) -0.0030(12) C27 0.0242(16) 0.0161(15) 0.0166(15) -0.0011(12) -0.0001(13) -0.0032(13) C28 0.0282(16) 0.0279(17) 0.0146(15) -0.0025(13) -0.0048(13) -0.0068(14) C29 0.055(2) 0.0321(19) 0.0235(17) -0.0050(14) -0.0092(16) -0.0116(17) C30 0.044(2) 0.048(2) 0.0209(17) 0.0076(15) -0.0047(15) -0.0105(17) C31 0.0369(18) 0.0321(19) 0.0290(18) 0.0006(14) -0.0120(15) 0.0018(15) C32 0.0175(14) 0.0148(14) 0.0184(15) -0.0041(12) 0.0006(12) -0.0025(12) C33 0.0167(14) 0.0181(15) 0.0219(15) -0.0046(12) -0.0014(12) -0.0031(12) C34 0.0250(16) 0.0116(14) 0.0143(14) -0.0027(11) 0.0019(12) -0.0034(12) C35 0.0227(15) 0.0168(15) 0.0185(15) -0.0066(12) -0.0055(12) -0.0043(12) C36 0.0306(17) 0.0229(16) 0.0221(16) -0.0020(13) -0.0023(14) -0.0027(14) C37 0.0308(17) 0.0218(16) 0.0228(16) -0.0099(13) -0.0012(13) -0.0025(13) C38 0.0235(16) 0.0177(15) 0.0294(17) -0.0040(13) -0.0009(13) -0.0067(13) _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 C16 1.225(3) . ? O2 C20 1.207(3) . ? O3 C20 1.349(3) . ? O3 C21 1.478(3) . ? O4 C27 1.208(3) . ? O5 C27 1.348(3) . ? O5 C28 1.474(3) . ? O6 C34 1.209(3) . ? O7 C34 1.336(3) . ? O7 C35 1.490(3) . ? N1 C16 1.360(3) . ? N1 C17 1.473(3) . ? C1 C2 1.532(4) . ? C2 C3 1.513(4) . ? C3 C4 1.521(4) . ? C4 C5 1.516(4) . ? C5 C6 1.522(4) . ? C6 C7 1.521(4) . ? C7 C8 1.522(4) . ? C8 C9 1.523(4) . ? C9 C10 1.523(4) . ? C10 C11 1.518(4) . ? C11 C12 1.529(4) . ? C12 C13 1.526(4) . ? C13 C14 1.524(4) . ? C14 C15 1.520(4) . ? C15 C16 1.518(4) . ? C17 C25 1.534(4) . ? C17 C32 1.539(3) . ? C17 C18 1.544(3) . ? C18 C19 1.528(3) . ? C19 C20 1.496(4) . ? C21 C23 1.519(4) . ? C21 C24 1.519(4) . ? C21 C22 1.522(4) . ? C25 C26 1.519(3) . ? C26 C27 1.500(4) . ? C28 C31 1.513(4) . ? C28 C30 1.518(4) . ? C28 C29 1.523(4) . ? C32 C33 1.523(3) . ? C33 C34 1.505(4) . ? C35 C36 1.509(4) . ? C35 C37 1.518(4) . ? C35 C38 1.521(4) . ? 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 C20 O3 C21 121.3(2) . . ? C27 O5 C28 120.7(2) . . ? C34 O7 C35 120.4(2) . . ? C16 N1 C17 127.2(2) . . ? C3 C2 C1 113.4(3) . . ? C2 C3 C4 113.9(2) . . ? C5 C4 C3 114.5(2) . . ? C4 C5 C6 114.2(2) . . ? C7 C6 C5 114.5(2) . . ? C6 C7 C8 113.9(2) . . ? C7 C8 C9 114.1(2) . . ? C8 C9 C10 113.5(2) . . ? C11 C10 C9 114.6(2) . . ? C10 C11 C12 112.9(2) . . ? C13 C12 C11 115.4(2) . . ? C14 C13 C12 111.8(2) . . ? C15 C14 C13 114.9(2) . . ? C16 C15 C14 110.5(2) . . ? O1 C16 N1 123.0(2) . . ? O1 C16 C15 122.2(3) . . ? N1 C16 C15 114.8(2) . . ? N1 C17 C25 104.40(19) . . ? N1 C17 C32 110.6(2) . . ? C25 C17 C32 112.4(2) . . ? N1 C17 C18 109.3(2) . . ? C25 C17 C18 112.0(2) . . ? C32 C17 C18 108.1(2) . . ? C19 C18 C17 115.6(2) . . ? C20 C19 C18 116.0(2) . . ? O2 C20 O3 124.6(2) . . ? O2 C20 C19 126.1(2) . . ? O3 C20 C19 109.3(2) . . ? O3 C21 C23 109.6(2) . . ? O3 C21 C24 110.9(2) . . ? C23 C21 C24 111.9(2) . . ? O3 C21 C22 102.0(2) . . ? C23 C21 C22 110.8(2) . . ? C24 C21 C22 111.3(2) . . ? C26 C25 C17 117.5(2) . . ? C27 C26 C25 110.4(2) . . ? O4 C27 O5 124.2(2) . . ? O4 C27 C26 124.7(2) . . ? O5 C27 C26 111.1(2) . . ? O5 C28 C31 110.8(2) . . ? O5 C28 C30 102.5(2) . . ? C31 C28 C30 111.0(2) . . ? O5 C28 C29 109.7(2) . . ? C31 C28 C29 111.8(2) . . ? C30 C28 C29 110.6(2) . . ? C33 C32 C17 116.0(2) . . ? C34 C33 C32 111.6(2) . . ? O6 C34 O7 124.3(2) . . ? O6 C34 C33 124.2(2) . . ? O7 C34 C33 111.6(2) . . ? O7 C35 C36 110.4(2) . . ? O7 C35 C37 101.51(19) . . ? C36 C35 C37 111.3(2) . . ? O7 C35 C38 109.9(2) . . ? C36 C35 C38 112.4(2) . . ? C37 C35 C38 110.8(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 C1 C2 C3 C4 -178.6(3) . . . . ? C2 C3 C4 C5 -177.9(2) . . . . ? C3 C4 C5 C6 -179.9(2) . . . . ? C4 C5 C6 C7 -178.3(2) . . . . ? C5 C6 C7 C8 178.9(2) . . . . ? C6 C7 C8 C9 -179.1(2) . . . . ? C7 C8 C9 C10 179.4(2) . . . . ? C8 C9 C10 C11 -178.1(2) . . . . ? C9 C10 C11 C12 -179.8(2) . . . . ? C10 C11 C12 C13 177.2(2) . . . . ? C11 C12 C13 C14 -172.4(2) . . . . ? C12 C13 C14 C15 -179.0(2) . . . . ? C13 C14 C15 C16 -175.2(2) . . . . ? C17 N1 C16 O1 -4.2(4) . . . . ? C17 N1 C16 C15 177.9(2) . . . . ? C14 C15 C16 O1 -55.3(3) . . . . ? C14 C15 C16 N1 122.6(2) . . . . ? C16 N1 C17 C25 -175.0(2) . . . . ? C16 N1 C17 C32 -53.9(3) . . . . ? C16 N1 C17 C18 65.1(3) . . . . ? N1 C17 C18 C19 56.9(3) . . . . ? C25 C17 C18 C19 -58.2(3) . . . . ? C32 C17 C18 C19 177.4(2) . . . . ? C17 C18 C19 C20 98.3(3) . . . . ? C21 O3 C20 O2 6.1(4) . . . . ? C21 O3 C20 C19 -172.3(2) . . . . ? C18 C19 C20 O2 5.8(4) . . . . ? C18 C19 C20 O3 -175.9(2) . . . . ? C20 O3 C21 C23 60.4(3) . . . . ? C20 O3 C21 C24 -63.5(3) . . . . ? C20 O3 C21 C22 177.9(2) . . . . ? N1 C17 C25 C26 175.8(2) . . . . ? C32 C17 C25 C26 55.8(3) . . . . ? C18 C17 C25 C26 -66.2(3) . . . . ? C17 C25 C26 C27 169.0(2) . . . . ? C28 O5 C27 O4 -4.4(4) . . . . ? C28 O5 C27 C26 174.9(2) . . . . ? C25 C26 C27 O4 -11.2(4) . . . . ? C25 C26 C27 O5 169.5(2) . . . . ? C27 O5 C28 C31 63.0(3) . . . . ? C27 O5 C28 C30 -178.5(2) . . . . ? C27 O5 C28 C29 -61.0(3) . . . . ? N1 C17 C32 C33 -50.3(3) . . . . ? C25 C17 C32 C33 66.0(3) . . . . ? C18 C17 C32 C33 -169.9(2) . . . . ? C17 C32 C33 C34 155.9(2) . . . . ? C35 O7 C34 O6 -3.0(4) . . . . ? C35 O7 C34 C33 176.9(2) . . . . ? C32 C33 C34 O6 14.8(4) . . . . ? C32 C33 C34 O7 -165.2(2) . . . . ? C34 O7 C35 C36 -58.0(3) . . . . ? C34 O7 C35 C37 -176.2(2) . . . . ? C34 O7 C35 C38 66.5(3) . . . . ? 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 N1 H1 O6 0.86 2.44 2.969(3) 120.3 1_455 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.243 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.050 data_cs661 _database_code_depnum_ccdc_archive 'CCDC 271917' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H43 N O7' _chemical_formula_sum 'C24 H43 N O7' _chemical_formula_weight 457.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.4497(8) _cell_length_b 15.755(2) _cell_length_c 29.520(4) _cell_angle_alpha 93.557(11) _cell_angle_beta 91.632(11) _cell_angle_gamma 91.894(12) _cell_volume 2527.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3409 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 25.39 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur' _diffrn_detector CCD _diffrn_detector_type 'Oxford Diffraction Sapphire 3 CCD' _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 18103 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 25.00 _reflns_number_total 18103 _reflns_number_gt 12927 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction)' _computing_cell_refinement 'CrysAlis (Oxford Diffraction)' _computing_data_reduction 'CrysAlis (Oxford Diffraction)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18103 _refine_ls_number_parameters 588 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1439 _refine_ls_R_factor_gt 0.1253 _refine_ls_wR_factor_ref 0.4168 _refine_ls_wR_factor_gt 0.3922 _refine_ls_goodness_of_fit_ref 1.631 _refine_ls_restrained_S_all 1.631 _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 0.9402(5) -0.22753(18) 0.18696(10) 0.0295(7) Uani 1 1 d . . . O2 O 0.6199(6) -0.31127(18) 0.20437(11) 0.0348(8) Uani 1 1 d . . . H2C H 0.7297 -0.3462 0.2090 0.052 Uiso 1 1 calc R . . O3 O -0.0527(5) -0.08821(18) 0.03149(9) 0.0293(7) Uani 1 1 d . . . O4 O 0.1958(6) -0.18031(19) -0.00359(10) 0.0337(8) Uani 1 1 d . . . H4A H 0.0900 -0.1783 -0.0247 0.050 Uiso 1 1 calc R . . O5 O 0.1050(6) 0.16500(18) 0.07480(10) 0.0307(7) Uani 1 1 d . . . O6 O 0.3519(5) 0.07355(17) 0.03878(9) 0.0281(7) Uani 1 1 d . . . H6C H 0.2492 0.0779 0.0173 0.042 Uiso 1 1 calc R . . O7 O 0.6665(5) 0.05544(18) 0.22407(9) 0.0271(7) Uani 1 1 d . . . O8 O 0.4314(6) 0.66534(17) 0.07165(9) 0.0294(7) Uani 1 1 d . . . O9 O 0.1575(5) 0.57057(17) 0.03766(9) 0.0273(7) Uani 1 1 d . . . H9C H 0.2505 0.5745 0.0156 0.041 Uiso 1 1 calc R . . O10 O 0.5692(5) 0.41664(18) 0.03401(9) 0.0294(7) Uani 1 1 d . . . O11 O 0.2972(6) 0.32064(19) 0.00055(10) 0.0339(8) Uani 1 1 d . . . H11A H 0.3952 0.3223 -0.0209 0.051 Uiso 1 1 calc R . . O12 O -0.3742(6) 0.26840(18) 0.19147(10) 0.0313(7) Uani 1 1 d . . . O13 O -0.0504(6) 0.19106(18) 0.20917(12) 0.0376(8) Uani 1 1 d . . . H13C H -0.1589 0.1530 0.2126 0.056 Uiso 1 1 calc R . . O14 O -0.0976(5) 0.55937(17) 0.22399(9) 0.0268(7) Uani 1 1 d . . . N1 N 0.3342(6) -0.0029(2) 0.18464(10) 0.0217(8) Uani 1 1 d . . . H1A H 0.1737 -0.0110 0.1850 0.026 Uiso 1 1 calc R . . N2 N 0.2287(6) 0.5059(2) 0.18680(10) 0.0210(7) Uani 1 1 d . . . H2D H 0.3896 0.5024 0.1878 0.025 Uiso 1 1 calc R . . C1 C 0.4571(7) -0.0339(2) 0.14284(13) 0.0232(9) Uani 1 1 d . . . C2 C 0.6389(7) -0.1026(2) 0.15422(14) 0.0226(9) Uani 1 1 d . . . H2A H 0.7219 -0.1211 0.1261 0.027 Uiso 1 1 calc R . . H2B H 0.7663 -0.0766 0.1758 0.027 Uiso 1 1 calc R . . C3 C 0.5273(8) -0.1812(2) 0.17458(14) 0.0249(9) Uani 1 1 d . . . H3A H 0.4313 -0.1633 0.2013 0.030 Uiso 1 1 calc R . . H3B H 0.4137 -0.2117 0.1519 0.030 Uiso 1 1 calc R . . C4 C 0.7222(8) -0.2400(3) 0.18877(13) 0.0248(9) Uani 1 1 d . . . C5 C 0.2498(8) -0.0712(3) 0.11066(13) 0.0236(9) Uani 1 1 d . . . H5A H 0.1468 -0.1109 0.1274 0.028 Uiso 1 1 calc R . . H5B H 0.1452 -0.0243 0.1020 0.028 Uiso 1 1 calc R . . C6 C 0.3338(7) -0.1183(3) 0.06750(13) 0.0240(9) Uani 1 1 d . . . H6A H 0.4790 -0.0875 0.0563 0.029 Uiso 1 1 calc R . . H6B H 0.3849 -0.1757 0.0748 0.029 Uiso 1 1 calc R . . C7 C 0.1398(9) -0.1271(3) 0.03064(14) 0.0265(10) Uani 1 1 d . . . C8 C 0.6006(8) 0.0399(2) 0.12194(14) 0.0249(9) Uani 1 1 d . . . H8A H 0.7465 0.0555 0.1418 0.030 Uiso 1 1 calc R . . H8B H 0.6608 0.0184 0.0922 0.030 Uiso 1 1 calc R . . C9 C 0.4599(8) 0.1207(3) 0.11481(14) 0.0291(10) Uani 1 1 d . . . H9A H 0.3660 0.1337 0.1425 0.035 Uiso 1 1 calc R . . H9B H 0.5823 0.1680 0.1126 0.035 Uiso 1 1 calc R . . C10 C 0.2861(8) 0.1214(2) 0.07493(13) 0.0241(9) Uani 1 1 d . . . C11 C 0.4440(8) 0.0365(2) 0.22207(14) 0.0240(9) Uani 1 1 d . . . C12 C 0.2829(8) 0.0525(3) 0.26220(14) 0.0273(10) Uani 1 1 d . . . H12A H 0.2950 0.0044 0.2821 0.033 Uiso 1 1 calc R . . H12B H 0.1099 0.0543 0.2512 0.033 Uiso 1 1 calc R . . C13 C 0.3513(8) 0.1348(3) 0.28979(14) 0.0291(10) Uani 1 1 d . . . H13A H 0.3268 0.1833 0.2706 0.035 Uiso 1 1 calc R . . H13B H 0.5275 0.1349 0.2989 0.035 Uiso 1 1 calc R . . C14 C 0.1994(8) 0.1468(3) 0.33214(14) 0.0308(10) Uani 1 1 d . . . H14A H 0.2163 0.0966 0.3504 0.037 Uiso 1 1 calc R . . H14B H 0.0241 0.1499 0.3229 0.037 Uiso 1 1 calc R . . C15 C 0.2766(9) 0.2270(3) 0.36159(13) 0.0310(10) Uani 1 1 d . . . H15A H 0.4557 0.2264 0.3681 0.037 Uiso 1 1 calc R . . H15B H 0.2449 0.2773 0.3441 0.037 Uiso 1 1 calc R . . C16 C 0.1461(9) 0.2370(3) 0.40635(15) 0.0341(11) Uani 1 1 d . . . H16A H 0.1703 0.1857 0.4234 0.041 Uiso 1 1 calc R . . H16B H -0.0323 0.2413 0.4000 0.041 Uiso 1 1 calc R . . C17 C 0.2395(9) 0.3156(3) 0.43570(14) 0.0318(10) Uani 1 1 d . . . H17A H 0.4195 0.3124 0.4403 0.038 Uiso 1 1 calc R . . H17B H 0.2083 0.3668 0.4189 0.038 Uiso 1 1 calc R . . C18 C 0.1246(9) 0.3268(3) 0.48200(14) 0.0315(11) Uani 1 1 d . . . H18A H 0.1500 0.2751 0.4987 0.038 Uiso 1 1 calc R . . H18B H -0.0546 0.3331 0.4777 0.038 Uiso 1 1 calc R . . C19 C 0.2327(9) 0.4041(3) 0.51033(14) 0.0317(11) Uani 1 1 d . . . H19A H 0.4123 0.3978 0.5138 0.038 Uiso 1 1 calc R . . H19B H 0.2062 0.4554 0.4933 0.038 Uiso 1 1 calc R . . C20 C 0.1286(9) 0.4187(3) 0.55717(14) 0.0320(11) Uani 1 1 d . . . H20A H 0.1506 0.3672 0.5742 0.038 Uiso 1 1 calc R . . H20B H -0.0499 0.4277 0.5540 0.038 Uiso 1 1 calc R . . C21 C 0.2509(9) 0.4948(3) 0.58390(14) 0.0317(11) Uani 1 1 d . . . H21A H 0.2296 0.5457 0.5663 0.038 Uiso 1 1 calc R . . H21B H 0.4293 0.4853 0.5865 0.038 Uiso 1 1 calc R . . C22 C 0.1563(9) 0.5139(3) 0.63142(14) 0.0302(10) Uani 1 1 d . . . H22A H -0.0221 0.5237 0.6292 0.036 Uiso 1 1 calc R . . H22B H 0.1800 0.4639 0.6496 0.036 Uiso 1 1 calc R . . C23 C 0.2857(10) 0.5911(3) 0.65555(14) 0.0370(12) Uani 1 1 d . . . H23A H 0.2641 0.6404 0.6368 0.044 Uiso 1 1 calc R . . H23B H 0.4637 0.5807 0.6577 0.044 Uiso 1 1 calc R . . C24 C 0.1976(11) 0.6143(3) 0.70294(15) 0.0467(14) Uani 1 1 d . . . H24A H 0.2904 0.6649 0.7159 0.070 Uiso 1 1 calc R . . H24B H 0.2233 0.5668 0.7222 0.070 Uiso 1 1 calc R . . H24C H 0.0224 0.6263 0.7013 0.070 Uiso 1 1 calc R . . C25 C 0.0959(7) 0.4692(2) 0.14522(13) 0.0214(9) Uani 1 1 d . . . C26 C -0.0538(8) 0.5381(2) 0.12226(13) 0.0246(9) Uani 1 1 d . . . H26A H -0.1227 0.5130 0.0929 0.030 Uiso 1 1 calc R . . H26B H -0.1937 0.5525 0.1416 0.030 Uiso 1 1 calc R . . C27 C 0.0877(8) 0.6206(2) 0.11356(14) 0.0277(10) Uani 1 1 d . . . H27A H -0.0327 0.6658 0.1108 0.033 Uiso 1 1 calc R . . H27B H 0.1939 0.6367 0.1407 0.033 Uiso 1 1 calc R . . C28 C 0.2459(8) 0.6203(2) 0.07269(13) 0.0253(10) Uani 1 1 d . . . C29 C 0.2957(7) 0.4337(2) 0.11380(13) 0.0210(9) Uani 1 1 d . . . H29A H 0.3989 0.4818 0.1042 0.025 Uiso 1 1 calc R . . H29B H 0.4027 0.3972 0.1313 0.025 Uiso 1 1 calc R . . C30 C 0.1946(8) 0.3822(3) 0.07177(13) 0.0244(9) Uani 1 1 d . . . H30A H 0.1455 0.3244 0.0803 0.029 Uiso 1 1 calc R . . H30B H 0.0455 0.4093 0.0603 0.029 Uiso 1 1 calc R . . C31 C 0.3755(8) 0.3749(3) 0.03431(13) 0.0227(9) Uani 1 1 d . . . C32 C -0.0817(7) 0.3978(2) 0.15783(13) 0.0219(9) Uani 1 1 d . . . H32A H -0.2021 0.4225 0.1789 0.026 Uiso 1 1 calc R . . H32B H -0.1737 0.3757 0.1299 0.026 Uiso 1 1 calc R . . C33 C 0.0337(8) 0.3236(2) 0.17962(15) 0.0267(10) Uani 1 1 d . . . H33A H 0.1439 0.2951 0.1578 0.032 Uiso 1 1 calc R . . H33B H 0.1346 0.3452 0.2066 0.032 Uiso 1 1 calc R . . C34 C -0.1558(9) 0.2599(3) 0.19382(14) 0.0272(10) Uani 1 1 d . . . C35 C 0.1244(8) 0.5444(2) 0.22340(13) 0.0218(9) Uani 1 1 d . . . C36 C 0.2927(8) 0.5645(3) 0.26506(13) 0.0252(9) Uani 1 1 d . . . H36A H 0.4643 0.5710 0.2553 0.030 Uiso 1 1 calc R . . H36B H 0.2840 0.5163 0.2850 0.030 Uiso 1 1 calc R . . C37 C 0.2231(8) 0.6464(2) 0.29220(13) 0.0238(9) Uani 1 1 d . . . H37A H 0.2520 0.6956 0.2736 0.029 Uiso 1 1 calc R . . H37B H 0.0458 0.6429 0.2986 0.029 Uiso 1 1 calc R . . C38 C 0.3692(8) 0.6608(3) 0.33672(14) 0.0288(10) Uani 1 1 d . . . H38A H 0.5443 0.6720 0.3303 0.035 Uiso 1 1 calc R . . H38B H 0.3578 0.6087 0.3538 0.035 Uiso 1 1 calc R . . C39 C 0.2747(8) 0.7356(3) 0.36570(13) 0.0275(10) Uani 1 1 d . . . H39A H 0.0962 0.7259 0.3695 0.033 Uiso 1 1 calc R . . H39B H 0.2968 0.7878 0.3490 0.033 Uiso 1 1 calc R . . C40 C 0.3985(8) 0.7512(3) 0.41292(14) 0.0304(10) Uani 1 1 d . . . H40A H 0.5750 0.7656 0.4096 0.037 Uiso 1 1 calc R . . H40B H 0.3856 0.6984 0.4294 0.037 Uiso 1 1 calc R . . C41 C 0.2794(9) 0.8237(3) 0.44067(13) 0.0296(10) Uani 1 1 d . . . H41A H 0.2954 0.8763 0.4241 0.035 Uiso 1 1 calc R . . H41B H 0.1019 0.8096 0.4428 0.035 Uiso 1 1 calc R . . C42 C 0.3890(8) 0.8416(3) 0.48860(13) 0.0294(10) Uani 1 1 d . . . H42A H 0.5650 0.8583 0.4868 0.035 Uiso 1 1 calc R . . H42B H 0.3775 0.7890 0.5052 0.035 Uiso 1 1 calc R . . C43 C 0.2569(8) 0.9124(3) 0.51491(13) 0.0281(10) Uani 1 1 d . . . H43A H 0.2686 0.9646 0.4979 0.034 Uiso 1 1 calc R . . H43B H 0.0808 0.8955 0.5161 0.034 Uiso 1 1 calc R . . C44 C 0.3562(8) 0.9334(3) 0.56313(13) 0.0292(10) Uani 1 1 d . . . H44A H 0.3467 0.8813 0.5802 0.035 Uiso 1 1 calc R . . H44B H 0.5312 0.9518 0.5622 0.035 Uiso 1 1 calc R . . C45 C 0.2158(8) 1.0027(3) 0.58791(13) 0.0279(10) Uani 1 1 d . . . H45A H 0.0409 0.9839 0.5884 0.033 Uiso 1 1 calc R . . H45B H 0.2248 1.0542 0.5703 0.033 Uiso 1 1 calc R . . C46 C 0.3056(8) 1.0271(3) 0.63647(13) 0.0275(10) Uani 1 1 d . . . H46A H 0.2935 0.9764 0.6545 0.033 Uiso 1 1 calc R . . H46B H 0.4807 1.0459 0.6363 0.033 Uiso 1 1 calc R . . C47 C 0.1595(9) 1.0976(3) 0.65890(14) 0.0349(11) Uani 1 1 d . . . H47A H 0.1684 1.1474 0.6401 0.042 Uiso 1 1 calc R . . H47B H -0.0148 1.0779 0.6592 0.042 Uiso 1 1 calc R . . C48 C 0.2434(10) 1.1260(3) 0.70701(15) 0.0402(12) Uani 1 1 d . . . H48A H 0.1396 1.1715 0.7187 0.060 Uiso 1 1 calc R . . H48B H 0.4146 1.1472 0.7071 0.060 Uiso 1 1 calc R . . H48C H 0.2304 1.0777 0.7263 0.060 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 0.0230(17) 0.0301(17) 0.0359(18) 0.0047(13) 0.0046(14) 0.0013(13) O2 0.0341(18) 0.0238(16) 0.048(2) 0.0137(14) 0.0077(16) 0.0036(14) O3 0.0304(17) 0.0347(17) 0.0229(16) 0.0000(13) 0.0007(13) 0.0064(15) O4 0.044(2) 0.0283(16) 0.0274(16) -0.0085(13) -0.0030(15) 0.0072(15) O5 0.0368(18) 0.0276(16) 0.0275(16) -0.0015(12) -0.0028(14) 0.0073(15) O6 0.0391(19) 0.0267(16) 0.0188(15) 0.0027(12) 0.0002(13) 0.0056(14) O7 0.0285(17) 0.0252(15) 0.0276(16) 0.0046(12) 0.0000(13) -0.0031(13) O8 0.0391(18) 0.0239(16) 0.0251(16) 0.0008(12) 0.0072(14) -0.0068(14) O9 0.0387(18) 0.0259(16) 0.0175(14) 0.0003(12) 0.0067(13) 0.0003(14) O10 0.0330(18) 0.0303(16) 0.0240(16) -0.0020(12) 0.0024(13) -0.0052(14) O11 0.0433(19) 0.0324(17) 0.0247(16) -0.0084(13) 0.0078(14) -0.0078(15) O12 0.0277(18) 0.0288(17) 0.0377(18) 0.0057(13) 0.0025(14) -0.0018(14) O13 0.0329(18) 0.0252(17) 0.056(2) 0.0187(15) -0.0024(16) -0.0028(14) O14 0.0343(18) 0.0228(15) 0.0246(15) 0.0066(12) 0.0065(13) 0.0061(13) N1 0.0220(18) 0.0243(18) 0.0191(17) 0.0025(14) 0.0021(15) -0.0012(15) N2 0.0216(18) 0.0240(18) 0.0175(17) 0.0008(13) 0.0054(14) 0.0001(15) C1 0.024(2) 0.022(2) 0.024(2) 0.0014(17) 0.0027(18) 0.0027(18) C2 0.021(2) 0.019(2) 0.028(2) 0.0061(17) 0.0058(18) 0.0036(17) C3 0.027(2) 0.023(2) 0.025(2) 0.0073(17) 0.0022(19) -0.0006(18) C4 0.031(3) 0.024(2) 0.020(2) 0.0033(17) 0.0057(18) 0.0030(19) C5 0.026(2) 0.021(2) 0.024(2) 0.0064(16) 0.0024(18) -0.0026(18) C6 0.022(2) 0.023(2) 0.027(2) 0.0033(17) 0.0028(18) 0.0013(18) C7 0.036(3) 0.019(2) 0.025(2) 0.0043(17) 0.008(2) -0.003(2) C8 0.031(2) 0.019(2) 0.025(2) 0.0052(16) 0.0013(19) -0.0031(18) C9 0.040(3) 0.023(2) 0.025(2) 0.0054(17) 0.000(2) 0.000(2) C10 0.032(2) 0.018(2) 0.022(2) 0.0021(16) 0.0047(19) -0.0026(19) C11 0.030(2) 0.020(2) 0.023(2) 0.0081(17) -0.0009(19) 0.0021(19) C12 0.030(2) 0.026(2) 0.026(2) 0.0036(17) 0.0038(19) -0.0034(19) C13 0.036(3) 0.027(2) 0.025(2) 0.0042(18) 0.001(2) -0.001(2) C14 0.034(3) 0.028(2) 0.029(2) -0.0001(18) 0.003(2) -0.002(2) C15 0.043(3) 0.030(2) 0.020(2) 0.0011(18) 0.001(2) -0.004(2) C16 0.042(3) 0.031(2) 0.028(2) 0.0018(19) 0.002(2) 0.003(2) C17 0.041(3) 0.030(2) 0.025(2) 0.0019(18) 0.006(2) 0.003(2) C18 0.039(3) 0.031(2) 0.026(2) 0.0049(18) 0.006(2) 0.003(2) C19 0.041(3) 0.031(2) 0.024(2) 0.0044(18) 0.001(2) 0.003(2) C20 0.040(3) 0.031(2) 0.026(2) 0.0072(18) 0.006(2) 0.000(2) C21 0.045(3) 0.027(2) 0.024(2) 0.0072(18) 0.004(2) 0.002(2) C22 0.042(3) 0.023(2) 0.026(2) 0.0061(18) 0.004(2) -0.001(2) C23 0.055(3) 0.033(3) 0.023(2) 0.0045(19) 0.007(2) 0.000(2) C24 0.077(4) 0.038(3) 0.025(2) 0.003(2) 0.009(3) -0.005(3) C25 0.024(2) 0.020(2) 0.020(2) -0.0002(16) 0.0011(17) -0.0001(17) C26 0.032(2) 0.022(2) 0.020(2) 0.0030(16) 0.0018(19) 0.0058(19) C27 0.041(3) 0.017(2) 0.025(2) -0.0006(17) 0.004(2) 0.0031(19) C28 0.038(3) 0.020(2) 0.019(2) 0.0019(16) 0.0031(19) 0.006(2) C29 0.022(2) 0.022(2) 0.020(2) 0.0044(16) 0.0039(17) 0.0034(17) C30 0.026(2) 0.023(2) 0.024(2) -0.0021(17) 0.0047(18) 0.0022(18) C31 0.031(2) 0.022(2) 0.015(2) 0.0000(16) -0.0011(18) 0.0075(19) C32 0.025(2) 0.019(2) 0.022(2) 0.0010(16) 0.0055(18) 0.0025(17) C33 0.027(2) 0.020(2) 0.033(2) 0.0045(17) 0.001(2) -0.0002(18) C34 0.036(3) 0.021(2) 0.025(2) 0.0023(17) 0.003(2) -0.001(2) C35 0.028(2) 0.020(2) 0.018(2) 0.0051(16) 0.0037(18) 0.0037(18) C36 0.030(2) 0.025(2) 0.020(2) 0.0017(17) -0.0011(18) 0.0016(19) C37 0.027(2) 0.023(2) 0.023(2) 0.0007(17) 0.0030(18) 0.0054(18) C38 0.033(3) 0.030(2) 0.023(2) 0.0006(18) 0.0000(19) -0.002(2) C39 0.039(3) 0.026(2) 0.018(2) 0.0012(17) 0.0014(19) -0.001(2) C40 0.038(3) 0.029(2) 0.024(2) -0.0036(18) -0.002(2) -0.003(2) C41 0.040(3) 0.028(2) 0.020(2) 0.0011(18) 0.002(2) -0.001(2) C42 0.037(3) 0.031(2) 0.020(2) -0.0005(18) 0.0046(19) 0.000(2) C43 0.038(3) 0.027(2) 0.019(2) -0.0001(17) 0.0009(19) 0.004(2) C44 0.041(3) 0.028(2) 0.019(2) 0.0002(17) -0.001(2) 0.001(2) C45 0.035(3) 0.027(2) 0.023(2) 0.0027(18) 0.0003(19) 0.002(2) C46 0.036(3) 0.026(2) 0.020(2) 0.0033(17) -0.0013(19) 0.003(2) C47 0.051(3) 0.032(2) 0.023(2) 0.0048(18) 0.002(2) 0.004(2) C48 0.060(3) 0.034(3) 0.026(2) -0.0020(19) -0.002(2) 0.001(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 C4 1.201(5) . ? O2 C4 1.349(5) . ? O3 C7 1.232(5) . ? O4 C7 1.321(5) . ? O5 C10 1.221(5) . ? O6 C10 1.333(5) . ? O7 C11 1.238(5) . ? O8 C28 1.218(5) . ? O9 C28 1.327(5) . ? O10 C31 1.226(5) . ? O11 C31 1.324(5) . ? O12 C34 1.203(5) . ? O13 C34 1.341(5) . ? O14 C35 1.240(5) . ? N1 C11 1.348(5) . ? N1 C1 1.484(5) . ? N2 C35 1.355(5) . ? N2 C25 1.482(5) . ? C1 C5 1.533(5) . ? C1 C2 1.538(5) . ? C1 C8 1.549(5) . ? C2 C3 1.525(5) . ? C3 C4 1.501(6) . ? C5 C6 1.524(5) . ? C6 C7 1.492(6) . ? C8 C9 1.531(5) . ? C9 C10 1.491(6) . ? C11 C12 1.508(6) . ? C12 C13 1.518(6) . ? C13 C14 1.524(6) . ? C14 C15 1.529(6) . ? C15 C16 1.520(6) . ? C16 C17 1.531(6) . ? C17 C18 1.522(6) . ? C18 C19 1.525(6) . ? C19 C20 1.517(6) . ? C20 C21 1.518(6) . ? C21 C22 1.525(6) . ? C22 C23 1.514(6) . ? C23 C24 1.519(6) . ? C25 C32 1.530(5) . ? C25 C29 1.547(5) . ? C25 C26 1.556(5) . ? C26 C27 1.528(6) . ? C27 C28 1.502(6) . ? C29 C30 1.519(5) . ? C30 C31 1.504(6) . ? C32 C33 1.515(5) . ? C33 C34 1.503(6) . ? C35 C36 1.524(5) . ? C36 C37 1.539(5) . ? C37 C38 1.518(6) . ? C38 C39 1.525(6) . ? C39 C40 1.534(5) . ? C40 C41 1.537(6) . ? C41 C42 1.526(6) . ? C42 C43 1.531(6) . ? C43 C44 1.521(5) . ? C44 C45 1.517(6) . ? C45 C46 1.524(5) . ? C46 C47 1.517(6) . ? C47 C48 1.516(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 N1 C1 126.4(3) . . ? C35 N2 C25 125.8(3) . . ? N1 C1 C5 105.3(3) . . ? N1 C1 C2 109.8(3) . . ? C5 C1 C2 110.8(3) . . ? N1 C1 C8 110.7(3) . . ? C5 C1 C8 111.6(3) . . ? C2 C1 C8 108.5(3) . . ? C3 C2 C1 115.6(3) . . ? C4 C3 C2 111.4(3) . . ? O1 C4 O2 123.2(4) . . ? O1 C4 C3 126.2(4) . . ? O2 C4 C3 110.6(4) . . ? C6 C5 C1 115.1(3) . . ? C7 C6 C5 113.2(3) . . ? O3 C7 O4 122.9(4) . . ? O3 C7 C6 123.8(4) . . ? O4 C7 C6 113.3(4) . . ? C9 C8 C1 116.6(4) . . ? C10 C9 C8 118.5(3) . . ? O5 C10 O6 123.0(4) . . ? O5 C10 C9 122.8(4) . . ? O6 C10 C9 114.2(4) . . ? O7 C11 N1 122.0(4) . . ? O7 C11 C12 121.8(4) . . ? N1 C11 C12 116.2(4) . . ? C11 C12 C13 113.1(4) . . ? C12 C13 C14 112.4(4) . . ? C13 C14 C15 112.9(4) . . ? C16 C15 C14 114.5(4) . . ? C15 C16 C17 112.5(4) . . ? C18 C17 C16 115.1(4) . . ? C17 C18 C19 112.5(4) . . ? C20 C19 C18 115.4(4) . . ? C19 C20 C21 112.4(4) . . ? C20 C21 C22 115.7(4) . . ? C23 C22 C21 112.4(4) . . ? C22 C23 C24 115.1(4) . . ? N2 C25 C32 109.3(3) . . ? N2 C25 C29 105.8(3) . . ? C32 C25 C29 110.6(3) . . ? N2 C25 C26 110.9(3) . . ? C32 C25 C26 108.7(3) . . ? C29 C25 C26 111.5(3) . . ? C27 C26 C25 116.0(3) . . ? C28 C27 C26 117.6(3) . . ? O8 C28 O9 123.9(4) . . ? O8 C28 C27 122.1(4) . . ? O9 C28 C27 113.9(4) . . ? C30 C29 C25 114.1(3) . . ? C31 C30 C29 113.2(3) . . ? O10 C31 O11 123.5(4) . . ? O10 C31 C30 124.2(4) . . ? O11 C31 C30 112.3(4) . . ? C33 C32 C25 116.0(3) . . ? C34 C33 C32 112.1(3) . . ? O12 C34 O13 123.8(4) . . ? O12 C34 C33 124.9(4) . . ? O13 C34 C33 111.3(4) . . ? O14 C35 N2 122.4(4) . . ? O14 C35 C36 121.4(4) . . ? N2 C35 C36 116.2(4) . . ? C35 C36 C37 112.3(3) . . ? C38 C37 C36 112.5(3) . . ? C37 C38 C39 111.5(3) . . ? C38 C39 C40 115.4(4) . . ? C39 C40 C41 111.5(4) . . ? C42 C41 C40 114.6(4) . . ? C41 C42 C43 111.9(4) . . ? C44 C43 C42 114.8(4) . . ? C45 C44 C43 112.6(4) . . ? C44 C45 C46 115.4(3) . . ? C47 C46 C45 112.6(3) . . ? C48 C47 C46 115.1(4) . . ? 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 C11 N1 C1 C5 -178.6(3) . . . . ? C11 N1 C1 C2 62.1(5) . . . . ? C11 N1 C1 C8 -57.8(5) . . . . ? N1 C1 C2 C3 59.7(4) . . . . ? C5 C1 C2 C3 -56.2(5) . . . . ? C8 C1 C2 C3 -179.1(3) . . . . ? C1 C2 C3 C4 -174.2(3) . . . . ? C2 C3 C4 O1 3.3(6) . . . . ? C2 C3 C4 O2 -176.6(3) . . . . ? N1 C1 C5 C6 -172.0(3) . . . . ? C2 C1 C5 C6 -53.3(4) . . . . ? C8 C1 C5 C6 67.8(4) . . . . ? C1 C5 C6 C7 -160.0(3) . . . . ? C5 C6 C7 O3 12.0(6) . . . . ? C5 C6 C7 O4 -168.7(3) . . . . ? N1 C1 C8 C9 -50.5(5) . . . . ? C5 C1 C8 C9 66.5(5) . . . . ? C2 C1 C8 C9 -171.1(3) . . . . ? C1 C8 C9 C10 -78.4(5) . . . . ? C8 C9 C10 O5 151.3(4) . . . . ? C8 C9 C10 O6 -31.7(5) . . . . ? C1 N1 C11 O7 4.2(6) . . . . ? C1 N1 C11 C12 -172.9(3) . . . . ? O7 C11 C12 C13 37.2(5) . . . . ? N1 C11 C12 C13 -145.7(4) . . . . ? C11 C12 C13 C14 -175.7(3) . . . . ? C12 C13 C14 C15 176.8(4) . . . . ? C13 C14 C15 C16 -174.5(4) . . . . ? C14 C15 C16 C17 176.9(4) . . . . ? C15 C16 C17 C18 -177.2(4) . . . . ? C16 C17 C18 C19 177.6(4) . . . . ? C17 C18 C19 C20 -179.4(3) . . . . ? C18 C19 C20 C21 178.1(4) . . . . ? C19 C20 C21 C22 179.9(3) . . . . ? C20 C21 C22 C23 -179.4(4) . . . . ? C21 C22 C23 C24 179.3(4) . . . . ? C35 N2 C25 C32 -61.2(5) . . . . ? C35 N2 C25 C29 179.7(3) . . . . ? C35 N2 C25 C26 58.6(5) . . . . ? N2 C25 C26 C27 51.3(5) . . . . ? C32 C25 C26 C27 171.4(3) . . . . ? C29 C25 C26 C27 -66.4(4) . . . . ? C25 C26 C27 C28 79.9(5) . . . . ? C26 C27 C28 O8 -150.1(4) . . . . ? C26 C27 C28 O9 33.3(5) . . . . ? N2 C25 C29 C30 172.0(3) . . . . ? C32 C25 C29 C30 53.7(4) . . . . ? C26 C25 C29 C30 -67.3(4) . . . . ? C25 C29 C30 C31 159.4(3) . . . . ? C29 C30 C31 O10 -11.3(6) . . . . ? C29 C30 C31 O11 171.4(3) . . . . ? N2 C25 C32 C33 -60.4(4) . . . . ? C29 C25 C32 C33 55.7(4) . . . . ? C26 C25 C32 C33 178.5(3) . . . . ? C25 C32 C33 C34 175.9(3) . . . . ? C32 C33 C34 O12 -5.0(6) . . . . ? C32 C33 C34 O13 174.3(3) . . . . ? C25 N2 C35 O14 -6.4(6) . . . . ? C25 N2 C35 C36 170.6(3) . . . . ? O14 C35 C36 C37 -35.8(5) . . . . ? N2 C35 C36 C37 147.1(3) . . . . ? C35 C36 C37 C38 172.9(3) . . . . ? C36 C37 C38 C39 -172.7(3) . . . . ? C37 C38 C39 C40 175.7(3) . . . . ? C38 C39 C40 C41 -176.2(4) . . . . ? C39 C40 C41 C42 178.6(3) . . . . ? C40 C41 C42 C43 -178.1(4) . . . . ? C41 C42 C43 C44 179.8(4) . . . . ? C42 C43 C44 C45 -179.0(4) . . . . ? C43 C44 C45 C46 -179.9(4) . . . . ? C44 C45 C46 C47 179.2(4) . . . . ? C45 C46 C47 C48 -178.8(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 O2 H2C O14 0.84 1.86 2.676(4) 164.8 1_645 O4 H4A O5 0.84 1.82 2.656(4) 171.5 2 O6 H6C O3 0.84 1.79 2.628(4) 175.0 2 O9 H9C O10 0.84 1.80 2.636(4) 176.0 2_665 O11 H11A O8 0.84 1.81 2.645(4) 170.8 2_665 O13 H13C O7 0.84 1.84 2.660(4) 166.4 1_455 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.697 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.119