# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1838 data_global _publ_contact_author_name 'Martin Lutz' _publ_contact_author_address ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; _publ_contact_author_email 'm.lutz@chem.uu.nl' _publ_contact_author_fax '[+31] 30 2533940' _publ_contact_author_phone '[+31] 30 2533902' loop_ _publ_author_name _publ_author_address 'Parlevliet, Floris J.' ; Institute of Molecular Chemistry University of Amsterdam Department of Inorganic Chemistry and Homogeneous Catalysis Nieuwe Achtergracht 166 1018 WV Amsterdam The Netherlands ; 'Kiener, Christoph' ; Institute of Molecular Chemistry University of Amsterdam Department of Inorganic Chemistry and Homogeneous Catalysis Nieuwe Achtergracht 166 1018 WV Amsterdam The Netherlands ; 'Fraanje, Jan' ; Institute of Molecular Chemistry University of Amsterdam Department of Crystallography Nieuwe Achtergracht 166 1018 WV Amsterdam The Netherlands ; 'Goubitz, Kees' ; Institute of Molecular Chemistry University of Amsterdam Department of Crystallography Nieuwe Achtergracht 166 1018 WV Amsterdam The Netherlands ; 'Lutz, Martin' ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Spek, Anthony L.' ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Kamer, Paul C.J.' ; Institute of Molecular Chemistry University of Amsterdam Department of Inorganic Chemistry and Homogeneous Catalysis Nieuwe Achtergracht 166 1018 WV Amsterdam The Netherlands ; 'van Leeuwen, Piet W.N.M.' ; Institute of Molecular Chemistry University of Amsterdam Department of Inorganic Chemistry and Homogeneous Catalysis Nieuwe Achtergracht 166 1018 WV Amsterdam The Netherlands ; _publ_section_title ; Calix[4]arene based monophosphites, identification of three conformations and their use in the rhodium-catalysed hydroformylation of 1-octene ; _journal_coden_Cambridge 186 data_s1833c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H59 O4 P, C7 H8' _chemical_formula_sum 'C58 H67 O4 P' _chemical_formula_weight 859.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 17.900(3) _cell_length_b 21.4197(19) _cell_length_c 24.477(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9384.9(18) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3696 _exptl_absorpt_coefficient_mu 0.106 _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 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4T' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 1.5 _diffrn_reflns_number 8602 _diffrn_reflns_av_R_equivalents 0.1099 _diffrn_reflns_av_sigmaI/netI 0.1452 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 20.03 _reflns_number_total 4389 _reflns_number_gt 2374 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Locally modified CAD4-Version 5 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)' _computing_data_reduction 'HELENA (Spek, 1997)' _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1998)' _computing_publication_material 'PLATON (Spek, 1998)' _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^)+(0.0695P)^2^+2.6138P] 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 constraint _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4389 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1543 _refine_ls_R_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.1798 _refine_ls_wR_factor_gt 0.1487 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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_multiplicit _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.61944(11) 0.58297(9) 0.27314(8) 0.0177(5) Uiso 1 1 d . . . O1 O 0.5159(3) 0.4609(2) 0.34632(18) 0.0198(13) Uiso 1 1 d . . . O2 O 0.5541(2) 0.5982(2) 0.31819(18) 0.0157(12) Uiso 1 1 d . . . O3 O 0.6202(2) 0.6484(2) 0.23828(18) 0.0189(12) Uiso 1 1 d . . . O4 O 0.5591(2) 0.5417(2) 0.23837(17) 0.0144(12) Uiso 1 1 d . . . C1 C 0.6275(4) 0.4376(3) 0.2963(3) 0.0162(19) Uiso 1 1 d . . . C2 C 0.5804(4) 0.4103(3) 0.2504(3) 0.0177(18) Uiso 1 1 d . . . H1 H 0.5956 0.3663 0.2448 0.021 Uiso 1 1 calc R . . H2 H 0.5275 0.4100 0.2622 0.021 Uiso 1 1 calc R . . C3 C 0.5854(4) 0.4442(3) 0.1958(3) 0.0142(19) Uiso 1 1 d . . . C4 C 0.5950(4) 0.4097(3) 0.1484(3) 0.0170(19) Uiso 1 1 d . . . H3 H 0.5991 0.3656 0.1510 0.020 Uiso 1 1 calc R . . C5 C 0.5987(4) 0.4375(3) 0.0969(3) 0.0147(19) Uiso 1 1 d . . . C6 C 0.5919(4) 0.5019(3) 0.0955(3) 0.020(2) Uiso 1 1 d . . . H4 H 0.5948 0.5220 0.0609 0.024 Uiso 1 1 calc R . . C7 C 0.5810(4) 0.5391(3) 0.1412(3) 0.0163(19) Uiso 1 1 d . . . C8 C 0.5747(4) 0.6085(3) 0.1336(3) 0.019(2) Uiso 1 1 d . . . H5 H 0.5586 0.6159 0.0955 0.023 Uiso 1 1 calc R . . H6 H 0.6257 0.6261 0.1371 0.023 Uiso 1 1 calc R . . C9 C 0.5243(4) 0.6465(3) 0.1699(3) 0.0166(19) Uiso 1 1 d . . . C10 C 0.4525(4) 0.6649(3) 0.1539(3) 0.0184(19) Uiso 1 1 d . . . H7 H 0.4344 0.6515 0.1194 0.022 Uiso 1 1 calc R . . C11 C 0.4063(4) 0.7022(3) 0.1865(3) 0.0163(19) Uiso 1 1 d . . . C12 C 0.4361(4) 0.7228(3) 0.2366(3) 0.0162(19) Uiso 1 1 d . . . H8 H 0.4061 0.7486 0.2594 0.019 Uiso 1 1 calc R . . C13 C 0.5076(4) 0.7070(3) 0.2542(3) 0.0160(18) Uiso 1 1 d . . . C14 C 0.5424(4) 0.7375(3) 0.3041(3) 0.021(2) Uiso 1 1 d . . . H9 H 0.5057 0.7688 0.3172 0.025 Uiso 1 1 calc R . . H10 H 0.5861 0.7613 0.2907 0.025 Uiso 1 1 calc R . . C15 C 0.5688(4) 0.7018(3) 0.3547(3) 0.020(2) Uiso 1 1 d . . . C16 C 0.5878(4) 0.7395(3) 0.3996(3) 0.0167(19) Uiso 1 1 d . . . H11 H 0.5843 0.7835 0.3958 0.020 Uiso 1 1 calc R . . C17 C 0.6116(4) 0.7150(3) 0.4490(3) 0.0132(18) Uiso 1 1 d . . . C18 C 0.6149(4) 0.6505(3) 0.4533(3) 0.0197(19) Uiso 1 1 d . . . H12 H 0.6306 0.6328 0.4870 0.024 Uiso 1 1 calc R . . C19 C 0.5963(4) 0.6104(3) 0.4108(3) 0.0139(19) Uiso 1 1 d . . . C20 C 0.5935(4) 0.5405(3) 0.4208(3) 0.023(2) Uiso 1 1 d . . . H13 H 0.5404 0.5275 0.4222 0.028 Uiso 1 1 calc R . . H14 H 0.6156 0.5320 0.4571 0.028 Uiso 1 1 calc R . . C21 C 0.6335(4) 0.4997(3) 0.3786(3) 0.0157(19) Uiso 1 1 d . . . C22 C 0.7109(4) 0.5000(3) 0.3750(3) 0.0166(19) Uiso 1 1 d . . . H15 H 0.7389 0.5230 0.4011 0.020 Uiso 1 1 calc R . . C23 C 0.7486(4) 0.4671(3) 0.3340(3) 0.0146(18) Uiso 1 1 d . . . C24 C 0.7053(4) 0.4389(3) 0.2938(3) 0.0151(19) Uiso 1 1 d . . . H16 H 0.7296 0.4198 0.2635 0.018 Uiso 1 1 calc R . . C25 C 0.5929(4) 0.4649(3) 0.3416(3) 0.0163(19) Uiso 1 1 d . . . C26 C 0.5740(4) 0.6379(3) 0.3612(3) 0.0147(18) Uiso 1 1 d . . . C27 C 0.5490(4) 0.6689(3) 0.2205(3) 0.0151(18) Uiso 1 1 d . . . C28 C 0.5779(4) 0.5080(3) 0.1915(3) 0.0147(19) Uiso 1 1 d . . . C29 C 0.4952(4) 0.4062(3) 0.3760(3) 0.027(2) Uiso 1 1 d . . . H17 H 0.4952 0.4154 0.4156 0.032 Uiso 1 1 calc R . . H18 H 0.5321 0.3727 0.3691 0.032 Uiso 1 1 calc R . . C30 C 0.4194(4) 0.3847(3) 0.3589(3) 0.0184(19) Uiso 1 1 d . . . C31 C 0.4092(4) 0.3267(3) 0.3367(3) 0.022(2) Uiso 1 1 d . . . H19 H 0.4510 0.3001 0.3312 0.027 Uiso 1 1 calc R . . C32 C 0.3387(4) 0.3064(4) 0.3223(3) 0.028(2) Uiso 1 1 d . . . H20 H 0.3318 0.2656 0.3079 0.034 Uiso 1 1 calc R . . C33 C 0.2794(4) 0.3449(4) 0.3286(3) 0.027(2) Uiso 1 1 d . . . H21 H 0.2311 0.3308 0.3185 0.032 Uiso 1 1 calc R . . C34 C 0.2876(4) 0.4040(4) 0.3495(3) 0.028(2) Uiso 1 1 d . . . H22 H 0.2456 0.4308 0.3532 0.034 Uiso 1 1 calc R . . C35 C 0.3582(4) 0.4242(4) 0.3652(3) 0.026(2) Uiso 1 1 d . . . H23 H 0.3647 0.4648 0.3802 0.031 Uiso 1 1 calc R . . C36 C 0.6105(4) 0.4005(3) 0.0441(3) 0.021(2) Uiso 1 1 d . . . C37 C 0.6865(4) 0.4187(4) 0.0184(3) 0.028(2) Uiso 1 1 d . . . H24 H 0.6941 0.3948 -0.0154 0.042 Uiso 1 1 calc R . . H25 H 0.7268 0.4093 0.0441 0.042 Uiso 1 1 calc R . . H26 H 0.6867 0.4634 0.0100 0.042 Uiso 1 1 calc R . . C38 C 0.6095(4) 0.3301(3) 0.0533(3) 0.031(2) Uiso 1 1 d . . . H27 H 0.6173 0.3087 0.0184 0.047 Uiso 1 1 calc R . . H28 H 0.5612 0.3178 0.0686 0.047 Uiso 1 1 calc R . . H29 H 0.6495 0.3187 0.0788 0.047 Uiso 1 1 calc R . . C39 C 0.5479(4) 0.4174(4) 0.0030(3) 0.029(2) Uiso 1 1 d . . . H30 H 0.5551 0.3937 -0.0308 0.044 Uiso 1 1 calc R . . H31 H 0.5499 0.4622 -0.0050 0.044 Uiso 1 1 calc R . . H32 H 0.4992 0.4070 0.0189 0.044 Uiso 1 1 calc R . . C40 C 0.3296(4) 0.7212(3) 0.1652(3) 0.0181(19) Uiso 1 1 d . . . C41 C 0.2821(4) 0.7511(4) 0.2098(3) 0.039(2) Uiso 1 1 d . . . H33 H 0.2762 0.7217 0.2401 0.059 Uiso 1 1 calc R . . H34 H 0.2329 0.7617 0.1949 0.059 Uiso 1 1 calc R . . H35 H 0.3068 0.7891 0.2229 0.059 Uiso 1 1 calc R . . C42 C 0.3379(5) 0.7675(4) 0.1185(3) 0.041(2) Uiso 1 1 d . . . H36 H 0.2883 0.7796 0.1051 0.062 Uiso 1 1 calc R . . H37 H 0.3663 0.7481 0.0887 0.062 Uiso 1 1 calc R . . H38 H 0.3645 0.8046 0.1314 0.062 Uiso 1 1 calc R . . C43 C 0.2865(4) 0.6648(4) 0.1450(3) 0.035(2) Uiso 1 1 d . . . H39 H 0.2806 0.6348 0.1749 0.053 Uiso 1 1 calc R . . H40 H 0.3138 0.6452 0.1148 0.053 Uiso 1 1 calc R . . H41 H 0.2371 0.6781 0.1321 0.053 Uiso 1 1 calc R . . C44 C 0.6307(4) 0.7569(4) 0.4980(3) 0.0217(19) Uiso 1 1 d . . . C45 C 0.7009(4) 0.7344(4) 0.5270(3) 0.035(2) Uiso 1 1 d . . . H42 H 0.6943 0.6909 0.5383 0.052 Uiso 1 1 calc R . . H43 H 0.7100 0.7604 0.5593 0.052 Uiso 1 1 calc R . . H44 H 0.7436 0.7375 0.5021 0.052 Uiso 1 1 calc R . . C46 C 0.5643(4) 0.7532(4) 0.5378(3) 0.032(2) Uiso 1 1 d . . . H45 H 0.5560 0.7096 0.5483 0.049 Uiso 1 1 calc R . . H46 H 0.5194 0.7696 0.5201 0.049 Uiso 1 1 calc R . . H47 H 0.5753 0.7780 0.5705 0.049 Uiso 1 1 calc R . . C47 C 0.6439(4) 0.8243(3) 0.4819(3) 0.028(2) Uiso 1 1 d . . . H48 H 0.5997 0.8404 0.4629 0.042 Uiso 1 1 calc R . . H49 H 0.6873 0.8267 0.4575 0.042 Uiso 1 1 calc R . . H50 H 0.6533 0.8493 0.5147 0.042 Uiso 1 1 calc R . . C48 C 0.8344(4) 0.4631(4) 0.3297(3) 0.022(2) Uiso 1 1 d . . . C49 C 0.8721(4) 0.4874(4) 0.3822(3) 0.030(2) Uiso 1 1 d . . . H51 H 0.8555 0.4624 0.4135 0.045 Uiso 1 1 calc R . . H52 H 0.8583 0.5311 0.3880 0.045 Uiso 1 1 calc R . . H53 H 0.9265 0.4840 0.3786 0.045 Uiso 1 1 calc R . . C50 C 0.8578(4) 0.3955(3) 0.3220(3) 0.033(2) Uiso 1 1 d . . . H54 H 0.8408 0.3707 0.3533 0.049 Uiso 1 1 calc R . . H55 H 0.9124 0.3931 0.3194 0.049 Uiso 1 1 calc R . . H56 H 0.8354 0.3790 0.2885 0.049 Uiso 1 1 calc R . . C51 C 0.8613(4) 0.5027(4) 0.2816(3) 0.031(2) Uiso 1 1 d . . . H57 H 0.8463 0.5462 0.2872 0.047 Uiso 1 1 calc R . . H58 H 0.8390 0.4870 0.2477 0.047 Uiso 1 1 calc R . . H59 H 0.9159 0.5002 0.2791 0.047 Uiso 1 1 calc R . . C52 C 0.1709(6) 0.1124(5) 0.3903(4) 0.063(3) Uiso 1 1 d . . . C53 C 0.2117(5) 0.0766(4) 0.4271(4) 0.048(3) Uiso 1 1 d . . . H60 H 0.2507 0.0506 0.4138 0.057 Uiso 1 1 calc R . . C54 C 0.1973(5) 0.0781(5) 0.4814(4) 0.059(3) Uiso 1 1 d . . . H61 H 0.2261 0.0534 0.5058 0.071 Uiso 1 1 calc R . . C55 C 0.1401(6) 0.1160(5) 0.5016(5) 0.083(4) Uiso 1 1 d . . . H62 H 0.1297 0.1177 0.5396 0.100 Uiso 1 1 calc R . . C56 C 0.1002(7) 0.1498(5) 0.4662(5) 0.087(4) Uiso 1 1 d . . . H63 H 0.0605 0.1751 0.4792 0.104 Uiso 1 1 calc R . . C57 C 0.1158(6) 0.1484(5) 0.4118(5) 0.083(4) Uiso 1 1 d . . . H64 H 0.0869 0.1737 0.3879 0.100 Uiso 1 1 calc R . . C58 C 0.1928(7) 0.1106(6) 0.3308(5) 0.117(5) Uiso 1 1 d . . . H65 H 0.2341 0.0811 0.3257 0.175 Uiso 1 1 calc R . . H66 H 0.2085 0.1523 0.3191 0.175 Uiso 1 1 calc R . . H67 H 0.1499 0.0972 0.3089 0.175 Uiso 1 1 calc R . . _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 P1 O4 1.634(5) . ? P1 O2 1.640(5) . ? P1 O3 1.640(5) . ? O1 C25 1.386(8) . ? O1 C29 1.427(8) . ? O2 C26 1.399(8) . ? O3 C27 1.417(8) . ? O4 C28 1.397(8) . ? C1 C24 1.395(9) . ? C1 C25 1.398(9) . ? C1 C2 1.523(9) . ? C2 C3 1.523(9) . ? C2 H1 0.9900 . ? C2 H2 0.9900 . ? C3 C28 1.378(9) . ? C3 C4 1.386(9) . ? C4 C5 1.394(9) . ? C4 H3 0.9500 . ? C5 C6 1.386(9) . ? C5 C36 1.530(9) . ? C6 C7 1.387(9) . ? C6 H4 0.9500 . ? C7 C28 1.400(9) . ? C7 C8 1.504(9) . ? C8 C9 1.506(9) . ? C8 H5 0.9900 . ? C8 H6 0.9900 . ? C9 C27 1.399(9) . ? C9 C10 1.400(9) . ? C10 C11 1.398(9) . ? C10 H7 0.9500 . ? C11 C12 1.410(9) . ? C11 C40 1.525(9) . ? C12 C13 1.392(9) . ? C12 H8 0.9500 . ? C13 C27 1.377(9) . ? C13 C14 1.518(9) . ? C14 C15 1.532(9) . ? C14 H9 0.9900 . ? C14 H10 0.9900 . ? C15 C26 1.380(9) . ? C15 C16 1.405(9) . ? C16 C17 1.385(9) . ? C16 H11 0.9500 . ? C17 C18 1.387(9) . ? C17 C44 1.536(10) . ? C18 C19 1.390(9) . ? C18 H12 0.9500 . ? C19 C26 1.407(9) . ? C19 C20 1.518(9) . ? C20 C21 1.529(9) . ? C20 H13 0.9900 . ? C20 H14 0.9900 . ? C21 C25 1.381(9) . ? C21 C22 1.388(9) . ? C22 C23 1.400(9) . ? C22 H15 0.9500 . ? C23 C24 1.392(9) . ? C23 C48 1.541(10) . ? C24 H16 0.9500 . ? C29 C30 1.492(9) . ? C29 H17 0.9900 . ? C29 H18 0.9900 . ? C30 C31 1.369(10) . ? C30 C35 1.394(9) . ? C31 C32 1.381(9) . ? C31 H19 0.9500 . ? C32 C33 1.353(9) . ? C32 H20 0.9500 . ? C33 C34 1.373(10) . ? C33 H21 0.9500 . ? C34 C35 1.390(10) . ? C34 H22 0.9500 . ? C35 H23 0.9500 . ? C36 C38 1.525(10) . ? C36 C39 1.548(10) . ? C36 C37 1.549(10) . ? C37 H24 0.9800 . ? C37 H25 0.9800 . ? C37 H26 0.9800 . ? C38 H27 0.9800 . ? C38 H28 0.9800 . ? C38 H29 0.9800 . ? C39 H30 0.9800 . ? C39 H31 0.9800 . ? C39 H32 0.9800 . ? C40 C43 1.515(10) . ? C40 C42 1.522(10) . ? C40 C41 1.523(10) . ? C41 H33 0.9800 . ? C41 H34 0.9800 . ? C41 H35 0.9800 . ? C42 H36 0.9800 . ? C42 H37 0.9800 . ? C42 H38 0.9800 . ? C43 H39 0.9800 . ? C43 H40 0.9800 . ? C43 H41 0.9800 . ? C44 C47 1.514(10) . ? C44 C45 1.522(10) . ? C44 C46 1.539(9) . ? C45 H42 0.9800 . ? C45 H43 0.9800 . ? C45 H44 0.9800 . ? C46 H45 0.9800 . ? C46 H46 0.9800 . ? C46 H47 0.9800 . ? C47 H48 0.9800 . ? C47 H49 0.9800 . ? C47 H50 0.9800 . ? C48 C50 1.519(10) . ? C48 C51 1.529(10) . ? C48 C49 1.544(10) . ? C49 H51 0.9800 . ? C49 H52 0.9800 . ? C49 H53 0.9800 . ? C50 H54 0.9800 . ? C50 H55 0.9800 . ? C50 H56 0.9800 . ? C51 H57 0.9800 . ? C51 H58 0.9800 . ? C51 H59 0.9800 . ? C52 C57 1.359(13) . ? C52 C53 1.388(12) . ? C52 C58 1.510(14) . ? C53 C54 1.355(12) . ? C53 H60 0.9500 . ? C54 C55 1.397(13) . ? C54 H61 0.9500 . ? C55 C56 1.335(14) . ? C55 H62 0.9500 . ? C56 C57 1.361(13) . ? C56 H63 0.9500 . ? C57 H64 0.9500 . ? C58 H65 0.9800 . ? C58 H66 0.9800 . ? C58 H67 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 P1 O2 89.2(2) . . ? O4 P1 O3 101.3(2) . . ? O2 P1 O3 100.7(2) . . ? C25 O1 C29 110.5(5) . . ? C26 O2 P1 116.4(4) . . ? C27 O3 P1 114.7(4) . . ? C28 O4 P1 123.2(4) . . ? C24 C1 C25 118.0(6) . . ? C24 C1 C2 121.9(6) . . ? C25 C1 C2 120.0(6) . . ? C3 C2 C1 115.5(6) . . ? C3 C2 H1 108.4 . . ? C1 C2 H1 108.4 . . ? C3 C2 H2 108.4 . . ? C1 C2 H2 108.4 . . ? H1 C2 H2 107.5 . . ? C28 C3 C4 118.5(7) . . ? C28 C3 C2 122.3(6) . . ? C4 C3 C2 119.2(6) . . ? C3 C4 C5 122.3(7) . . ? C3 C4 H3 118.8 . . ? C5 C4 H3 118.8 . . ? C6 C5 C4 116.4(7) . . ? C6 C5 C36 120.4(6) . . ? C4 C5 C36 123.2(6) . . ? C5 C6 C7 124.2(7) . . ? C5 C6 H4 117.9 . . ? C7 C6 H4 117.9 . . ? C6 C7 C28 116.3(7) . . ? C6 C7 C8 118.5(7) . . ? C28 C7 C8 125.2(7) . . ? C7 C8 C9 120.4(6) . . ? C7 C8 H5 107.2 . . ? C9 C8 H5 107.2 . . ? C7 C8 H6 107.2 . . ? C9 C8 H6 107.2 . . ? H5 C8 H6 106.9 . . ? C27 C9 C10 116.2(6) . . ? C27 C9 C8 121.2(6) . . ? C10 C9 C8 122.5(6) . . ? C11 C10 C9 123.0(7) . . ? C11 C10 H7 118.5 . . ? C9 C10 H7 118.5 . . ? C10 C11 C12 116.9(6) . . ? C10 C11 C40 119.4(6) . . ? C12 C11 C40 123.6(6) . . ? C13 C12 C11 122.7(6) . . ? C13 C12 H8 118.7 . . ? C11 C12 H8 118.7 . . ? C27 C13 C12 117.0(6) . . ? C27 C13 C14 121.1(6) . . ? C12 C13 C14 121.4(6) . . ? C13 C14 C15 124.3(6) . . ? C13 C14 H9 106.3 . . ? C15 C14 H9 106.3 . . ? C13 C14 H10 106.3 . . ? C15 C14 H10 106.3 . . ? H9 C14 H10 106.4 . . ? C26 C15 C16 117.6(7) . . ? C26 C15 C14 127.5(7) . . ? C16 C15 C14 114.8(6) . . ? C17 C16 C15 122.7(7) . . ? C17 C16 H11 118.7 . . ? C15 C16 H11 118.7 . . ? C16 C17 C18 117.1(6) . . ? C16 C17 C44 121.9(6) . . ? C18 C17 C44 120.9(6) . . ? C17 C18 C19 123.3(7) . . ? C17 C18 H12 118.4 . . ? C19 C18 H12 118.4 . . ? C18 C19 C26 117.1(6) . . ? C18 C19 C20 119.8(7) . . ? C26 C19 C20 122.9(6) . . ? C19 C20 C21 116.0(6) . . ? C19 C20 H13 108.3 . . ? C21 C20 H13 108.3 . . ? C19 C20 H14 108.3 . . ? C21 C20 H14 108.3 . . ? H13 C20 H14 107.4 . . ? C25 C21 C22 119.0(7) . . ? C25 C21 C20 120.4(6) . . ? C22 C21 C20 120.5(6) . . ? C21 C22 C23 121.7(7) . . ? C21 C22 H15 119.1 . . ? C23 C22 H15 119.1 . . ? C24 C23 C22 117.2(6) . . ? C24 C23 C48 118.8(6) . . ? C22 C23 C48 124.0(6) . . ? C23 C24 C1 122.2(7) . . ? C23 C24 H16 118.9 . . ? C1 C24 H16 118.9 . . ? C21 C25 O1 120.1(6) . . ? C21 C25 C1 120.9(6) . . ? O1 C25 C1 118.8(6) . . ? C15 C26 O2 120.0(6) . . ? C15 C26 C19 122.2(7) . . ? O2 C26 C19 117.8(6) . . ? C13 C27 C9 124.3(6) . . ? C13 C27 O3 119.0(6) . . ? C9 C27 O3 116.7(6) . . ? C3 C28 O4 118.3(6) . . ? C3 C28 C7 122.3(7) . . ? O4 C28 C7 119.1(6) . . ? O1 C29 C30 110.3(6) . . ? O1 C29 H17 109.6 . . ? C30 C29 H17 109.6 . . ? O1 C29 H18 109.6 . . ? C30 C29 H18 109.6 . . ? H17 C29 H18 108.1 . . ? C31 C30 C35 119.3(7) . . ? C31 C30 C29 120.9(7) . . ? C35 C30 C29 119.7(6) . . ? C30 C31 C32 120.6(7) . . ? C30 C31 H19 119.7 . . ? C32 C31 H19 119.7 . . ? C33 C32 C31 119.7(7) . . ? C33 C32 H20 120.1 . . ? C31 C32 H20 120.1 . . ? C32 C33 C34 121.4(8) . . ? C32 C33 H21 119.3 . . ? C34 C33 H21 119.3 . . ? C33 C34 C35 119.1(8) . . ? C33 C34 H22 120.4 . . ? C35 C34 H22 120.4 . . ? C34 C35 C30 119.7(7) . . ? C34 C35 H23 120.2 . . ? C30 C35 H23 120.2 . . ? C38 C36 C5 112.7(6) . . ? C38 C36 C39 108.6(6) . . ? C5 C36 C39 109.2(6) . . ? C38 C36 C37 108.6(6) . . ? C5 C36 C37 109.5(6) . . ? C39 C36 C37 108.2(6) . . ? C36 C37 H24 109.5 . . ? C36 C37 H25 109.5 . . ? H24 C37 H25 109.5 . . ? C36 C37 H26 109.5 . . ? H24 C37 H26 109.5 . . ? H25 C37 H26 109.5 . . ? C36 C38 H27 109.5 . . ? C36 C38 H28 109.5 . . ? H27 C38 H28 109.5 . . ? C36 C38 H29 109.5 . . ? H27 C38 H29 109.5 . . ? H28 C38 H29 109.5 . . ? C36 C39 H30 109.5 . . ? C36 C39 H31 109.5 . . ? H30 C39 H31 109.5 . . ? C36 C39 H32 109.5 . . ? H30 C39 H32 109.5 . . ? H31 C39 H32 109.5 . . ? C43 C40 C42 108.8(6) . . ? C43 C40 C41 106.6(6) . . ? C42 C40 C41 108.6(6) . . ? C43 C40 C11 111.0(6) . . ? C42 C40 C11 110.0(6) . . ? C41 C40 C11 111.8(6) . . ? C40 C41 H33 109.5 . . ? C40 C41 H34 109.5 . . ? H33 C41 H34 109.5 . . ? C40 C41 H35 109.5 . . ? H33 C41 H35 109.5 . . ? H34 C41 H35 109.5 . . ? C40 C42 H36 109.5 . . ? C40 C42 H37 109.5 . . ? H36 C42 H37 109.5 . . ? C40 C42 H38 109.5 . . ? H36 C42 H38 109.5 . . ? H37 C42 H38 109.5 . . ? C40 C43 H39 109.5 . . ? C40 C43 H40 109.5 . . ? H39 C43 H40 109.5 . . ? C40 C43 H41 109.5 . . ? H39 C43 H41 109.5 . . ? H40 C43 H41 109.5 . . ? C47 C44 C45 107.1(6) . . ? C47 C44 C17 112.9(6) . . ? C45 C44 C17 111.2(6) . . ? C47 C44 C46 109.6(6) . . ? C45 C44 C46 109.0(6) . . ? C17 C44 C46 107.0(6) . . ? C44 C45 H42 109.5 . . ? C44 C45 H43 109.5 . . ? H42 C45 H43 109.5 . . ? C44 C45 H44 109.5 . . ? H42 C45 H44 109.5 . . ? H43 C45 H44 109.5 . . ? C44 C46 H45 109.5 . . ? C44 C46 H46 109.5 . . ? H45 C46 H46 109.5 . . ? C44 C46 H47 109.5 . . ? H45 C46 H47 109.5 . . ? H46 C46 H47 109.5 . . ? C44 C47 H48 109.5 . . ? C44 C47 H49 109.5 . . ? H48 C47 H49 109.5 . . ? C44 C47 H50 109.5 . . ? H48 C47 H50 109.5 . . ? H49 C47 H50 109.5 . . ? C50 C48 C51 110.3(6) . . ? C50 C48 C23 109.7(6) . . ? C51 C48 C23 109.7(6) . . ? C50 C48 C49 107.6(6) . . ? C51 C48 C49 108.4(6) . . ? C23 C48 C49 111.1(6) . . ? C48 C49 H51 109.5 . . ? C48 C49 H52 109.5 . . ? H51 C49 H52 109.5 . . ? C48 C49 H53 109.5 . . ? H51 C49 H53 109.5 . . ? H52 C49 H53 109.5 . . ? C48 C50 H54 109.5 . . ? C48 C50 H55 109.5 . . ? H54 C50 H55 109.5 . . ? C48 C50 H56 109.5 . . ? H54 C50 H56 109.5 . . ? H55 C50 H56 109.5 . . ? C48 C51 H57 109.5 . . ? C48 C51 H58 109.5 . . ? H57 C51 H58 109.5 . . ? C48 C51 H59 109.5 . . ? H57 C51 H59 109.5 . . ? H58 C51 H59 109.5 . . ? C57 C52 C53 116.5(10) . . ? C57 C52 C58 125.1(11) . . ? C53 C52 C58 118.4(10) . . ? C54 C53 C52 121.5(10) . . ? C54 C53 H60 119.3 . . ? C52 C53 H60 119.3 . . ? C53 C54 C55 120.1(10) . . ? C53 C54 H61 120.0 . . ? C55 C54 H61 120.0 . . ? C56 C55 C54 118.5(12) . . ? C56 C55 H62 120.8 . . ? C54 C55 H62 120.8 . . ? C55 C56 C57 120.9(13) . . ? C55 C56 H63 119.5 . . ? C57 C56 H63 119.5 . . ? C52 C57 C56 122.6(12) . . ? C52 C57 H64 118.7 . . ? C56 C57 H64 118.7 . . ? C52 C58 H65 109.5 . . ? C52 C58 H66 109.5 . . ? H65 C58 H66 109.5 . . ? C52 C58 H67 109.5 . . ? H65 C58 H67 109.5 . . ? H66 C58 H67 109.5 . . ? 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 O4 P1 O2 C26 -177.4(4) . . . . ? O3 P1 O2 C26 -76.0(5) . . . . ? O4 P1 O3 C27 41.4(5) . . . . ? O2 P1 O3 C27 -50.0(5) . . . . ? O2 P1 O4 C28 -175.9(5) . . . . ? O3 P1 O4 C28 83.3(5) . . . . ? C24 C1 C2 C3 -64.1(9) . . . . ? C25 C1 C2 C3 113.1(7) . . . . ? C1 C2 C3 C28 -48.8(10) . . . . ? C1 C2 C3 C4 133.7(7) . . . . ? C28 C3 C4 C5 1.3(11) . . . . ? C2 C3 C4 C5 178.9(6) . . . . ? C3 C4 C5 C6 -0.4(10) . . . . ? C3 C4 C5 C36 179.0(6) . . . . ? C4 C5 C6 C7 -0.7(11) . . . . ? C36 C5 C6 C7 179.8(6) . . . . ? C5 C6 C7 C28 0.8(11) . . . . ? C5 C6 C7 C8 179.8(7) . . . . ? C6 C7 C8 C9 146.1(7) . . . . ? C28 C7 C8 C9 -35.1(11) . . . . ? C7 C8 C9 C27 85.6(9) . . . . ? C7 C8 C9 C10 -98.6(8) . . . . ? C27 C9 C10 C11 -1.6(10) . . . . ? C8 C9 C10 C11 -177.5(6) . . . . ? C9 C10 C11 C12 2.0(10) . . . . ? C9 C10 C11 C40 178.6(6) . . . . ? C10 C11 C12 C13 -0.7(10) . . . . ? C40 C11 C12 C13 -177.2(6) . . . . ? C11 C12 C13 C27 -0.9(10) . . . . ? C11 C12 C13 C14 170.9(6) . . . . ? C27 C13 C14 C15 -67.7(9) . . . . ? C12 C13 C14 C15 120.9(8) . . . . ? C13 C14 C15 C26 8.3(12) . . . . ? C13 C14 C15 C16 -170.1(6) . . . . ? C26 C15 C16 C17 0.3(11) . . . . ? C14 C15 C16 C17 178.8(6) . . . . ? C15 C16 C17 C18 -1.1(10) . . . . ? C15 C16 C17 C44 -178.7(6) . . . . ? C16 C17 C18 C19 0.5(11) . . . . ? C44 C17 C18 C19 178.2(6) . . . . ? C17 C18 C19 C26 0.7(11) . . . . ? C17 C18 C19 C20 -173.5(7) . . . . ? C18 C19 C20 C21 -132.6(7) . . . . ? C26 C19 C20 C21 53.6(10) . . . . ? C19 C20 C21 C25 -106.7(8) . . . . ? C19 C20 C21 C22 69.6(9) . . . . ? C25 C21 C22 C23 1.6(11) . . . . ? C20 C21 C22 C23 -174.8(6) . . . . ? C21 C22 C23 C24 6.0(10) . . . . ? C21 C22 C23 C48 -177.0(7) . . . . ? C22 C23 C24 C1 -6.2(10) . . . . ? C48 C23 C24 C1 176.6(6) . . . . ? C25 C1 C24 C23 -1.1(11) . . . . ? C2 C1 C24 C23 176.1(6) . . . . ? C22 C21 C25 O1 176.1(6) . . . . ? C20 C21 C25 O1 -7.5(10) . . . . ? C22 C21 C25 C1 -9.3(11) . . . . ? C20 C21 C25 C1 167.0(6) . . . . ? C29 O1 C25 C21 -94.9(7) . . . . ? C29 O1 C25 C1 90.4(7) . . . . ? C24 C1 C25 C21 9.1(10) . . . . ? C2 C1 C25 C21 -168.2(6) . . . . ? C24 C1 C25 O1 -176.3(6) . . . . ? C2 C1 C25 O1 6.4(10) . . . . ? C16 C15 C26 O2 178.6(6) . . . . ? C14 C15 C26 O2 0.3(11) . . . . ? C16 C15 C26 C19 1.0(11) . . . . ? C14 C15 C26 C19 -177.3(6) . . . . ? P1 O2 C26 C15 86.0(7) . . . . ? P1 O2 C26 C19 -96.3(6) . . . . ? C18 C19 C26 C15 -1.5(11) . . . . ? C20 C19 C26 C15 172.5(7) . . . . ? C18 C19 C26 O2 -179.1(6) . . . . ? C20 C19 C26 O2 -5.2(10) . . . . ? C12 C13 C27 C9 1.4(10) . . . . ? C14 C13 C27 C9 -170.4(7) . . . . ? C12 C13 C27 O3 -176.0(6) . . . . ? C14 C13 C27 O3 12.2(10) . . . . ? C10 C9 C27 C13 -0.2(10) . . . . ? C8 C9 C27 C13 175.8(7) . . . . ? C10 C9 C27 O3 177.3(6) . . . . ? C8 C9 C27 O3 -6.8(9) . . . . ? P1 O3 C27 C13 89.2(7) . . . . ? P1 O3 C27 C9 -88.4(6) . . . . ? C4 C3 C28 O4 172.2(6) . . . . ? C2 C3 C28 O4 -5.2(10) . . . . ? C4 C3 C28 C7 -1.2(11) . . . . ? C2 C3 C28 C7 -178.6(6) . . . . ? P1 O4 C28 C3 103.6(7) . . . . ? P1 O4 C28 C7 -82.8(7) . . . . ? C6 C7 C28 C3 0.1(11) . . . . ? C8 C7 C28 C3 -178.8(7) . . . . ? C6 C7 C28 O4 -173.2(6) . . . . ? C8 C7 C28 O4 7.9(11) . . . . ? C25 O1 C29 C30 -152.3(6) . . . . ? O1 C29 C30 C31 119.8(7) . . . . ? O1 C29 C30 C35 -59.7(9) . . . . ? C35 C30 C31 C32 -2.1(11) . . . . ? C29 C30 C31 C32 178.4(7) . . . . ? C30 C31 C32 C33 1.9(11) . . . . ? C31 C32 C33 C34 -0.3(11) . . . . ? C32 C33 C34 C35 -1.0(11) . . . . ? C33 C34 C35 C30 0.8(11) . . . . ? C31 C30 C35 C34 0.8(11) . . . . ? C29 C30 C35 C34 -179.7(7) . . . . ? C6 C5 C36 C38 -174.7(7) . . . . ? C4 C5 C36 C38 5.9(10) . . . . ? C6 C5 C36 C39 -53.9(9) . . . . ? C4 C5 C36 C39 126.6(7) . . . . ? C6 C5 C36 C37 64.3(9) . . . . ? C4 C5 C36 C37 -115.1(7) . . . . ? C10 C11 C40 C43 50.7(9) . . . . ? C12 C11 C40 C43 -132.9(7) . . . . ? C10 C11 C40 C42 -69.8(8) . . . . ? C12 C11 C40 C42 106.6(8) . . . . ? C10 C11 C40 C41 169.5(6) . . . . ? C12 C11 C40 C41 -14.1(10) . . . . ? C16 C17 C44 C47 -17.7(10) . . . . ? C18 C17 C44 C47 164.7(6) . . . . ? C16 C17 C44 C45 -138.1(7) . . . . ? C18 C17 C44 C45 44.3(9) . . . . ? C16 C17 C44 C46 103.0(8) . . . . ? C18 C17 C44 C46 -74.6(8) . . . . ? C24 C23 C48 C50 -51.9(9) . . . . ? C22 C23 C48 C50 131.1(7) . . . . ? C24 C23 C48 C51 69.4(9) . . . . ? C22 C23 C48 C51 -107.6(8) . . . . ? C24 C23 C48 C49 -170.8(6) . . . . ? C22 C23 C48 C49 12.2(10) . . . . ? C57 C52 C53 C54 -0.4(15) . . . . ? C58 C52 C53 C54 177.1(10) . . . . ? C52 C53 C54 C55 0.3(15) . . . . ? C53 C54 C55 C56 0.5(16) . . . . ? C54 C55 C56 C57 -1.2(18) . . . . ? C53 C52 C57 C56 -0.3(17) . . . . ? C58 C52 C57 C56 -177.6(11) . . . . ? C55 C56 C57 C52 1.2(19) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 20.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.453 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.067 #===END data_m13par #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H59 O4 P, C H2 Cl2' _chemical_formula_structural ? _chemical_formula_sum 'C52 H61 Cl2 O4 P' _chemical_formula_weight 851.88 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 12.013(2) _cell_length_b 13.3530(10) _cell_length_c 16.616(6) _cell_angle_alpha 75.59(2) _cell_angle_beta 73.23(2) _cell_angle_gamma 67.607(10) _cell_volume 2330.3(10) _cell_formula_units_Z 2 _cell_measurement_temperature 223 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 40.1 _cell_measurement_theta_max 41.1 _cell_special_details ; ? ; _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.400 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 1.91 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type 'Psi-scans' _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 1.00 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 223 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device CAD4 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 2 1 2 0 4 # number of measured reflections (redundant set) _diffrn_reflns_number 9560 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 74.79 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_reduction_process ; perpendicular_monochr_Lp ; # number of unique reflections _reflns_number_total 9560 # number of observed reflections (> n sig(I)) _reflns_number_gt 8336 _reflns_observed_criterion refl_observed_if_Iobs_>2.500_sigma(Iobs) _computing_data_collection ? _computing_cell_refinement 'local program' _computing_data_reduction xtal_DIFDAT_ADDREF _computing_structure_solution xtal _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics xtal _computing_publication_material 'xtal_BONDLA_CIFIO, PLATON (Spek, 1990)' #======================================================================= # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method zachariasen _refine_ls_extinction_coef 1622(**) _refine_ls_extinction_expression 'EQ22_P292_"CRYST._COMP."_MUNKSGAARD_1970' _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack none _refine_ls_number_reflns 8336 _refine_ls_number_parameters 775 _refine_ls_number_restraints 61 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.1040 _refine_ls_R_factor_gt 0.0970 _refine_ls_wR_factor_ref 0.0960 _refine_ls_wR_factor_gt 0.0940 _refine_ls_goodness_of_fit_ref 0.801 _refine_ls_restrained_S_all ? _refine_ls_shift/su_max 0.668 _refine_ls_shift/su_mean 0.046 _refine_diff_density_max 1.017 _refine_diff_density_min -1.374 _refine_diff_density_rms ? # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv P P Uani 0.07251(9) 0.21505(8) 0.28738(6) 1.000 0.0344(3) O1 O Uani 0.2262(3) 0.3132(2) 0.33945(19) 1.000 0.0404(9) O2 O Uani 0.1209(2) 0.1387(2) 0.37070(16) 1.000 0.0344(8) O3 O Uani -0.0025(2) 0.1515(2) 0.26345(17) 1.000 0.0376(8) O4 O Uani 0.1996(2) 0.1852(2) 0.21272(16) 1.000 0.0343(8) C1 C Uani 0.3969(4) 0.2527(3) 0.2246(3) 1.000 0.0372(12) C2 C Uani 0.3311(5) 0.3483(4) 0.1647(3) 1.000 0.0445(14) C3 C Uani 0.2705(4) 0.3230(3) 0.1075(3) 1.000 0.0369(11) C4 C Uani 0.2757(4) 0.3852(3) 0.0261(3) 1.000 0.0414(12) C5 C Uani 0.2184(4) 0.3775(3) -0.0328(3) 1.000 0.0425(12) C6 C Uani 0.1595(4) 0.3005(3) -0.0089(3) 1.000 0.0426(14) C7 C Uani 0.1501(4) 0.2354(3) 0.0717(3) 1.000 0.0370(12) C8 C Uani 0.0719(5) 0.1632(4) 0.0862(3) 1.000 0.0445(14) C9 C Uani 0.0974(4) 0.0550(3) 0.1445(2) 1.000 0.0374(12) C10 C Uani 0.1493(4) -0.0445(4) 0.1139(3) 1.000 0.0433(14) C11 C Uani 0.1619(4) -0.1456(3) 0.1679(3) 1.000 0.0432(14) C12 C Uani 0.1195(4) -0.1430(3) 0.2551(2) 1.000 0.0384(12) C13 C Uani 0.0676(4) -0.0451(3) 0.2883(2) 1.000 0.0328(11) C14 C Uani 0.0269(4) -0.0427(3) 0.3829(2) 1.000 0.0354(11) C15 C Uani 0.1329(4) -0.0533(3) 0.4197(2) 1.000 0.0325(11) C16 C Uani 0.1920(4) -0.1557(3) 0.4648(2) 1.000 0.0365(12) C17 C Uani 0.2884(4) -0.1732(3) 0.5025(2) 1.000 0.0373(12) C18 C Uani 0.3235(4) -0.0830(3) 0.4967(2) 1.000 0.0352(12) C19 C Uani 0.2693(3) 0.0198(3) 0.4522(2) 1.000 0.0312(11) C20 C Uani 0.3110(4) 0.1132(3) 0.4506(2) 1.000 0.0339(11) C21 C Uani 0.3874(4) 0.1412(3) 0.3637(2) 1.000 0.0322(11) C22 C Uani 0.5022(4) 0.0675(3) 0.3329(2) 1.000 0.0345(12) C23 C Uani 0.5694(4) 0.0861(4) 0.2501(3) 1.000 0.0395(12) C24 C Uani 0.5115(4) 0.1779(4) 0.1963(3) 1.000 0.0406(14) C25 C Uani 0.3391(4) 0.2367(3) 0.3101(2) 1.000 0.0334(11) C26 C Uani 0.1767(3) 0.0320(3) 0.4114(2) 1.000 0.0308(11) C27 C Uani 0.0573(4) 0.0517(3) 0.2320(2) 1.000 0.0334(12) C28 C Uani 0.2046(4) 0.2489(3) 0.1304(2) 1.000 0.0342(11) C29 C Uani 0.2390(4) 0.3995(4) 0.3681(3) 1.000 0.0438(16) C30 C Uani 0.1180(4) 0.4923(3) 0.3802(3) 1.000 0.0414(14) C31 C Uani 0.1008(5) 0.5683(4) 0.4296(3) 1.000 0.0528(17) C32 C Uani -0.0071(6) 0.6547(4) 0.4422(3) 1.000 0.0587(18) C33 C Uani -0.1009(6) 0.6661(4) 0.4049(3) 1.000 0.0694(19) C34 C Uani -0.0858(6) 0.5916(5) 0.3560(4) 1.000 0.078(2) C35 C Uani 0.0245(5) 0.5036(4) 0.3428(3) 1.000 0.0599(17) C36 C Uani 0.2212(5) 0.4515(4) -0.1204(3) 1.000 0.0519(16) C37 C Uani 0.237(2) 0.5563(11) -0.1177(7) 1.000 0.185(8) C38 C Uani 0.0912(8) 0.4912(9) -0.1424(5) 1.000 0.116(3) C39 C Uani 0.3145(15) 0.3886(12) -0.1848(6) 1.000 0.176(5) C40 C Uani 0.2134(6) -0.2550(4) 0.1344(3) 1.000 0.0586(19) C41 C Uani 0.289(2) -0.2473(8) 0.0453(6) 1.000 0.170(6) C42 C Uani 0.1007(11) -0.2945(9) 0.1450(10) 1.000 0.126(6) C43 C Uani 0.2978(8) -0.3425(5) 0.1899(5) 1.000 0.091(3) C44 C Uani 0.3558(5) -0.2853(4) 0.5485(3) 1.000 0.0489(16) C45 C Uani 0.4928(7) -0.3199(6) 0.5018(5) 1.000 0.085(3) C46 C Uani 0.2993(9) -0.3715(5) 0.5538(7) 1.000 0.092(3) C47 C Uani 0.3487(8) -0.2757(5) 0.6414(4) 1.000 0.078(3) C48 C Uani 0.7008(4) 0.0109(5) 0.2178(3) 1.000 0.0571(17) C49 C Uani 0.7506(8) -0.0760(10) 0.2868(5) 1.000 0.125(4) C50 C Uani 0.7851(7) 0.0845(9) 0.1843(6) 1.000 0.103(4) C51 C Uani 0.7070(8) -0.0340(7) 0.1416(5) 1.000 0.093(3) Cl1S Cl Uani 0.4463(3) -0.1632(2) 0.27381(17) 1.000 0.1423(12) Cl2S Cl Uani 0.4714(3) -0.0924(4) 0.0932(2) 1.000 0.218(2) C1S C Uani 0.3957(8) -0.0612(8) 0.2020(7) 1.000 0.113(4) H2A H Uiso 0.26757 0.40225 0.19898 1.000 0.0533 H2B H Uiso 0.39085 0.38318 0.12847 1.000 0.0533 H4 H Uiso 0.31992 0.43445 0.01047 1.000 0.0496 H6 H Uiso 0.12377 0.29115 -0.04873 1.000 0.0511 H8A H Uiso -0.01375 0.20722 0.10726 1.000 0.0534 H8B H Uiso 0.07616 0.14841 0.03030 1.000 0.0534 H10 H Uiso 0.17697 -0.04402 0.05485 1.000 0.0520 H12 H Uiso 0.12616 -0.20948 0.29270 1.000 0.0461 H14A H Uiso -0.00508 -0.10304 0.41112 1.000 0.0425 H14B H Uiso -0.03977 0.02638 0.39359 1.000 0.0425 H16 H Uiso 0.16486 -0.21471 0.46952 1.000 0.0437 H18 H Uiso 0.38607 -0.09178 0.52381 1.000 0.0422 H20A H Uiso 0.36018 0.09296 0.49368 1.000 0.0406 H20B H Uiso 0.23886 0.17765 0.46452 1.000 0.0406 H22 H Uiso 0.53556 0.00299 0.36916 1.000 0.0414 H24 H Uiso 0.55154 0.18946 0.13889 1.000 0.0487 H29A H Uiso 0.30178 0.42641 0.32629 1.000 0.0526 H29B H Uiso 0.26619 0.37161 0.42209 1.000 0.0526 H31 H Uiso 0.16450 0.56067 0.45519 1.000 0.0633 H32 H Uiso -0.01708 0.70576 0.47598 1.000 0.0704 H33 H Uiso -0.17517 0.72514 0.41315 1.000 0.0833 H34 H Uiso -0.15012 0.59947 0.33093 1.000 0.0937 H35 H Uiso 0.03467 0.45275 0.30878 1.000 0.0719 H37A H Uiso 0.17215 0.59315 -0.07375 1.000 0.2782 H37B H Uiso 0.23250 0.60327 -0.17239 1.000 0.2782 H37C H Uiso 0.31660 0.54048 -0.10522 1.000 0.2782 H38A H Uiso 0.02982 0.53279 -0.09955 1.000 0.1744 H38B H Uiso 0.07062 0.42810 -0.14356 1.000 0.1744 H38C H Uiso 0.09269 0.53728 -0.19771 1.000 0.1744 H39A H Uiso 0.29822 0.32210 -0.18270 1.000 0.2637 H39B H Uiso 0.39559 0.36962 -0.17359 1.000 0.2637 H39C H Uiso 0.31149 0.43242 -0.24077 1.000 0.2637 H41A H Uiso 0.31968 -0.31816 0.02669 1.000 0.2546 H41B H Uiso 0.35798 -0.22545 0.04378 1.000 0.2546 H41C H Uiso 0.23826 -0.19331 0.00777 1.000 0.2546 H42A H Uiso 0.05599 -0.29764 0.20388 1.000 0.1894 H42B H Uiso 0.13091 -0.36677 0.12884 1.000 0.1894 H42C H Uiso 0.04610 -0.24332 0.10878 1.000 0.1894 H43A H Uiso 0.25212 -0.35002 0.24837 1.000 0.1361 H43B H Uiso 0.36746 -0.32084 0.18705 1.000 0.1361 H43C H Uiso 0.32729 -0.41207 0.16944 1.000 0.1361 H45A H Uiso 0.52646 -0.26345 0.49935 1.000 0.1269 H45B H Uiso 0.49944 -0.32964 0.44446 1.000 0.1269 H45C H Uiso 0.53853 -0.38834 0.53226 1.000 0.1269 H46A H Uiso 0.34500 -0.44078 0.58335 1.000 0.1381 H46B H Uiso 0.30272 -0.38026 0.49682 1.000 0.1381 H46C H Uiso 0.21407 -0.34855 0.58462 1.000 0.1381 H47A H Uiso 0.38412 -0.22110 0.64059 1.000 0.1176 H47B H Uiso 0.39435 -0.34605 0.66971 1.000 0.1176 H47C H Uiso 0.26320 -0.25396 0.67181 1.000 0.1176 H49A H Uiso 0.74424 -0.04235 0.33412 1.000 0.1878 H49B H Uiso 0.83641 -0.11635 0.26527 1.000 0.1878 H49C H Uiso 0.70354 -0.12582 0.30590 1.000 0.1878 H50A H Uiso 0.75459 0.14185 0.13922 1.000 0.1549 H50B H Uiso 0.86889 0.03979 0.16239 1.000 0.1549 H50C H Uiso 0.78394 0.11736 0.23057 1.000 0.1549 H51A H Uiso 0.67351 0.02597 0.09900 1.000 0.1395 H51B H Uiso 0.65931 -0.08321 0.15862 1.000 0.1395 H51C H Uiso 0.79218 -0.07374 0.11799 1.000 0.1395 H11S H Uiso 0.41041 0.00321 0.20887 1.000 0.1354 H12S H Uiso 0.30651 -0.04329 0.21023 1.000 0.1354 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 P 0.0326(5) 0.0278(5) 0.0337(5) -0.0031(4) -0.0032(4) -0.0041(4) O1 0.0365(15) 0.0262(14) 0.0503(17) -0.0046(12) -0.0042(13) -0.0064(12) O2 0.0355(14) 0.0300(13) 0.0292(13) -0.0016(11) -0.0010(11) -0.0079(11) O3 0.0311(14) 0.0365(15) 0.0366(15) -0.0030(12) -0.0047(11) -0.0056(12) O4 0.0340(14) 0.0322(14) 0.0269(13) 0.0053(11) -0.0031(11) -0.0093(11) C1 0.042(2) 0.035(2) 0.033(2) 0.0050(16) -0.0075(17) -0.0180(18) C2 0.054(3) 0.035(2) 0.044(2) 0.0099(19) -0.014(2) -0.022(2) C3 0.036(2) 0.0276(19) 0.035(2) 0.0019(16) -0.0039(17) -0.0046(16) C4 0.041(2) 0.034(2) 0.037(2) 0.0041(17) -0.0010(18) -0.0109(18) C5 0.047(2) 0.034(2) 0.031(2) 0.0027(17) -0.0006(18) -0.0074(18) C6 0.052(3) 0.035(2) 0.032(2) 0.0026(17) -0.0090(19) -0.010(2) C7 0.040(2) 0.028(2) 0.033(2) 0.0011(16) -0.0058(17) -0.0058(17) C8 0.054(3) 0.042(2) 0.036(2) 0.0043(19) -0.015(2) -0.017(2) C9 0.041(2) 0.038(2) 0.031(2) 0.0021(17) -0.0061(17) -0.0166(18) C10 0.055(3) 0.043(2) 0.028(2) -0.0037(17) 0.0002(19) -0.020(2) C11 0.055(3) 0.037(2) 0.032(2) -0.0045(17) -0.0008(19) -0.016(2) C12 0.047(2) 0.034(2) 0.029(2) 0.0028(16) -0.0020(17) -0.0173(18) C13 0.032(2) 0.037(2) 0.0262(18) -0.0022(15) -0.0010(15) -0.0136(16) C14 0.035(2) 0.040(2) 0.0268(19) -0.0045(16) 0.0042(16) -0.0161(17) C15 0.034(2) 0.034(2) 0.0221(17) -0.0058(15) 0.0051(14) -0.0105(16) C16 0.041(2) 0.034(2) 0.030(2) -0.0052(16) 0.0033(17) -0.0157(18) C17 0.039(2) 0.033(2) 0.031(2) -0.0064(16) 0.0022(17) -0.0087(17) C18 0.034(2) 0.036(2) 0.029(2) -0.0044(16) -0.0006(16) -0.0095(17) C19 0.031(2) 0.0307(19) 0.0244(17) -0.0066(14) 0.0053(14) -0.0090(15) C20 0.036(2) 0.033(2) 0.0265(19) -0.0059(15) 0.0018(16) -0.0104(17) C21 0.034(2) 0.031(2) 0.0287(19) -0.0022(15) -0.0024(15) -0.0126(16) C22 0.036(2) 0.031(2) 0.029(2) -0.0009(15) -0.0046(16) -0.0071(16) C23 0.035(2) 0.045(2) 0.030(2) -0.0046(17) 0.0017(16) -0.0112(18) C24 0.041(2) 0.051(3) 0.026(2) 0.0018(18) 0.0008(17) -0.022(2) C25 0.034(2) 0.0264(18) 0.034(2) -0.0032(15) -0.0017(16) -0.0088(16) C26 0.031(2) 0.0285(18) 0.0220(17) -0.0049(14) 0.0063(14) -0.0063(15) C27 0.031(2) 0.031(2) 0.034(2) -0.0059(16) -0.0031(16) -0.0083(16) C28 0.034(2) 0.0260(18) 0.030(2) 0.0031(15) -0.0021(16) -0.0047(15) C29 0.048(3) 0.036(2) 0.044(3) -0.008(2) -0.002(2) -0.015(2) C30 0.052(3) 0.029(2) 0.031(2) 0.0003(16) 0.0020(18) -0.0116(18) C31 0.059(3) 0.043(3) 0.054(3) -0.014(2) 0.009(2) -0.026(2) C32 0.076(4) 0.036(2) 0.050(3) -0.010(2) 0.013(3) -0.021(2) C33 0.086(4) 0.037(3) 0.044(3) -0.004(2) 0.002(3) 0.011(3) C34 0.080(4) 0.066(4) 0.060(3) -0.020(3) -0.028(3) 0.022(3) C35 0.067(3) 0.045(3) 0.049(3) -0.016(2) -0.018(3) 0.011(2) C36 0.064(3) 0.048(3) 0.031(2) 0.010(2) -0.006(2) -0.018(2) C37 0.42(2) 0.100(8) 0.081(7) 0.063(6) -0.109(11) -0.143(12) C38 0.092(6) 0.122(7) 0.065(5) 0.042(5) -0.015(4) 0.003(5) C39 0.182(11) 0.133(9) 0.046(4) 0.031(5) 0.043(5) 0.050(8) C40 0.082(4) 0.042(3) 0.044(3) -0.010(2) 0.001(3) -0.021(3) C41 0.309(17) 0.059(5) 0.064(5) -0.028(4) 0.074(8) -0.050(9) C42 0.139(9) 0.090(7) 0.184(12) -0.061(8) -0.037(9) -0.049(6) C43 0.114(6) 0.042(3) 0.085(5) -0.022(3) -0.002(4) 0.001(4) C44 0.053(3) 0.031(2) 0.054(3) 0.001(2) -0.012(2) -0.009(2) C45 0.064(4) 0.060(4) 0.103(6) -0.010(4) -0.020(4) 0.008(3) C46 0.108(6) 0.041(3) 0.133(8) 0.026(4) -0.064(6) -0.028(4) C47 0.120(6) 0.050(3) 0.066(4) 0.018(3) -0.045(4) -0.028(4) C48 0.040(3) 0.068(3) 0.042(3) -0.012(2) 0.005(2) -0.003(2) C49 0.064(5) 0.145(8) 0.063(5) -0.001(5) 0.005(4) 0.054(5) C50 0.045(4) 0.149(8) 0.100(6) -0.025(6) 0.009(4) -0.030(4) C51 0.072(5) 0.102(6) 0.068(4) -0.032(4) 0.005(4) 0.008(4) Cl1S 0.129(2) 0.149(2) 0.120(2) -0.0390(17) 0.0223(16) -0.0399(18) Cl2S 0.162(3) 0.371(6) 0.145(3) 0.076(3) -0.065(2) -0.163(4) C1S 0.071(5) 0.114(7) 0.157(9) -0.025(6) -0.032(5) -0.027(5) #======================================================================= # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1S C1S 1.621(11) . . yes Cl2S C1S 1.846(11) . . yes P O3 1.627(3) . . yes P O4 1.649(3) . . yes P O2 1.614(3) . . yes O1 C25 1.390(5) . . yes O1 C29 1.424(6) . . yes O2 C26 1.411(4) . . yes O3 C27 1.402(4) . . yes O4 C28 1.418(4) . . yes C1 C24 1.388(7) . . no C1 C2 1.516(7) . . no C1 C25 1.392(6) . . no C2 C3 1.515(8) . . no C3 C4 1.398(6) . . no C3 C28 1.409(7) . . no C4 C5 1.391(7) . . no C5 C36 1.542(7) . . no C5 C6 1.380(7) . . no C6 C7 1.404(6) . . no C7 C8 1.521(8) . . no C7 C28 1.399(7) . . no C8 C9 1.502(6) . . no C9 C27 1.389(4) . . no C9 C10 1.391(6) . . no C10 C11 1.404(6) . . no C11 C12 1.395(6) . . no C11 C40 1.531(6) . . no C12 C13 1.393(5) . . no C13 C14 1.510(5) . . no C13 C27 1.380(5) . . no C14 C15 1.511(7) . . no C15 C16 1.412(5) . . no C15 C26 1.389(6) . . no C16 C17 1.388(7) . . no C17 C18 1.394(6) . . no C17 C44 1.531(6) . . no C18 C19 1.395(5) . . no C19 C20 1.503(6) . . no C19 C26 1.402(5) . . no C20 C21 1.515(5) . . no C21 C25 1.388(5) . . no C21 C22 1.393(6) . . no C22 C23 1.396(6) . . no C23 C48 1.536(8) . . no C23 C24 1.396(7) . . no C29 C30 1.507(7) . . no C30 C31 1.380(7) . . no C30 C35 1.378(8) . . no C31 C32 1.371(8) . . no C32 C33 1.379(10) . . no C33 C34 1.365(8) . . no C34 C35 1.400(9) . . no C36 C37 1.495(18) . . no C36 C39 1.464(14) . . no C36 C38 1.567(13) . . no C40 C42 1.582(16) . . no C40 C41 1.499(13) . . no C40 C43 1.531(10) . . no C44 C46 1.518(11) . . no C44 C45 1.545(11) . . no C44 C47 1.556(8) . . no C48 C51 1.502(10) . . no C48 C49 1.491(11) . . no C48 C50 1.569(12) . . no C2 H2B 0.9800 . . no C2 H2A 0.9800 . . no C4 H4 0.9400 . . no C6 H6 0.9401 . . no C8 H8B 0.9801 . . no C8 H8A 0.9800 . . no C10 H10 0.9400 . . no C12 H12 0.9399 . . no C14 H14B 0.9800 . . no C14 H14A 0.9800 . . no C16 H16 0.9400 . . no C18 H18 0.9400 . . no C20 H20A 0.9801 . . no C20 H20B 0.9800 . . no C22 H22 0.9400 . . no C24 H24 0.9400 . . no C29 H29B 0.9799 . . no C29 H29A 0.9800 . . no C31 H31 0.9400 . . no C32 H32 0.9400 . . no C33 H33 0.9400 . . no C34 H34 0.9400 . . no C35 H35 0.9399 . . no C37 H37B 0.9700 . . no C37 H37A 0.9700 . . no C37 H37C 0.9699 . . no C38 H38B 0.9700 . . no C38 H38A 0.9700 . . no C38 H38C 0.9700 . . no C39 H39C 0.9701 . . no C39 H39A 0.9700 . . no C39 H39B 0.9700 . . no C41 H41B 0.9700 . . no C41 H41A 0.9700 . . no C41 H41C 0.9700 . . no C42 H42B 0.9700 . . no C42 H42A 0.9700 . . no C42 H42C 0.9701 . . no C43 H43B 0.9700 . . no C43 H43C 0.9701 . . no C43 H43A 0.9700 . . no C45 H45C 0.9700 . . no C45 H45A 0.9699 . . no C45 H45B 0.9700 . . no C46 H46C 0.9700 . . no C46 H46B 0.9699 . . no C46 H46A 0.9699 . . no C47 H47B 0.9700 . . no C47 H47A 0.9700 . . no C47 H47C 0.9700 . . no C49 H49B 0.9700 . . no C49 H49A 0.9700 . . no C49 H49C 0.9699 . . no C50 H50B 0.9700 . . no C50 H50C 0.9700 . . no C50 H50A 0.9700 . . no C51 H51C 0.9700 . . no C51 H51A 0.9700 . . no C51 H51B 0.9700 . . no C1S H11S 0.9799 . . no C1S H12S 0.9800 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 P O3 104.68(14) . . . yes O2 P O4 101.39(14) . . . yes O3 P O4 99.70(14) . . . yes C25 O1 C29 112.6(4) . . . yes P O2 C26 147.5(2) . . . yes P O3 C27 122.1(3) . . . yes P O4 C28 120.4(3) . . . yes C2 C1 C24 122.0(4) . . . no C2 C1 C25 119.3(4) . . . no C24 C1 C25 118.7(4) . . . no C1 C2 C3 117.1(4) . . . no C2 C3 C4 115.3(4) . . . no C2 C3 C28 126.3(4) . . . no C4 C3 C28 118.2(4) . . . no C3 C4 C5 123.0(4) . . . no C4 C5 C6 116.7(4) . . . no C4 C5 C36 121.3(4) . . . no C6 C5 C36 122.0(5) . . . no C5 C6 C7 123.5(5) . . . no C6 C7 C8 114.2(4) . . . no C6 C7 C28 118.0(4) . . . no C8 C7 C28 127.7(4) . . . no C7 C8 C9 121.2(5) . . . no C8 C9 C10 122.1(3) . . . no C8 C9 C27 120.1(3) . . . no C10 C9 C27 117.5(4) . . . no C9 C10 C11 122.5(4) . . . no C10 C11 C12 117.1(4) . . . no C10 C11 C40 122.7(4) . . . no C12 C11 C40 120.1(4) . . . no C11 C12 C13 122.2(3) . . . no C12 C13 C14 122.1(3) . . . no C12 C13 C27 118.0(3) . . . no C14 C13 C27 119.8(3) . . . no C13 C14 C15 111.0(4) . . . no C14 C15 C16 118.6(4) . . . no C14 C15 C26 123.8(3) . . . no C16 C15 C26 117.6(4) . . . no C15 C16 C17 123.0(4) . . . no C16 C17 C18 117.0(4) . . . no C16 C17 C44 123.0(4) . . . no C18 C17 C44 120.0(4) . . . no C17 C18 C19 122.5(4) . . . no C18 C19 C20 119.0(4) . . . no C18 C19 C26 118.4(4) . . . no C20 C19 C26 122.6(3) . . . no C19 C20 C21 110.7(3) . . . no C20 C21 C22 120.9(3) . . . no C20 C21 C25 120.2(4) . . . no C22 C21 C25 118.6(3) . . . no C21 C22 C23 122.3(4) . . . no C22 C23 C24 116.7(5) . . . no C22 C23 C48 122.8(4) . . . no C24 C23 C48 120.4(4) . . . no C1 C24 C23 122.3(4) . . . no O1 C25 C1 119.0(3) . . . yes O1 C25 C21 120.1(3) . . . yes C1 C25 C21 120.7(4) . . . no O2 C26 C15 122.1(4) . . . yes O2 C26 C19 116.1(3) . . . yes C15 C26 C19 121.3(3) . . . no O3 C27 C9 118.1(3) . . . yes O3 C27 C13 119.0(3) . . . yes C9 C27 C13 122.7(3) . . . no O4 C28 C3 118.5(4) . . . yes O4 C28 C7 121.0(4) . . . yes C3 C28 C7 120.5(4) . . . no O1 C29 C30 110.4(4) . . . yes C29 C30 C31 119.1(5) . . . no C29 C30 C35 121.7(4) . . . no C31 C30 C35 119.2(5) . . . no C30 C31 C32 121.5(6) . . . no C31 C32 C33 119.5(5) . . . no C32 C33 C34 119.9(6) . . . no C33 C34 C35 120.7(7) . . . no C30 C35 C34 119.3(5) . . . no C5 C36 C37 111.3(6) . . . no C5 C36 C38 109.2(5) . . . no C5 C36 C39 109.0(6) . . . no C37 C36 C38 103.0(10) . . . no C37 C36 C39 114.3(10) . . . no C38 C36 C39 109.8(8) . . . no C11 C40 C41 112.2(6) . . . no C11 C40 C42 107.3(6) . . . no C11 C40 C43 110.2(5) . . . no C41 C40 C42 113.8(11) . . . no C41 C40 C43 106.9(9) . . . no C42 C40 C43 106.2(7) . . . no C17 C44 C45 108.0(5) . . . no C17 C44 C46 112.6(6) . . . no C17 C44 C47 109.6(4) . . . no C45 C44 C46 111.3(6) . . . no C45 C44 C47 108.2(6) . . . no C46 C44 C47 107.1(6) . . . no C23 C48 C49 112.2(5) . . . no C23 C48 C50 107.2(6) . . . no C23 C48 C51 110.8(5) . . . no C49 C48 C50 107.8(7) . . . no C49 C48 C51 113.1(7) . . . no C50 C48 C51 105.3(6) . . . no C1 C2 H2A 108.03 . . . no C1 C2 H2B 108.03 . . . no C3 C2 H2A 108.03 . . . no C3 C2 H2B 108.02 . . . no H2A C2 H2B 107.26 . . . no C3 C4 H4 118.51 . . . no C5 C4 H4 118.52 . . . no C5 C6 H6 118.25 . . . no C7 C6 H6 118.25 . . . no C7 C8 H8A 107.03 . . . no C7 C8 H8B 107.04 . . . no C9 C8 H8A 107.03 . . . no C9 C8 H8B 107.04 . . . no H8A C8 H8B 106.77 . . . no C9 C10 H10 118.77 . . . no C11 C10 H10 118.77 . . . no C11 C12 H12 118.91 . . . no C13 C12 H12 118.92 . . . no C13 C14 H14A 109.44 . . . no C13 C14 H14B 109.45 . . . no C15 C14 H14A 109.45 . . . no C15 C14 H14B 109.44 . . . no H14A C14 H14B 108.04 . . . no C15 C16 H16 118.51 . . . no C17 C16 H16 118.51 . . . no C17 C18 H18 118.74 . . . no C19 C18 H18 118.75 . . . no C19 C20 H20A 109.51 . . . no C19 C20 H20B 109.50 . . . no C21 C20 H20A 109.50 . . . no C21 C20 H20B 109.50 . . . no H20A C20 H20B 108.07 . . . no C21 C22 H22 118.85 . . . no C23 C22 H22 118.84 . . . no C1 C24 H24 118.84 . . . no C23 C24 H24 118.84 . . . no O1 C29 H29A 109.57 . . . no O1 C29 H29B 109.57 . . . no C30 C29 H29A 109.57 . . . no C30 C29 H29B 109.57 . . . no H29A C29 H29B 108.12 . . . no C30 C31 H31 119.26 . . . no C32 C31 H31 119.26 . . . no C31 C32 H32 120.27 . . . no C33 C32 H32 120.27 . . . no C32 C33 H33 120.03 . . . no C34 C33 H33 120.02 . . . no C33 C34 H34 119.67 . . . no C35 C34 H34 119.67 . . . no C30 C35 H35 120.35 . . . no C34 C35 H35 120.36 . . . no C36 C37 H37A 109.48 . . . no C36 C37 H37B 109.47 . . . no C36 C37 H37C 109.47 . . . no H37A C37 H37B 109.47 . . . no H37A C37 H37C 109.47 . . . no H37B C37 H37C 109.47 . . . no C36 C38 H38A 109.47 . . . no C36 C38 H38B 109.47 . . . no C36 C38 H38C 109.47 . . . no H38A C38 H38B 109.47 . . . no H38A C38 H38C 109.47 . . . no H38B C38 H38C 109.47 . . . no C36 C39 H39A 109.47 . . . no C36 C39 H39B 109.47 . . . no C36 C39 H39C 109.47 . . . no H39A C39 H39B 109.47 . . . no H39A C39 H39C 109.47 . . . no H39B C39 H39C 109.47 . . . no C40 C41 H41A 109.47 . . . no C40 C41 H41B 109.47 . . . no C40 C41 H41C 109.47 . . . no H41A C41 H41B 109.48 . . . no H41A C41 H41C 109.47 . . . no H41B C41 H41C 109.47 . . . no C40 C42 H42A 109.47 . . . no C40 C42 H42B 109.47 . . . no C40 C42 H42C 109.47 . . . no H42A C42 H42B 109.47 . . . no H42A C42 H42C 109.48 . . . no H42B C42 H42C 109.47 . . . no C40 C43 H43A 109.47 . . . no C40 C43 H43B 109.47 . . . no C40 C43 H43C 109.47 . . . no H43A C43 H43B 109.47 . . . no H43A C43 H43C 109.48 . . . no H43B C43 H43C 109.47 . . . no C44 C45 H45A 109.47 . . . no C44 C45 H45B 109.47 . . . no C44 C45 H45C 109.48 . . . no H45A C45 H45B 109.47 . . . no H45A C45 H45C 109.47 . . . no H45B C45 H45C 109.47 . . . no C44 C46 H46A 109.47 . . . no C44 C46 H46B 109.47 . . . no C44 C46 H46C 109.47 . . . no H46A C46 H46B 109.47 . . . no H46A C46 H46C 109.47 . . . no H46B C46 H46C 109.48 . . . no C44 C47 H47A 109.47 . . . no C44 C47 H47B 109.47 . . . no C44 C47 H47C 109.47 . . . no H47A C47 H47B 109.48 . . . no H47A C47 H47C 109.47 . . . no H47B C47 H47C 109.47 . . . no C48 C49 H49A 109.47 . . . no C48 C49 H49B 109.47 . . . no C48 C49 H49C 109.47 . . . no H49A C49 H49B 109.47 . . . no H49A C49 H49C 109.46 . . . no H49B C49 H49C 109.47 . . . no C48 C50 H50A 109.47 . . . no C48 C50 H50B 109.47 . . . no C48 C50 H50C 109.47 . . . no H50A C50 H50B 109.46 . . . no H50A C50 H50C 109.47 . . . no H50B C50 H50C 109.47 . . . no C48 C51 H51A 109.47 . . . no C48 C51 H51B 109.47 . . . no C48 C51 H51C 109.47 . . . no H51A C51 H51B 109.47 . . . no H51A C51 H51C 109.47 . . . no H51B C51 H51C 109.48 . . . no Cl1S C1S Cl2S 112.0(6) . . . yes Cl1S C1S H11S 109.22 . . . no Cl1S C1S H12S 109.21 . . . no Cl2S C1S H11S 109.21 . . . no Cl2S C1S H12S 109.22 . . . no H11S C1S H12S 107.91 . . . no 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 O3 P O2 C26 44.9(5) . . . . no O4 P O2 C26 -58.5(5) . . . . no O2 P O3 C27 -69.3(3) . . . . no O4 P O3 C27 35.3(3) . . . . no O2 P O4 C28 -168.8(3) . . . . no O3 P O4 C28 83.9(3) . . . . no C29 O1 C25 C1 -89.5(5) . . . . no C29 O1 C25 C21 96.3(5) . . . . no C25 O1 C29 C30 167.1(3) . . . . no P O2 C26 C15 -52.5(6) . . . . no P O2 C26 C19 135.1(4) . . . . no P O3 C27 C9 -89.9(5) . . . . no P O3 C27 C13 93.8(5) . . . . no P O4 C28 C3 105.2(4) . . . . no P O4 C28 C7 -77.5(4) . . . . no C25 C1 C2 C3 -101.7(5) . . . . no C24 C1 C2 C3 75.9(7) . . . . no C2 C1 C25 O1 -4.4(7) . . . . no C2 C1 C24 C23 -176.2(5) . . . . no C25 C1 C24 C23 1.4(8) . . . . no C24 C1 C25 C21 -7.9(7) . . . . no C24 C1 C25 O1 177.9(4) . . . . no C2 C1 C25 C21 169.8(5) . . . . no C1 C2 C3 C28 40.1(7) . . . . no C1 C2 C3 C4 -144.0(4) . . . . no C2 C3 C28 O4 -4.5(7) . . . . no C2 C3 C4 C5 -176.0(4) . . . . no C28 C3 C4 C5 0.3(7) . . . . no C4 C3 C28 C7 2.4(6) . . . . no C2 C3 C28 C7 178.2(4) . . . . no C4 C3 C28 O4 179.7(4) . . . . no C3 C4 C5 C6 -3.0(7) . . . . no C3 C4 C5 C36 177.1(4) . . . . no C36 C5 C6 C7 -176.9(4) . . . . no C4 C5 C6 C7 3.2(7) . . . . no C4 C5 C36 C39 101.2(9) . . . . no C6 C5 C36 C37 154.4(10) . . . . no C6 C5 C36 C38 41.4(7) . . . . no C6 C5 C36 C39 -78.6(10) . . . . no C4 C5 C36 C37 -25.7(11) . . . . no C4 C5 C36 C38 -138.7(6) . . . . no C5 C6 C7 C8 175.1(4) . . . . no C5 C6 C7 C28 -0.7(7) . . . . no C6 C7 C8 C9 150.2(4) . . . . no C6 C7 C28 C3 -2.2(6) . . . . no C8 C7 C28 O4 5.5(7) . . . . no C8 C7 C28 C3 -177.4(4) . . . . no C6 C7 C28 O4 -179.4(4) . . . . no C28 C7 C8 C9 -34.6(7) . . . . no C7 C8 C9 C27 79.4(6) . . . . no C7 C8 C9 C10 -107.5(6) . . . . no C8 C9 C27 O3 -2.4(7) . . . . no C8 C9 C27 C13 173.8(5) . . . . no C10 C9 C27 O3 -175.9(4) . . . . no C10 C9 C27 C13 0.3(8) . . . . no C27 C9 C10 C11 0.0(8) . . . . no C8 C9 C10 C11 -173.4(5) . . . . no C9 C10 C11 C40 177.1(5) . . . . no C9 C10 C11 C12 0.2(8) . . . . no C10 C11 C40 C41 21.0(12) . . . . no C10 C11 C40 C42 -104.7(8) . . . . no C10 C11 C40 C43 140.0(6) . . . . no C12 C11 C40 C41 -162.2(10) . . . . no C12 C11 C40 C42 72.1(8) . . . . no C10 C11 C12 C13 -0.5(8) . . . . no C40 C11 C12 C13 -177.5(5) . . . . no C12 C11 C40 C43 -43.2(8) . . . . no C11 C12 C13 C14 -177.2(5) . . . . no C11 C12 C13 C27 0.8(8) . . . . no C12 C13 C27 O3 175.5(4) . . . . no C12 C13 C27 C9 -0.6(8) . . . . no C27 C13 C14 C15 -91.5(5) . . . . no C14 C13 C27 C9 177.4(5) . . . . no C14 C13 C27 O3 -6.4(7) . . . . no C12 C13 C14 C15 86.5(5) . . . . no C13 C14 C15 C16 -102.3(4) . . . . no C13 C14 C15 C26 77.3(4) . . . . no C26 C15 C16 C17 1.8(5) . . . . no C14 C15 C26 O2 3.2(5) . . . . no C16 C15 C26 O2 -177.3(3) . . . . no C16 C15 C26 C19 -5.2(5) . . . . no C14 C15 C26 C19 175.2(3) . . . . no C14 C15 C16 C17 -178.6(3) . . . . no C15 C16 C17 C44 -177.6(4) . . . . no C15 C16 C17 C18 2.1(5) . . . . no C44 C17 C18 C19 176.9(4) . . . . no C16 C17 C44 C45 118.9(5) . . . . no C16 C17 C44 C47 -123.4(6) . . . . no C18 C17 C44 C45 -60.8(6) . . . . no C16 C17 C44 C46 -4.3(7) . . . . no C16 C17 C18 C19 -2.8(5) . . . . no C18 C17 C44 C47 57.0(7) . . . . no C18 C17 C44 C46 176.0(5) . . . . no C17 C18 C19 C26 -0.5(5) . . . . no C17 C18 C19 C20 178.8(3) . . . . no C18 C19 C26 O2 177.1(3) . . . . no C18 C19 C20 C21 107.5(4) . . . . no C26 C19 C20 C21 -73.2(5) . . . . no C20 C19 C26 C15 -174.7(3) . . . . no C20 C19 C26 O2 -2.1(5) . . . . no C18 C19 C26 C15 4.6(5) . . . . no C19 C20 C21 C25 107.6(4) . . . . no C19 C20 C21 C22 -66.4(6) . . . . no C20 C21 C22 C23 173.6(4) . . . . no C20 C21 C25 C1 -166.8(4) . . . . no C25 C21 C22 C23 -0.5(7) . . . . no C20 C21 C25 O1 7.4(7) . . . . no C22 C21 C25 C1 7.4(7) . . . . no C22 C21 C25 O1 -178.4(4) . . . . no C21 C22 C23 C48 174.4(5) . . . . no C21 C22 C23 C24 -5.6(7) . . . . no C22 C23 C48 C49 -5.4(8) . . . . no C22 C23 C24 C1 5.1(8) . . . . no C48 C23 C24 C1 -174.9(5) . . . . no C24 C23 C48 C49 174.5(6) . . . . no C24 C23 C48 C50 56.4(7) . . . . no C24 C23 C48 C51 -58.0(7) . . . . no C22 C23 C48 C50 -123.6(6) . . . . no C22 C23 C48 C51 122.1(6) . . . . no O1 C29 C30 C31 161.7(4) . . . . no O1 C29 C30 C35 -18.7(6) . . . . no C29 C30 C31 C32 179.5(5) . . . . no C31 C30 C35 C34 -0.2(8) . . . . no C35 C30 C31 C32 0.0(8) . . . . no C29 C30 C35 C34 -179.8(5) . . . . no C30 C31 C32 C33 0.1(9) . . . . no C31 C32 C33 C34 0.1(8) . . . . no C32 C33 C34 C35 -0.3(9) . . . . no C33 C34 C35 C30 0.4(9) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl1S C39 3.560(15) . 2_655 no Cl2S C51 3.546(11) . . no Cl2S C10 3.599(7) . . no Cl2S Cl2S 3.523(5) . 2_655 no Cl1S H51B 3.0969 . . no Cl2S H41B 2.9838 . . no Cl2S H51B 2.8259 . . no P C8 3.581(5) . . no P C14 3.589(4) . . no P O1 3.034(4) . . no P C25 3.455(5) . . no P H35 3.1267 . . no O1 O2 2.926(4) . . no O1 O4 3.171(4) . . no O1 P 3.034(4) . . no O2 O1 2.926(4) . . no O2 C13 3.418(5) . . no O2 C21 3.183(6) . . no O2 C25 3.167(6) . . no O3 C7 3.344(6) . . no O4 C25 2.983(5) . . no O4 C1S 3.248(10) . . no O4 C9 3.037(5) . . no O4 C1 2.908(6) . . no O4 O1 3.171(4) . . no O1 H20B 2.3913 . . no O1 H35 2.4420 . . no O1 H2A 2.3470 . . no O2 H20B 2.6360 . . no O2 H14B 2.7600 . . no O3 H14B 2.4251 . . no O3 H47C 2.8915 . 2_556 no O3 H8A 2.5440 . . no O4 H11S 2.7600 . . no O4 H12S 2.8296 . . no C1 O4 2.908(6) . . no C1S C10 3.576(12) . . no C1S O4 3.248(10) . . no C2 C29 3.396(7) . . no C7 O3 3.344(6) . . no C8 P 3.581(5) . . no C9 O4 3.037(5) . . no C9 C50 3.498(11) . 1_455 no C10 Cl2S 3.599(7) . . no C10 C1S 3.576(12) . . no C13 O2 3.418(5) . . no C14 C26 3.583(5) . 2_556 no C14 C15 3.560(5) . 2_556 no C14 P 3.589(4) . . no C15 C14 3.560(5) . 2_556 no C15 C15 3.585(6) . 2_556 no C20 C29 3.578(6) . . no C21 O2 3.183(6) . . no C25 O4 2.983(5) . . no C25 P 3.455(5) . . no C25 O2 3.167(6) . . no C26 C14 3.583(5) . 2_556 no C26 C27 3.578(5) . . no C27 C26 3.578(5) . . no C27 C50 3.427(11) . 1_455 no C27 C28 3.540(6) . . no C28 C27 3.540(6) . . no C29 C20 3.578(6) . . no C29 C2 3.396(7) . . no C30 C32 3.343(7) . 2_566 no C31 C32 3.562(8) . 2_566 no C31 C31 3.555(8) . 2_566 no C32 C30 3.343(7) . 2_566 no C32 C31 3.562(8) . 2_566 no C33 C49 3.587(12) . 1_465 no C39 Cl1S 3.560(15) . 2_655 no C49 C33 3.587(12) . 1_645 no C50 C9 3.498(11) . 1_655 no C50 C27 3.427(11) . 1_655 no C51 Cl2S 3.546(11) . . no C1 H29A 2.8910 . . no C1S H51B 2.9518 . . no C2 H29A 2.9982 . . no C4 H37C 2.6847 . . no C4 H37A 2.8769 . . no C6 H38A 3.0248 . 2_565 no C6 H39A 2.8939 . . no C6 H38B 2.6729 . . no C7 H38A 3.0831 . 2_565 no C9 H50B 2.7548 . 1_455 no C9 H12S 2.7538 . . no C10 H41B 2.9293 . . no C10 H41C 2.6905 . . no C10 H50B 3.0430 . 1_455 no C10 H12S 2.8124 . . no C11 H12S 2.8932 . . no C12 H42A 2.8320 . . no C12 H43A 2.6245 . . no C12 H12S 2.8625 . . no C13 H12S 2.7945 . . no C15 H14B 3.0416 . 2_556 no C16 H46C 2.8103 . . no C16 H14B 2.9993 . 2_556 no C16 H46B 2.7603 . . no C18 H45A 2.6992 . . no C18 H47A 2.7266 . . no C19 H22 3.0406 . . no C22 H49C 2.8121 . . no C22 H47A 3.0326 . 2_656 no C22 H49A 2.7159 . . no C22 H11S 3.0188 . . no C23 H11S 2.8435 . . no C24 H51A 2.7066 . . no C24 H11S 2.9545 . . no C24 H50A 2.6864 . . no C27 H12S 2.7226 . . no C27 H50B 2.8918 . 1_455 no C27 H50C 3.0650 . 1_455 no C29 H20B 2.9971 . . no C29 H2A 2.7235 . . no C33 H29B 3.0344 . 2_566 no C33 H20B 3.0579 . 2_566 no C34 H42A 3.0086 . 1_565 no C37 H4 2.5377 . . no C38 H6 2.6827 . . no C41 H10 2.5519 . . no C42 H12 3.0806 . . no C43 H12 2.6479 . . no C45 H18 2.8921 . . no C46 H16 2.4945 . . no C46 H31 3.0846 . 1_545 no C47 H18 2.8277 . . no C47 H50C 3.0415 . 2_656 no C49 H33 2.9589 . 1_645 no C49 H22 2.5022 . . no C50 H24 2.8469 . . no C51 H24 2.8512 . . no H2A H29A 2.3854 . . no H2A C29 2.7235 . . no H2A O1 2.3470 . . no H2B H4 2.2115 . . no H2B H24 2.5716 . . no H4 C37 2.5377 . . no H4 H37A 2.5868 . . no H4 H37C 2.0852 . . no H4 H2B 2.2115 . . no H6 C38 2.6827 . . no H6 H38B 2.1193 . . no H6 H8B 2.1990 . . no H8A O3 2.5440 . . no H8B H10 2.3723 . . no H8B H6 2.1990 . . no H10 H41B 2.5707 . . no H10 H41C 2.1103 . . no H10 H8B 2.3723 . . no H10 C41 2.5519 . . no H11S C24 2.9545 . . no H11S C23 2.8435 . . no H11S O4 2.7600 . . no H11S C22 3.0188 . . no H12 H14A 2.5044 . . no H12 C43 2.6479 . . no H12 C42 3.0806 . . no H12 H42A 2.5716 . . no H12 H43A 2.0580 . . no H12S O4 2.8296 . . no H12S C12 2.8625 . . no H12S C13 2.7945 . . no H12S C27 2.7226 . . no H12S C9 2.7538 . . no H12S C10 2.8124 . . no H12S C11 2.8932 . . no H14A H32 2.5538 . 1_545 no H14A H16 2.3316 . . no H14A H12 2.5044 . . no H14B C15 3.0416 . 2_556 no H14B O3 2.4251 . . no H14B O2 2.7600 . . no H14B C16 2.9993 . 2_556 no H16 H14A 2.3316 . . no H16 C46 2.4945 . . no H16 H46B 2.2316 . . no H16 H46C 2.3124 . . no H18 C47 2.8277 . . no H18 C45 2.8921 . . no H18 H47A 2.2549 . . no H18 H20A 2.3072 . . no H18 H45A 2.3209 . . no H20A H18 2.3072 . . no H20B O1 2.3913 . . no H20B O2 2.6360 . . no H20B C29 2.9971 . . no H20B C33 3.0579 . 2_566 no H20B H32 2.5662 . 2_566 no H20B H33 2.4619 . 2_566 no H22 C49 2.5022 . . no H22 C19 3.0406 . . no H22 H49A 2.2730 . . no H22 H49C 2.2730 . . no H24 C50 2.8469 . . no H24 H51A 2.2527 . . no H24 H50A 2.2756 . . no H24 C51 2.8512 . . no H24 H2B 2.5716 . . no H29A C2 2.9982 . . no H29A C1 2.8910 . . no H29A H2A 2.3854 . . no H29B H31 2.4742 . . no H29B C33 3.0344 . 2_566 no H31 H29B 2.4742 . . no H31 C46 3.0846 . 1_565 no H31 H46B 2.4062 . 1_565 no H32 H20B 2.5662 . 2_566 no H32 H14A 2.5538 . 1_565 no H33 C49 2.9589 . 1_465 no H33 H20B 2.4619 . 2_566 no H35 O1 2.4420 . . no H35 P 3.1267 . . no H37A C4 2.8769 . . no H37A H4 2.5868 . . no H37A H38A 2.3242 . . no H37B H39C 2.5327 . . no H37B H38C 2.3440 . . no H37C H4 2.0852 . . no H37C H39B 2.5327 . . no H37C C4 2.6847 . . no H38A C6 3.0248 . 2_565 no H38A C7 3.0831 . 2_565 no H38A H37A 2.3242 . . no H38B H39A 2.5269 . . no H38B C6 2.6729 . . no H38B H6 2.1193 . . no H38C H37B 2.3440 . . no H38C H39C 2.4475 . . no H39A C6 2.8939 . . no H39A H38B 2.5269 . . no H39B H37C 2.5327 . . no H39C H37B 2.5327 . . no H39C H38C 2.4475 . . no H41A H43C 2.4009 . . no H41B C10 2.9293 . . no H41B Cl2S 2.9838 . . no H41B H10 2.5707 . . no H41B H43B 2.4165 . . no H41C C10 2.6905 . . no H41C H10 2.1103 . . no H41C H50A 2.3523 . 2_655 no H42A C34 3.0086 . 1_545 no H42A C12 2.8320 . . no H42A H12 2.5716 . . no H42A H43A 2.4656 . . no H42B H43C 2.4524 . . no H43A H12 2.0580 . . no H43A H42A 2.4656 . . no H43A C12 2.6245 . . no H43B H41B 2.4165 . . no H43C H41A 2.4009 . . no H43C H42B 2.4524 . . no H45A C18 2.6992 . . no H45A H18 2.3209 . . no H45A H47A 2.5218 . . no H45B H46B 2.5566 . . no H45C H46A 2.5341 . . no H45C H47B 2.4797 . . no H46A H45C 2.5341 . . no H46A H47B 2.4446 . . no H46B H45B 2.5566 . . no H46B C16 2.7603 . . no H46B H31 2.4062 . 1_545 no H46B H16 2.2316 . . no H46C H47C 2.4525 . . no H46C C16 2.8103 . . no H46C H16 2.3124 . . no H47A C18 2.7266 . . no H47A C22 3.0326 . 2_656 no H47A H18 2.2549 . . no H47A H45A 2.5218 . . no H47B H45C 2.4797 . . no H47B H46A 2.4446 . . no H47C O3 2.8915 . 2_556 no H47C H46C 2.4525 . . no H47C H50C 2.5366 . 2_656 no H49A C22 2.7159 . . no H49A H22 2.2730 . . no H49A H50C 2.4922 . . no H49B H50B 2.4254 . . no H49B H51C 2.5341 . . no H49C H22 2.2730 . . no H49C C22 2.8121 . . no H49C H51B 2.5341 . . no H50A C24 2.6864 . . no H50A H24 2.2756 . . no H50A H41C 2.3523 . 2_655 no H50A H51A 2.4142 . . no H50B C10 3.0430 . 1_655 no H50B C9 2.7548 . 1_655 no H50B C27 2.8918 . 1_655 no H50B H49B 2.4254 . . no H50B H51C 2.3885 . . no H50C H47C 2.5366 . 2_656 no H50C C47 3.0415 . 2_656 no H50C C27 3.0650 . 1_655 no H50C H49A 2.4922 . . no H51A H24 2.2527 . . no H51A C24 2.7066 . . no H51A H50A 2.4142 . . no H51B Cl2S 2.8259 . . no H51B Cl1S 3.0969 . . no H51B C1S 2.9518 . . no H51B H49C 2.5341 . . no H51C H50B 2.3885 . . no H51C H49B 2.5341 . . no 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 _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C2 H2A O1 0.9800 2.3470 2.811(6) 108.13 . yes C14 H14B O3 0.9800 2.4251 2.817(4) 103.28 . yes C20 H20B O1 0.9800 2.3913 2.853(5) 108.15 . yes C51 H51B Cl2S 0.9700 2.8259 3.546(11) 131.69 . yes # End of Crystallographic Information File