Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Boron templated catechol phosphines as bidentate ligands in silver complexes ; loop_ _publ_author_name _publ_author_address S.H.Chikkali ; Institut f\"ur Anorganische Chemie Universit\"at Stuttgart Pfaffenwaldring 55 D-70550 Stuttgart Bundesrepublik Deutschland ; D.Gudat ; Institut f\"ur Anorganische Chemie Universit\"at Stuttgart Pfaffenwaldring 55 D-70550 Stuttgart Bundesrepublik Deutschland ; F.Lissner ; Institut f\"ur Anorganische Chemie Universit\"at Stuttgart Pfaffenwaldring 55 D-70550 Stuttgart Bundesrepublik Deutschland ; T.Schleid ; Institut f\"ur Anorganische Chemie Universit\"at Stuttgart Pfaffenwaldring 55 D-70550 Stuttgart Bundesrepublik Deutschland ; M.Nieger ; Laboratory of Inorganic Chemistry Department of Chemistry Universitity of Helsinki P.O. Box 55 FIN-00014 University of Helsinki Finland ; # Attachment 'dalton.cif' # 1. SUBMISSION DETAILS _publ_contact_author ; Martin Nieger Laboratory of Inorganic Chemistry Department of Chemistry Universitity of Helsinki P.O. Box 55 FIN-00014 University of Helsinki Finland ; _publ_contact_author_email NIEGER@JOYX.JOENSUU.FI _publ_contact_author_fax '049 228 73-5327' _publ_contact_author_phone '049 228 73-5823' _publ_contact_letter ; enclosed you will find the necessary data for our publication in J. Chem. Soc., Dalton Trans. ; _publ_requested_coeditor_name ? _publ_contact_author_name 'Martin Nieger' #============================================================================== data_dg004_hy_compound_4 _database_code_depnum_ccdc_archive 'CCDC 648045' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver-bis{3-[(diphenylphosphanyl)-methyl]-benzene-1,2-diol}-triflate ; _chemical_name_common ;Silver-bis(3-((diphenylphosphanyl)-methyl)-benzene-1,2-diol)- triflate ; _chemical_melting_point ? _chemical_formula_moiety ; C38 H34 Ag O4 P2 - CF3SO3 - CH2Cl2 - C3H7NO ; _chemical_formula_sum 'C43 H43 Ag Cl2 F3 N O8 P2 S' _chemical_formula_weight 1031.55 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' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n #(no.14) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.818(1) _cell_length_b 22.343(2) _cell_length_c 15.085(1) _cell_angle_alpha 90.00 _cell_angle_beta 104.46(1) _cell_angle_gamma 90.00 _cell_volume 4509.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 274 _cell_measurement_theta_min 7 _cell_measurement_theta_max 20 _exptl_crystal_description plates _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 0.747 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6172 _exptl_absorpt_correction_T_max 0.9157 _exptl_absorpt_process_details 'SADABS, Tmin:Tmax=0.6409' _exptl_special_details ; dx = 40 mm, 120 sec./deg., 1 deg. 3 sets, 459 frames ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type NoniusKappaCCD _diffrn_measurement_method 'rotation in phi and omega, 1 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37390 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7908 _reflns_number_gt 5128 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DIRAX _computing_data_reduction EVALCCD _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Geometrical restraints (DFIX, SADI) were used for refinement of the OH- groups. For O20 2 possible H positions are localized. The position of H20 is this that position which makes a suitable H-bond to the major part of the disordered CH2Cl. The other peak makes a hydrogen to to the minor part.Restraints (DFIX, SADI and SIMU) are also used for refinement of the disordered CH2CL2 (0.75 : 0.25). ; _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^)+(0.0568P)^2^+24.9000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7908 _refine_ls_number_parameters 561 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.1064 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1603 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.062 _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 Ag1 Ag 0.5000 0.0000 0.0000 0.03105(19) Uani 1 2 d S . . C1 C 0.6855(4) 0.0915(3) 0.1277(4) 0.0225(13) Uani 1 1 d D . . O1 O 0.7107(3) 0.03207(19) 0.1297(3) 0.0319(10) Uani 1 1 d D . . H1 H 0.7713(15) 0.0266(19) 0.132(5) 0.048 Uiso 1 1 d D . . C2 C 0.7307(4) 0.1335(3) 0.0821(4) 0.0264(14) Uani 1 1 d D . . O2 O 0.8038(3) 0.11212(19) 0.0436(3) 0.0337(10) Uani 1 1 d D . . H2 H 0.844(3) 0.1388(15) 0.037(5) 0.051 Uiso 1 1 d D . . C3 C 0.7004(4) 0.1921(3) 0.0787(5) 0.0371(16) Uani 1 1 d . . . H3 H 0.7299 0.2206 0.0467 0.044 Uiso 1 1 calc R . . C4 C 0.6273(5) 0.2104(3) 0.1212(5) 0.0427(18) Uani 1 1 d . . . H4 H 0.6067 0.2511 0.1181 0.051 Uiso 1 1 calc R . . C5 C 0.5843(4) 0.1691(3) 0.1682(5) 0.0358(16) Uani 1 1 d . . . H5 H 0.5351 0.1817 0.1984 0.043 Uiso 1 1 calc R . . C6 C 0.6126(4) 0.1093(3) 0.1715(4) 0.0254(13) Uani 1 1 d . . . C7 C 0.5669(4) 0.0616(3) 0.2208(4) 0.0236(13) Uani 1 1 d . . . H7A H 0.5446 0.0801 0.2719 0.028 Uiso 1 1 calc R . . H7B H 0.6180 0.0310 0.2467 0.028 Uiso 1 1 calc R . . P1 P 0.46014(10) 0.02584(7) 0.14139(10) 0.0222(3) Uani 1 1 d . . . C8 C 0.4277(4) -0.0382(3) 0.2030(4) 0.0213(12) Uani 1 1 d . . . C9 C 0.3498(4) -0.0748(3) 0.1564(4) 0.0285(14) Uani 1 1 d . . . H9 H 0.3178 -0.0664 0.0943 0.034 Uiso 1 1 calc R . . C10 C 0.3185(5) -0.1231(3) 0.1988(5) 0.0337(15) Uani 1 1 d . . . H10 H 0.2651 -0.1475 0.1662 0.040 Uiso 1 1 calc R . . C11 C 0.3654(5) -0.1360(3) 0.2897(4) 0.0338(15) Uani 1 1 d . . . H11 H 0.3434 -0.1687 0.3197 0.041 Uiso 1 1 calc R . . C12 C 0.4444(4) -0.1008(3) 0.3362(4) 0.0311(14) Uani 1 1 d . . . H12 H 0.4778 -0.1103 0.3977 0.037 Uiso 1 1 calc R . . C13 C 0.4750(4) -0.0521(3) 0.2937(4) 0.0276(14) Uani 1 1 d . . . H13 H 0.5286 -0.0279 0.3264 0.033 Uiso 1 1 calc R . . C14 C 0.3531(4) 0.0753(3) 0.1321(4) 0.0229(13) Uani 1 1 d . . . C15 C 0.3376(4) 0.1063(3) 0.2073(4) 0.0314(15) Uani 1 1 d . . . H15 H 0.3871 0.1053 0.2637 0.038 Uiso 1 1 calc R . . C16 C 0.2499(5) 0.1388(3) 0.2002(5) 0.0409(17) Uani 1 1 d . . . H16 H 0.2403 0.1606 0.2514 0.049 Uiso 1 1 calc R . . C17 C 0.1763(5) 0.1392(3) 0.1181(5) 0.0420(18) Uani 1 1 d . . . H17 H 0.1154 0.1601 0.1136 0.050 Uiso 1 1 calc R . . C18 C 0.1923(5) 0.1095(3) 0.0441(5) 0.0416(18) Uani 1 1 d . . . H18 H 0.1427 0.1107 -0.0123 0.050 Uiso 1 1 calc R . . C19 C 0.2803(4) 0.0773(3) 0.0497(4) 0.0316(15) Uani 1 1 d . . . H19 H 0.2904 0.0570 -0.0025 0.038 Uiso 1 1 calc R . . Ag2 Ag 0.5000 0.5000 0.0000 0.0334(2) Uani 1 2 d S . . C20 C 0.7441(4) 0.4651(3) 0.0899(4) 0.0270(14) Uani 1 1 d D . . O20 O 0.6937(4) 0.4550(2) 0.1563(3) 0.0452(12) Uani 1 1 d D . . H20 H 0.680(6) 0.4190(9) 0.162(4) 0.068 Uiso 1 1 d D . . C21 C 0.7823(4) 0.4169(3) 0.0498(4) 0.0266(13) Uani 1 1 d D . . O21 O 0.7679(3) 0.36111(19) 0.0819(3) 0.0345(10) Uani 1 1 d D . . H21 H 0.808(4) 0.3355(15) 0.071(5) 0.052 Uiso 1 1 d D . . C22 C 0.8304(4) 0.4273(3) -0.0187(4) 0.0312(14) Uani 1 1 d . . . H22 H 0.8543 0.3947 -0.0475 0.037 Uiso 1 1 calc R . . C23 C 0.8438(5) 0.4854(3) -0.0453(5) 0.0375(16) Uani 1 1 d . . . H23 H 0.8770 0.4925 -0.0924 0.045 Uiso 1 1 calc R . . C24 C 0.8085(4) 0.5335(3) -0.0031(4) 0.0338(15) Uani 1 1 d . . . H24 H 0.8191 0.5733 -0.0205 0.041 Uiso 1 1 calc R . . C25 C 0.7577(4) 0.5231(3) 0.0645(4) 0.0264(14) Uani 1 1 d . . . C26 C 0.7178(4) 0.5740(3) 0.1114(4) 0.0299(14) Uani 1 1 d . . . H26A H 0.7601 0.6099 0.1128 0.036 Uiso 1 1 calc R . . H26B H 0.7200 0.5627 0.1754 0.036 Uiso 1 1 calc R . . P2 P 0.58818(11) 0.59103(7) 0.04946(10) 0.0268(4) Uani 1 1 d . . . C27 C 0.5408(4) 0.6414(3) 0.1237(4) 0.0266(13) Uani 1 1 d . . . C28 C 0.4415(4) 0.6597(3) 0.0932(5) 0.0375(16) Uani 1 1 d . . . H28 H 0.4008 0.6449 0.0372 0.045 Uiso 1 1 calc R . . C29 C 0.4028(5) 0.7000(3) 0.1458(5) 0.0470(19) Uani 1 1 d . . . H29 H 0.3355 0.7130 0.1250 0.056 Uiso 1 1 calc R . . C30 C 0.4606(5) 0.7212(3) 0.2276(5) 0.0448(18) Uani 1 1 d . . . H30 H 0.4331 0.7481 0.2636 0.054 Uiso 1 1 calc R . . C31 C 0.5587(5) 0.7032(3) 0.2569(5) 0.0471(19) Uani 1 1 d . . . H31 H 0.5991 0.7182 0.3129 0.057 Uiso 1 1 calc R . . C32 C 0.5989(5) 0.6635(3) 0.2054(4) 0.0356(16) Uani 1 1 d . . . H32 H 0.6667 0.6514 0.2262 0.043 Uiso 1 1 calc R . . C33 C 0.5977(4) 0.6386(3) -0.0463(4) 0.0365(16) Uani 1 1 d . . . C34 C 0.5476(7) 0.6227(4) -0.1336(5) 0.060(2) Uani 1 1 d . . . H34 H 0.5083 0.5873 -0.1446 0.072 Uiso 1 1 calc R . . C35 C 0.5557(10) 0.6603(5) -0.2067(6) 0.089(4) Uani 1 1 d . . . H35 H 0.5232 0.6491 -0.2677 0.107 Uiso 1 1 calc R . . C36 C 0.6089(7) 0.7119(5) -0.1916(7) 0.079(3) Uani 1 1 d . . . H36 H 0.6137 0.7365 -0.2417 0.095 Uiso 1 1 calc R . . C37 C 0.6554(6) 0.7285(6) -0.1043(8) 0.111(5) Uani 1 1 d . . . H37 H 0.6927 0.7646 -0.0939 0.133 Uiso 1 1 calc R . . C38 C 0.6488(6) 0.6929(5) -0.0300(6) 0.083(4) Uani 1 1 d . . . H38 H 0.6787 0.7055 0.0308 0.100 Uiso 1 1 calc R . . S1 S 0.91657(10) 0.25434(7) -0.03442(10) 0.0272(3) Uani 1 1 d . . . O11 O 0.9097(3) 0.28657(18) 0.0472(3) 0.0330(10) Uani 1 1 d . . . O12 O 0.8469(3) 0.2735(3) -0.1161(3) 0.0562(15) Uani 1 1 d . . . O13 O 0.9282(4) 0.1908(2) -0.0222(4) 0.0493(13) Uani 1 1 d . . . C1T C 1.0372(5) 0.2776(3) -0.0506(4) 0.0321(15) Uani 1 1 d . . . F1 F 1.0606(3) 0.2490(2) -0.1191(3) 0.0540(11) Uani 1 1 d . . . F2 F 1.1103(3) 0.2687(2) 0.0235(3) 0.0540(11) Uani 1 1 d . . . F3 F 1.0364(3) 0.33628(18) -0.0694(3) 0.0601(12) Uani 1 1 d . . . O1D O 0.8861(3) -0.0084(2) 0.1201(4) 0.0493(13) Uani 1 1 d . . . C1D C 0.9593(5) 0.0029(3) 0.1829(5) 0.0431(17) Uani 1 1 d . . . H1D H 0.9483 0.0230 0.2350 0.052 Uiso 1 1 calc R . . N1D N 1.0531(4) -0.0112(3) 0.1832(4) 0.0432(15) Uani 1 1 d . . . C2D C 1.1371(6) 0.0025(4) 0.2606(6) 0.069(3) Uani 1 1 d . . . H2D1 H 1.1144 0.0285 0.3038 0.103 Uiso 1 1 calc R . . H2D2 H 1.1893 0.0230 0.2386 0.103 Uiso 1 1 calc R . . H2D3 H 1.1640 -0.0347 0.2914 0.103 Uiso 1 1 calc R . . C3D C 1.0749(5) -0.0430(4) 0.1065(5) 0.053(2) Uani 1 1 d . . . H3D1 H 1.0134 -0.0476 0.0579 0.079 Uiso 1 1 calc R . . H3D2 H 1.1021 -0.0826 0.1268 0.079 Uiso 1 1 calc R . . H3D3 H 1.1240 -0.0204 0.0831 0.079 Uiso 1 1 calc R . . C1C C 0.3607(5) 0.1340(5) -0.1739(6) 0.071(3) Uiso 0.75 1 d PDU A 1 H1C1 H 0.3884 0.1442 -0.2265 0.086 Uiso 0.75 1 calc PR A 1 H1C2 H 0.3509 0.0901 -0.1744 0.086 Uiso 0.75 1 calc PR A 1 Cl1 Cl 0.4472(2) 0.15345(14) -0.0739(2) 0.0686(8) Uiso 0.75 1 d PDU A 1 Cl2 Cl 0.2458(2) 0.16824(16) -0.1889(2) 0.0831(9) Uiso 0.75 1 d PDU A 1 C1C' C 0.3238(11) 0.1089(11) -0.190(2) 0.071(3) Uiso 0.25 1 d PDU B 2 H1C3 H 0.3625 0.1096 -0.2371 0.086 Uiso 0.25 1 calc PR B 2 H1C4 H 0.3358 0.0703 -0.1568 0.086 Uiso 0.25 1 calc PR B 2 Cl1' Cl 0.3556(6) 0.1677(4) -0.1163(6) 0.0686(8) Uiso 0.25 1 d PDU B 2 Cl2' Cl 0.1998(7) 0.1193(5) -0.2381(7) 0.0831(9) Uiso 0.25 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0267(3) 0.0500(4) 0.0185(3) -0.0054(3) 0.0096(3) -0.0074(3) C1 0.015(3) 0.028(3) 0.020(3) -0.004(2) -0.005(2) -0.006(2) O1 0.021(2) 0.033(2) 0.045(3) -0.002(2) 0.013(2) -0.0016(19) C2 0.013(3) 0.036(4) 0.029(3) -0.006(3) 0.003(2) -0.004(2) O2 0.025(2) 0.042(3) 0.038(3) -0.006(2) 0.014(2) -0.0134(19) C3 0.026(3) 0.039(4) 0.045(4) 0.006(3) 0.007(3) -0.009(3) C4 0.028(3) 0.032(4) 0.069(5) 0.004(3) 0.014(3) 0.001(3) C5 0.024(3) 0.039(4) 0.047(4) -0.009(3) 0.014(3) 0.003(3) C6 0.014(3) 0.039(4) 0.021(3) -0.005(3) 0.000(2) -0.004(2) C7 0.013(3) 0.038(3) 0.018(3) -0.002(3) 0.001(2) -0.003(2) P1 0.0151(7) 0.0351(8) 0.0159(7) -0.0022(6) 0.0031(6) -0.0035(6) C8 0.013(3) 0.033(3) 0.019(3) 0.000(2) 0.007(2) 0.002(2) C9 0.026(3) 0.037(4) 0.021(3) 0.000(3) 0.004(3) -0.002(3) C10 0.031(3) 0.027(3) 0.043(4) -0.002(3) 0.009(3) -0.003(3) C11 0.040(4) 0.025(3) 0.040(4) 0.006(3) 0.018(3) 0.006(3) C12 0.029(3) 0.033(4) 0.031(3) 0.010(3) 0.006(3) 0.006(3) C13 0.025(3) 0.037(4) 0.020(3) 0.001(3) 0.004(3) 0.003(3) C14 0.017(3) 0.027(3) 0.023(3) 0.002(3) 0.004(2) -0.005(2) C15 0.024(3) 0.038(4) 0.030(4) -0.002(3) 0.004(3) -0.003(3) C16 0.031(4) 0.042(4) 0.053(5) -0.005(3) 0.016(3) 0.005(3) C17 0.025(3) 0.035(4) 0.063(5) 0.010(4) 0.007(3) 0.003(3) C18 0.026(3) 0.042(4) 0.048(4) 0.011(3) -0.007(3) 0.002(3) C19 0.025(3) 0.037(4) 0.030(3) -0.003(3) 0.000(3) -0.004(3) Ag2 0.0248(3) 0.0413(4) 0.0317(4) -0.0088(3) 0.0024(3) 0.0005(3) C20 0.018(3) 0.043(4) 0.021(3) 0.003(3) 0.005(2) 0.002(3) O20 0.046(3) 0.058(3) 0.038(3) 0.006(3) 0.023(2) 0.004(3) C21 0.018(3) 0.035(4) 0.024(3) 0.006(3) 0.000(2) 0.006(3) O21 0.034(2) 0.035(3) 0.037(3) 0.007(2) 0.014(2) 0.008(2) C22 0.031(3) 0.034(4) 0.030(3) -0.002(3) 0.010(3) 0.004(3) C23 0.041(4) 0.043(4) 0.035(4) 0.002(3) 0.022(3) 0.005(3) C24 0.028(3) 0.038(4) 0.034(4) 0.001(3) 0.006(3) -0.002(3) C25 0.014(3) 0.038(3) 0.023(3) -0.003(3) -0.004(2) 0.005(2) C26 0.021(3) 0.040(4) 0.024(3) -0.004(3) -0.004(3) 0.006(3) P2 0.0189(7) 0.0377(9) 0.0207(8) 0.0005(7) -0.0009(6) 0.0045(7) C27 0.023(3) 0.026(3) 0.030(3) 0.006(3) 0.007(3) 0.003(2) C28 0.023(3) 0.050(4) 0.038(4) 0.010(3) 0.006(3) 0.006(3) C29 0.027(4) 0.057(5) 0.063(5) 0.018(4) 0.022(4) 0.015(3) C30 0.047(4) 0.052(5) 0.042(4) 0.005(4) 0.024(4) 0.019(4) C31 0.051(4) 0.051(5) 0.036(4) -0.006(3) 0.005(3) 0.022(4) C32 0.028(3) 0.045(4) 0.030(4) -0.001(3) 0.000(3) 0.016(3) C33 0.024(3) 0.057(5) 0.029(4) 0.013(3) 0.007(3) 0.016(3) C34 0.105(7) 0.045(5) 0.031(4) 0.000(3) 0.017(4) 0.024(5) C35 0.177(12) 0.069(7) 0.025(4) 0.015(4) 0.033(6) 0.066(8) C36 0.071(6) 0.109(9) 0.075(7) 0.054(7) 0.051(6) 0.050(6) C37 0.034(5) 0.174(12) 0.113(9) 0.108(9) -0.006(5) -0.028(6) C38 0.050(5) 0.111(8) 0.069(6) 0.052(6) -0.022(4) -0.046(5) S1 0.0201(7) 0.0328(8) 0.0290(8) -0.0057(7) 0.0069(6) -0.0012(6) O11 0.037(2) 0.032(2) 0.031(2) 0.0007(19) 0.0106(19) 0.003(2) O12 0.026(2) 0.107(4) 0.031(3) -0.012(3) 0.000(2) 0.017(3) O13 0.050(3) 0.029(3) 0.083(4) -0.011(3) 0.042(3) -0.010(2) C1T 0.030(3) 0.033(4) 0.033(4) 0.002(3) 0.006(3) -0.003(3) F1 0.040(2) 0.075(3) 0.057(3) -0.021(2) 0.030(2) -0.008(2) F2 0.026(2) 0.071(3) 0.057(3) -0.001(2) -0.0045(19) -0.0005(19) F3 0.066(3) 0.039(2) 0.087(3) 0.015(2) 0.041(3) -0.005(2) O1D 0.028(2) 0.063(3) 0.058(3) -0.007(3) 0.012(2) 0.005(2) C1D 0.034(4) 0.038(4) 0.058(5) -0.008(4) 0.015(4) -0.003(3) N1D 0.031(3) 0.045(4) 0.050(4) 0.005(3) 0.005(3) -0.004(3) C2D 0.044(4) 0.073(6) 0.078(6) 0.010(5) -0.005(4) -0.019(4) C3D 0.035(4) 0.065(5) 0.065(5) 0.009(4) 0.024(4) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P1 2.4026(15) 3_655 ? Ag1 P1 2.4026(15) . ? C1 O1 1.370(7) . ? C1 C6 1.395(8) . ? C1 C2 1.399(8) . ? O1 H1 0.839(10) . ? C2 O2 1.371(7) . ? C2 C3 1.373(9) . ? O2 H2 0.838(10) . ? C3 C4 1.386(9) . ? C3 H3 0.9500 . ? C4 C5 1.385(9) . ? C4 H4 0.9500 . ? C5 C6 1.388(9) . ? C5 H5 0.9500 . ? C6 C7 1.523(8) . ? C7 P1 1.835(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? P1 C8 1.822(6) . ? P1 C14 1.823(6) . ? C8 C9 1.395(8) . ? C8 C13 1.395(8) . ? C9 C10 1.378(9) . ? C9 H9 0.9500 . ? C10 C11 1.392(9) . ? C10 H10 0.9500 . ? C11 C12 1.385(9) . ? C11 H11 0.9500 . ? C12 C13 1.383(8) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.390(8) . ? C14 C19 1.391(8) . ? C15 C16 1.394(9) . ? C15 H15 0.9500 . ? C16 C17 1.393(10) . ? C16 H16 0.9500 . ? C17 C18 1.363(10) . ? C17 H17 0.9500 . ? C18 C19 1.397(9) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? Ag2 P2 2.3924(16) . ? Ag2 P2 2.3924(16) 3_665 ? C20 O20 1.374(7) . ? C20 C25 1.377(9) . ? C20 C21 1.400(8) . ? O20 H20 0.834(10) . ? C21 O21 1.370(7) . ? C21 C22 1.380(8) . ? O21 H21 0.838(10) . ? C22 C23 1.384(9) . ? C22 H22 0.9500 . ? C23 C24 1.398(9) . ? C23 H23 0.9500 . ? C24 C25 1.394(9) . ? C24 H24 0.9500 . ? C25 C26 1.515(8) . ? C26 P2 1.842(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? P2 C27 1.820(6) . ? P2 C33 1.824(7) . ? C27 C32 1.383(8) . ? C27 C28 1.395(8) . ? C28 C29 1.392(10) . ? C28 H28 0.9500 . ? C29 C30 1.376(10) . ? C29 H29 0.9500 . ? C30 C31 1.376(9) . ? C30 H30 0.9500 . ? C31 C32 1.384(9) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.373(10) . ? C33 C38 1.395(11) . ? C34 C35 1.413(12) . ? C34 H34 0.9500 . ? C35 C36 1.357(15) . ? C35 H35 0.9500 . ? C36 C37 1.365(15) . ? C36 H36 0.9500 . ? C37 C38 1.395(11) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? S1 O12 1.427(5) . ? S1 O13 1.436(5) . ? S1 O11 1.449(4) . ? S1 C1T 1.820(6) . ? C1T F1 1.321(7) . ? C1T F2 1.322(7) . ? C1T F3 1.341(7) . ? O1D C1D 1.227(8) . ? C1D N1D 1.333(8) . ? C1D H1D 0.9500 . ? N1D C3D 1.453(9) . ? N1D C2D 1.458(9) . ? C2D H2D1 0.9800 . ? C2D H2D2 0.9800 . ? C2D H2D3 0.9800 . ? C3D H3D1 0.9800 . ? C3D H3D2 0.9800 . ? C3D H3D3 0.9800 . ? C1C Cl2 1.725(6) . ? C1C Cl1 1.729(6) . ? C1C H1C1 0.9900 . ? C1C H1C2 0.9900 . ? C1C' Cl2' 1.702(7) . ? C1C' Cl1' 1.706(7) . ? C1C' H1C3 0.9900 . ? C1C' H1C4 0.9900 . ? 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 P1 Ag1 P1 180.00(10) 3_655 . ? O1 C1 C6 118.4(5) . . ? O1 C1 C2 121.3(5) . . ? C6 C1 C2 120.3(5) . . ? C1 O1 H1 113(3) . . ? O2 C2 C3 124.5(6) . . ? O2 C2 C1 116.2(5) . . ? C3 C2 C1 119.3(6) . . ? C2 O2 H2 113(3) . . ? C2 C3 C4 121.0(6) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 119.7(6) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.4(6) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 119.2(6) . . ? C5 C6 C7 122.9(5) . . ? C1 C6 C7 117.8(5) . . ? C6 C7 P1 110.5(4) . . ? C6 C7 H7A 109.5 . . ? P1 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? P1 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C8 P1 C14 102.5(2) . . ? C8 P1 C7 105.6(3) . . ? C14 P1 C7 106.9(3) . . ? C8 P1 Ag1 113.88(19) . . ? C14 P1 Ag1 116.04(19) . . ? C7 P1 Ag1 111.02(19) . . ? C9 C8 C13 118.4(5) . . ? C9 C8 P1 117.5(4) . . ? C13 C8 P1 124.1(4) . . ? C10 C9 C8 121.2(6) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 119.7(6) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 119.8(6) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C13 C12 C11 120.3(6) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C8 120.5(6) . . ? C12 C13 H13 119.7 . . ? C8 C13 H13 119.7 . . ? C15 C14 C19 119.2(5) . . ? C15 C14 P1 121.8(4) . . ? C19 C14 P1 118.7(5) . . ? C14 C15 C16 120.3(6) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C17 C16 C15 120.0(7) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C18 C17 C16 119.6(6) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 121.1(6) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C14 C19 C18 119.7(6) . . ? C14 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? P2 Ag2 P2 180.0 . 3_665 ? O20 C20 C25 119.1(5) . . ? O20 C20 C21 120.3(6) . . ? C25 C20 C21 120.7(5) . . ? C20 O20 H20 113(3) . . ? O21 C21 C22 123.9(5) . . ? O21 C21 C20 116.3(5) . . ? C22 C21 C20 119.8(6) . . ? C21 O21 H21 113(3) . . ? C21 C22 C23 120.0(6) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 120.1(6) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 120.1(6) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C20 C25 C24 119.3(6) . . ? C20 C25 C26 119.1(5) . . ? C24 C25 C26 121.6(6) . . ? C25 C26 P2 109.9(4) . . ? C25 C26 H26A 109.7 . . ? P2 C26 H26A 109.7 . . ? C25 C26 H26B 109.7 . . ? P2 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? C27 P2 C33 103.6(3) . . ? C27 P2 C26 105.6(3) . . ? C33 P2 C26 105.6(3) . . ? C27 P2 Ag2 118.95(19) . . ? C33 P2 Ag2 112.3(2) . . ? C26 P2 Ag2 109.7(2) . . ? C32 C27 C28 119.5(6) . . ? C32 C27 P2 123.4(4) . . ? C28 C27 P2 117.0(5) . . ? C29 C28 C27 119.2(6) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C30 C29 C28 120.9(6) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C31 119.5(7) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C30 C31 C32 120.6(7) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C27 C32 C31 120.3(6) . . ? C27 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 C38 120.3(7) . . ? C34 C33 P2 119.4(6) . . ? C38 C33 P2 120.1(6) . . ? C33 C34 C35 118.5(9) . . ? C33 C34 H34 120.8 . . ? C35 C34 H34 120.8 . . ? C36 C35 C34 121.3(9) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C35 C36 C37 119.8(9) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C36 C37 C38 120.8(10) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C37 C38 C33 119.1(9) . . ? C37 C38 H38 120.4 . . ? C33 C38 H38 120.4 . . ? O12 S1 O13 115.9(3) . . ? O12 S1 O11 114.3(3) . . ? O13 S1 O11 114.3(3) . . ? O12 S1 C1T 103.9(3) . . ? O13 S1 C1T 102.8(3) . . ? O11 S1 C1T 103.2(3) . . ? F1 C1T F2 107.7(5) . . ? F1 C1T F3 107.4(5) . . ? F2 C1T F3 106.8(5) . . ? F1 C1T S1 112.3(4) . . ? F2 C1T S1 112.1(4) . . ? F3 C1T S1 110.3(4) . . ? O1D C1D N1D 124.6(7) . . ? O1D C1D H1D 117.7 . . ? N1D C1D H1D 117.7 . . ? C1D N1D C3D 120.5(6) . . ? C1D N1D C2D 122.2(7) . . ? C3D N1D C2D 117.3(6) . . ? N1D C2D H2D1 109.5 . . ? N1D C2D H2D2 109.5 . . ? H2D1 C2D H2D2 109.5 . . ? N1D C2D H2D3 109.5 . . ? H2D1 C2D H2D3 109.5 . . ? H2D2 C2D H2D3 109.5 . . ? N1D C3D H3D1 109.5 . . ? N1D C3D H3D2 109.5 . . ? H3D1 C3D H3D2 109.5 . . ? N1D C3D H3D3 109.5 . . ? H3D1 C3D H3D3 109.5 . . ? H3D2 C3D H3D3 109.5 . . ? Cl2 C1C Cl1 114.6(5) . . ? Cl2 C1C H1C1 108.6 . . ? Cl1 C1C H1C1 108.6 . . ? Cl2 C1C H1C2 108.6 . . ? Cl1 C1C H1C2 108.6 . . ? H1C1 C1C H1C2 107.6 . . ? Cl2' C1C' Cl1' 103.9(7) . . ? Cl2' C1C' H1C3 111.0 . . ? Cl1' C1C' H1C3 111.0 . . ? Cl2' C1C' H1C4 111.0 . . ? Cl1' C1C' H1C4 111.0 . . ? H1C3 C1C' H1C4 109.0 . . ? 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 O1 C1 C2 O2 -2.8(7) . . . . ? C6 C1 C2 O2 178.0(5) . . . . ? O1 C1 C2 C3 177.4(5) . . . . ? C6 C1 C2 C3 -1.9(8) . . . . ? O2 C2 C3 C4 -178.6(6) . . . . ? C1 C2 C3 C4 1.3(9) . . . . ? C2 C3 C4 C5 0.3(10) . . . . ? C3 C4 C5 C6 -1.2(10) . . . . ? C4 C5 C6 C1 0.6(9) . . . . ? C4 C5 C6 C7 -179.0(6) . . . . ? O1 C1 C6 C5 -178.4(5) . . . . ? C2 C1 C6 C5 0.9(8) . . . . ? O1 C1 C6 C7 1.3(7) . . . . ? C2 C1 C6 C7 -179.4(5) . . . . ? C5 C6 C7 P1 92.3(6) . . . . ? C1 C6 C7 P1 -87.3(5) . . . . ? C6 C7 P1 C8 170.1(4) . . . . ? C6 C7 P1 C14 -81.2(4) . . . . ? C6 C7 P1 Ag1 46.2(4) . . . . ? P1 Ag1 P1 C8 -40.9(2) 3_655 . . . ? P1 Ag1 P1 C14 -159.5(2) 3_655 . . . ? P1 Ag1 P1 C7 78.2(2) 3_655 . . . ? C14 P1 C8 C9 70.3(5) . . . . ? C7 P1 C8 C9 -177.9(4) . . . . ? Ag1 P1 C8 C9 -55.8(5) . . . . ? C14 P1 C8 C13 -108.8(5) . . . . ? C7 P1 C8 C13 2.9(6) . . . . ? Ag1 P1 C8 C13 125.0(5) . . . . ? C13 C8 C9 C10 1.2(9) . . . . ? P1 C8 C9 C10 -178.0(5) . . . . ? C8 C9 C10 C11 -0.3(9) . . . . ? C9 C10 C11 C12 -1.2(9) . . . . ? C10 C11 C12 C13 1.8(9) . . . . ? C11 C12 C13 C8 -1.0(9) . . . . ? C9 C8 C13 C12 -0.6(8) . . . . ? P1 C8 C13 C12 178.6(5) . . . . ? C8 P1 C14 C15 72.7(5) . . . . ? C7 P1 C14 C15 -38.1(5) . . . . ? Ag1 P1 C14 C15 -162.6(4) . . . . ? C8 P1 C14 C19 -101.0(5) . . . . ? C7 P1 C14 C19 148.2(5) . . . . ? Ag1 P1 C14 C19 23.7(5) . . . . ? C19 C14 C15 C16 0.4(9) . . . . ? P1 C14 C15 C16 -173.3(5) . . . . ? C14 C15 C16 C17 1.4(10) . . . . ? C15 C16 C17 C18 -2.3(10) . . . . ? C16 C17 C18 C19 1.5(10) . . . . ? C15 C14 C19 C18 -1.2(9) . . . . ? P1 C14 C19 C18 172.7(5) . . . . ? C17 C18 C19 C14 0.2(10) . . . . ? O20 C20 C21 O21 -1.2(8) . . . . ? C25 C20 C21 O21 177.7(5) . . . . ? O20 C20 C21 C22 178.2(5) . . . . ? C25 C20 C21 C22 -2.9(8) . . . . ? O21 C21 C22 C23 -178.4(6) . . . . ? C20 C21 C22 C23 2.2(9) . . . . ? C21 C22 C23 C24 -0.1(9) . . . . ? C22 C23 C24 C25 -1.4(9) . . . . ? O20 C20 C25 C24 -179.8(5) . . . . ? C21 C20 C25 C24 1.3(8) . . . . ? O20 C20 C25 C26 0.7(8) . . . . ? C21 C20 C25 C26 -178.3(5) . . . . ? C23 C24 C25 C20 0.8(8) . . . . ? C23 C24 C25 C26 -179.6(5) . . . . ? C20 C25 C26 P2 -89.1(6) . . . . ? C24 C25 C26 P2 91.4(6) . . . . ? C25 C26 P2 C27 168.9(4) . . . . ? C25 C26 P2 C33 -81.7(5) . . . . ? C25 C26 P2 Ag2 39.6(5) . . . . ? P2 Ag2 P2 C27 -57.7(3) 3_665 . . . ? P2 Ag2 P2 C33 -178.8(3) 3_665 . . . ? P2 Ag2 P2 C26 64.0(3) 3_665 . . . ? C33 P2 C27 C32 -106.3(6) . . . . ? C26 P2 C27 C32 4.5(6) . . . . ? Ag2 P2 C27 C32 128.2(5) . . . . ? C33 P2 C27 C28 71.2(5) . . . . ? C26 P2 C27 C28 -178.0(5) . . . . ? Ag2 P2 C27 C28 -54.3(5) . . . . ? C32 C27 C28 C29 0.0(10) . . . . ? P2 C27 C28 C29 -177.6(5) . . . . ? C27 C28 C29 C30 -0.9(10) . . . . ? C28 C29 C30 C31 1.3(11) . . . . ? C29 C30 C31 C32 -0.8(12) . . . . ? C28 C27 C32 C31 0.4(10) . . . . ? P2 C27 C32 C31 177.8(5) . . . . ? C30 C31 C32 C27 0.0(11) . . . . ? C27 P2 C33 C34 -123.1(6) . . . . ? C26 P2 C33 C34 126.2(6) . . . . ? Ag2 P2 C33 C34 6.6(6) . . . . ? C27 P2 C33 C38 51.9(7) . . . . ? C26 P2 C33 C38 -58.9(7) . . . . ? Ag2 P2 C33 C38 -178.5(6) . . . . ? C38 C33 C34 C35 4.9(12) . . . . ? P2 C33 C34 C35 179.8(6) . . . . ? C33 C34 C35 C36 -2.1(14) . . . . ? C34 C35 C36 C37 -0.3(15) . . . . ? C35 C36 C37 C38 -0.1(16) . . . . ? C36 C37 C38 C33 2.9(16) . . . . ? C34 C33 C38 C37 -5.3(13) . . . . ? P2 C33 C38 C37 179.8(8) . . . . ? O12 S1 C1T F1 -65.2(5) . . . . ? O13 S1 C1T F1 56.1(5) . . . . ? O11 S1 C1T F1 175.3(4) . . . . ? O12 S1 C1T F2 173.4(5) . . . . ? O13 S1 C1T F2 -65.3(5) . . . . ? O11 S1 C1T F2 53.9(5) . . . . ? O12 S1 C1T F3 54.5(5) . . . . ? O13 S1 C1T F3 175.8(5) . . . . ? O11 S1 C1T F3 -65.0(5) . . . . ? O1D C1D N1D C3D -1.2(11) . . . . ? O1D C1D N1D C2D -179.0(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O1D 0.839(10) 1.816(18) 2.625(6) 161(5) . O2 H2 O13 0.838(10) 2.00(2) 2.807(6) 161(6) . O20 H20 Cl2' 0.834(10) 1.70(6) 2.288(11) 126(6) 4_666 O20 H20 Cl2 0.834(10) 2.95(6) 3.566(6) 133(7) 4_666 O21 H21 O11 0.838(10) 1.887(14) 2.720(6) 172(5) . C1C' H1C4 O1 0.99 2.44 3.35(3) 152.2 3_655 C9 H9 O2 0.95 2.54 3.332(7) 141.1 3_655 C29 H29 O12 0.95 2.51 3.418(8) 160.4 3_665 C36 H36 O12 0.95 2.48 3.401(10) 162.5 2_654 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.391 _refine_diff_density_min -2.510 _refine_diff_density_rms 0.107 #============================================================================== data_gudat141_compound_5 _database_code_depnum_ccdc_archive 'CCDC 648046' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver-bis{4-[(diphenylphosphanyl)-methyl]-benzene-1,2-diol}-triflate ; _chemical_name_common ;Silver-bis(4-((diphenylphosphanyl)-methyl)-benzene-1,2-diol)- triflate ; _chemical_melting_point ? _chemical_formula_moiety '[C38 H34 Ag O4 P2]+ [CF3SO3]-, 2 thf' _chemical_formula_sum 'C47 H50 Ag F3 O9 P2 S' _chemical_formula_weight 1017.74 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' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c #(No.14) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.3659(3) _cell_length_b 16.1257(4) _cell_length_c 19.8458(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.338(1) _cell_angle_gamma 90.00 _cell_volume 4593.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9322 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description plates _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 0.621 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; dx = 40 mm, 240 sec./deg., 1 deg., 2 sets, 267 frames, mos.= 0.773(2) deg. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 1 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25126 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.0857 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.02 _reflns_number_total 8092 _reflns_number_gt 5179 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Geometrical restraints (DFIX, SADI) were used for refinement of the OH- groups, and gemetric restraints and restraints for the displacement parameters (SADI, SME, SIMU) were used for refinement of the two thf molecules. ; _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^)+(0.0131P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8092 _refine_ls_number_parameters 580 _refine_ls_number_restraints 110 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0612 _refine_ls_wR_factor_gt 0.0555 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.905 _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 Ag1 Ag 0.648250(13) 0.266684(13) 0.268904(12) 0.02354(7) Uani 1 1 d . . . P1 P 0.74140(4) 0.26493(5) 0.17119(4) 0.02151(18) Uani 1 1 d . . . C1 C 0.67042(16) 0.26485(17) 0.09182(14) 0.0217(7) Uani 1 1 d . . . H1A H 0.6613 0.3228 0.0765 0.026 Uiso 1 1 calc R . . H1B H 0.7049 0.2353 0.0569 0.026 Uiso 1 1 calc R . . C2 C 0.57642(17) 0.22462(17) 0.09771(13) 0.0195(7) Uani 1 1 d . . . C3 C 0.49966(17) 0.27230(18) 0.11391(14) 0.0231(7) Uani 1 1 d . . . H3 H 0.5073 0.3297 0.1233 0.028 Uiso 1 1 calc R . . C4 C 0.41257(17) 0.23669(18) 0.11639(14) 0.0221(7) Uani 1 1 d D . . O4 O 0.33838(12) 0.28811(11) 0.12913(11) 0.0300(5) Uani 1 1 d D . . H4 H 0.2914(11) 0.2616(13) 0.1393(15) 0.045 Uiso 1 1 d D . . C5 C 0.40042(18) 0.15266(18) 0.10440(14) 0.0233(7) Uani 1 1 d D . . O5 O 0.31173(12) 0.12279(12) 0.10869(11) 0.0321(5) Uani 1 1 d D . . H5 H 0.3091(15) 0.0732(10) 0.0948(15) 0.048 Uiso 1 1 d D . . C6 C 0.47694(18) 0.10450(17) 0.08938(14) 0.0251(7) Uani 1 1 d . . . H6 H 0.4695 0.0467 0.0817 0.030 Uiso 1 1 calc R . . C7 C 0.56394(18) 0.14055(18) 0.08554(14) 0.0239(7) Uani 1 1 d . . . H7 H 0.6158 0.1074 0.0744 0.029 Uiso 1 1 calc R . . C8 C 0.82429(17) 0.34787(17) 0.15582(15) 0.0216(7) Uani 1 1 d . . . C9 C 0.85473(17) 0.39698(17) 0.20993(15) 0.0250(8) Uani 1 1 d . . . H9 H 0.8368 0.3839 0.2542 0.030 Uiso 1 1 calc R . . C10 C 0.91113(18) 0.46481(19) 0.19928(17) 0.0318(8) Uani 1 1 d . . . H10 H 0.9311 0.4986 0.2363 0.038 Uiso 1 1 calc R . . C11 C 0.93849(19) 0.48380(19) 0.13563(19) 0.0356(9) Uani 1 1 d . . . H11 H 0.9771 0.5306 0.1288 0.043 Uiso 1 1 calc R . . C12 C 0.90996(19) 0.43500(19) 0.08150(17) 0.0348(8) Uani 1 1 d . . . H12 H 0.9293 0.4477 0.0375 0.042 Uiso 1 1 calc R . . C13 C 0.85269(18) 0.36713(19) 0.09198(16) 0.0318(8) Uani 1 1 d . . . H13 H 0.8328 0.3335 0.0548 0.038 Uiso 1 1 calc R . . C14 C 0.80763(17) 0.16839(16) 0.17387(15) 0.0205(7) Uani 1 1 d . . . C15 C 0.80867(18) 0.12131(17) 0.23244(15) 0.0256(7) Uani 1 1 d . . . H15 H 0.7751 0.1399 0.2698 0.031 Uiso 1 1 calc R . . C16 C 0.85817(19) 0.04732(17) 0.23717(17) 0.0283(8) Uani 1 1 d . . . H16 H 0.8589 0.0158 0.2776 0.034 Uiso 1 1 calc R . . C17 C 0.90594(18) 0.02031(19) 0.18301(17) 0.0295(8) Uani 1 1 d . . . H17 H 0.9393 -0.0305 0.1859 0.035 Uiso 1 1 calc R . . C18 C 0.90622(19) 0.06612(19) 0.12422(17) 0.0340(8) Uani 1 1 d . . . H18 H 0.9396 0.0468 0.0870 0.041 Uiso 1 1 calc R . . C19 C 0.85778(18) 0.14023(19) 0.11962(16) 0.0303(8) Uani 1 1 d . . . H19 H 0.8587 0.1721 0.0794 0.036 Uiso 1 1 calc R . . P2 P 0.53192(5) 0.22570(5) 0.34561(4) 0.02059(18) Uani 1 1 d . . . C20 C 0.57604(17) 0.20276(16) 0.43172(14) 0.0240(7) Uani 1 1 d . . . H20A H 0.6080 0.2523 0.4509 0.029 Uiso 1 1 calc R . . H20B H 0.5232 0.1894 0.4603 0.029 Uiso 1 1 calc R . . C21 C 0.64320(19) 0.13062(17) 0.43229(14) 0.0215(7) Uani 1 1 d . . . C22 C 0.61451(19) 0.05181(18) 0.45003(15) 0.0281(8) Uani 1 1 d . . . H22 H 0.5519 0.0429 0.4619 0.034 Uiso 1 1 calc R . . C23 C 0.6764(2) -0.01407(19) 0.45057(16) 0.0307(8) Uani 1 1 d D . . O23 O 0.64626(15) -0.09151(13) 0.47083(12) 0.0449(6) Uani 1 1 d D . . H23 H 0.668(2) -0.1275(11) 0.4439(13) 0.067 Uiso 1 1 d D . . C24 C 0.7687(2) -0.00225(19) 0.43402(16) 0.0311(8) Uani 1 1 d D . . O24 O 0.83271(14) -0.06595(13) 0.43502(13) 0.0460(6) Uani 1 1 d D . . H24 H 0.8167(18) -0.1023(14) 0.4635(14) 0.069 Uiso 1 1 d D . . C25 C 0.7975(2) 0.07485(18) 0.41482(15) 0.0305(8) Uani 1 1 d . . . H25 H 0.8598 0.0832 0.4019 0.037 Uiso 1 1 calc R . . C26 C 0.73513(18) 0.14115(18) 0.41427(14) 0.0237(7) Uani 1 1 d . . . H26 H 0.7558 0.1946 0.4013 0.028 Uiso 1 1 calc R . . C27 C 0.46457(18) 0.13391(17) 0.32175(15) 0.0205(7) Uani 1 1 d . . . C28 C 0.39108(18) 0.10734(17) 0.36020(15) 0.0285(8) Uani 1 1 d . . . H28 H 0.3744 0.1383 0.3986 0.034 Uiso 1 1 calc R . . C29 C 0.34249(19) 0.03624(18) 0.34252(17) 0.0334(8) Uani 1 1 d . . . H29 H 0.2928 0.0179 0.3689 0.040 Uiso 1 1 calc R . . C30 C 0.3665(2) -0.00812(19) 0.28629(17) 0.0349(9) Uani 1 1 d . . . H30 H 0.3325 -0.0567 0.2739 0.042 Uiso 1 1 calc R . . C31 C 0.4392(2) 0.01727(18) 0.24788(17) 0.0345(8) Uani 1 1 d . . . H31 H 0.4557 -0.0138 0.2095 0.041 Uiso 1 1 calc R . . C32 C 0.48767(18) 0.08821(17) 0.26592(15) 0.0270(8) Uani 1 1 d . . . H32 H 0.5377 0.1060 0.2396 0.032 Uiso 1 1 calc R . . C33 C 0.44743(17) 0.30859(17) 0.35423(15) 0.0199(7) Uani 1 1 d . . . C34 C 0.43655(18) 0.35151(17) 0.41371(16) 0.0259(8) Uani 1 1 d . . . H34 H 0.4707 0.3351 0.4535 0.031 Uiso 1 1 calc R . . C35 C 0.37615(18) 0.41833(18) 0.41576(16) 0.0292(8) Uani 1 1 d . . . H35 H 0.3688 0.4474 0.4568 0.035 Uiso 1 1 calc R . . C36 C 0.32679(19) 0.44252(18) 0.35832(18) 0.0328(9) Uani 1 1 d . . . H36 H 0.2856 0.4885 0.3598 0.039 Uiso 1 1 calc R . . C37 C 0.33686(19) 0.40030(19) 0.29849(17) 0.0355(9) Uani 1 1 d . . . H37 H 0.3024 0.4171 0.2590 0.043 Uiso 1 1 calc R . . C38 C 0.39714(18) 0.33360(18) 0.29617(16) 0.0312(8) Uani 1 1 d . . . H38 H 0.4043 0.3048 0.2550 0.037 Uiso 1 1 calc R . . S1 S 0.75257(5) 0.39855(5) 0.41809(4) 0.0262(2) Uani 1 1 d . . . O1 O 0.72178(13) 0.37398(12) 0.35117(10) 0.0387(6) Uani 1 1 d . . . O2 O 0.77207(13) 0.33251(11) 0.46489(10) 0.0370(6) Uani 1 1 d . . . O3 O 0.70195(12) 0.46728(12) 0.44516(11) 0.0382(6) Uani 1 1 d . . . C39 C 0.8673(2) 0.4432(2) 0.40479(17) 0.0306(8) Uani 1 1 d . . . F1 F 0.86163(10) 0.50658(10) 0.36178(9) 0.0396(5) Uani 1 1 d . . . F2 F 0.90755(11) 0.47048(11) 0.46205(9) 0.0459(5) Uani 1 1 d . . . F3 F 0.92422(11) 0.38707(11) 0.37918(10) 0.0482(5) Uani 1 1 d . . . O1T O 0.17748(12) 0.23612(13) 0.17956(11) 0.0388(6) Uani 1 1 d DU . . C1T C 0.1888(2) 0.1798(2) 0.23594(18) 0.0457(10) Uani 1 1 d DU . . H1T1 H 0.2479 0.1912 0.2617 0.055 Uiso 1 1 calc R . . H1T2 H 0.1896 0.1216 0.2200 0.055 Uiso 1 1 calc R . . C2T C 0.1071(3) 0.1943(2) 0.2793(2) 0.0605(11) Uani 1 1 d DU . . H2T1 H 0.0540 0.1581 0.2655 0.073 Uiso 1 1 calc R . . H2T2 H 0.1239 0.1844 0.3275 0.073 Uiso 1 1 calc R . . C3T C 0.0847(3) 0.2834(2) 0.2665(2) 0.0648(12) Uani 1 1 d DU . . H3T1 H 0.1232 0.3198 0.2966 0.078 Uiso 1 1 calc R . . H3T2 H 0.0180 0.2948 0.2735 0.078 Uiso 1 1 calc R . . C4T C 0.1073(2) 0.2960(2) 0.19428(18) 0.0484(10) Uani 1 1 d DU . . H4T1 H 0.0511 0.2876 0.1645 0.058 Uiso 1 1 calc R . . H4T2 H 0.1309 0.3530 0.1873 0.058 Uiso 1 1 calc R . . O2T O 0.84408(14) -0.19012(13) 0.52716(12) 0.0477(7) Uani 1 1 d DU . . C5T C 0.78461(19) -0.26109(19) 0.53876(17) 0.0415(9) Uani 1 1 d DU . . H5T1 H 0.7323 -0.2627 0.5048 0.050 Uiso 1 1 calc R . . H5T2 H 0.7588 -0.2579 0.5842 0.050 Uiso 1 1 calc R . . C6T C 0.8451(2) -0.33760(19) 0.53297(18) 0.0427(9) Uani 1 1 d DU . . H6T1 H 0.8713 -0.3551 0.5777 0.051 Uiso 1 1 calc R . . H6T2 H 0.8095 -0.3842 0.5122 0.051 Uiso 1 1 calc R . . C7T C 0.9205(2) -0.3085(2) 0.48818(19) 0.0568(11) Uani 1 1 d DU . . H7T1 H 0.9778 -0.3422 0.4949 0.068 Uiso 1 1 calc R . . H7T2 H 0.8997 -0.3105 0.4400 0.068 Uiso 1 1 calc R . . C8T C 0.9355(2) -0.2212(2) 0.5117(2) 0.0579(12) Uani 1 1 d DU . . H8T1 H 0.9779 -0.2198 0.5523 0.070 Uiso 1 1 calc R . . H8T2 H 0.9630 -0.1874 0.4759 0.070 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02433(12) 0.02549(13) 0.02130(14) -0.00029(12) 0.00694(9) 0.00026(11) P1 0.0199(4) 0.0264(4) 0.0184(5) -0.0013(4) 0.0036(3) 0.0002(4) C1 0.0242(14) 0.0233(16) 0.0178(17) 0.0026(14) 0.0017(13) 0.0031(14) C2 0.0231(15) 0.0220(18) 0.0135(17) -0.0005(14) 0.0017(13) -0.0013(14) C3 0.0305(16) 0.0189(16) 0.0199(18) 0.0020(15) 0.0004(14) -0.0008(14) C4 0.0203(15) 0.0257(18) 0.0205(18) -0.0014(15) 0.0033(13) 0.0060(15) O4 0.0267(11) 0.0287(14) 0.0351(15) -0.0033(10) 0.0080(11) -0.0007(9) C5 0.0240(16) 0.029(2) 0.0170(19) 0.0017(15) 0.0017(14) -0.0035(15) O5 0.0242(11) 0.0311(13) 0.0413(16) -0.0040(12) 0.0063(10) -0.0037(10) C6 0.0321(17) 0.0216(18) 0.0216(19) -0.0006(14) 0.0011(15) 0.0007(14) C7 0.0239(16) 0.0270(19) 0.0208(19) 0.0021(15) -0.0006(14) 0.0055(14) C8 0.0172(15) 0.0270(19) 0.021(2) 0.0017(15) 0.0046(14) 0.0020(13) C9 0.0257(16) 0.0291(19) 0.020(2) 0.0044(15) 0.0013(15) 0.0005(15) C10 0.0302(18) 0.036(2) 0.029(2) -0.0009(17) -0.0010(16) -0.0055(15) C11 0.0302(18) 0.033(2) 0.044(3) 0.0037(18) 0.0065(18) -0.0063(15) C12 0.0345(18) 0.042(2) 0.028(2) 0.0052(18) 0.0099(16) -0.0085(16) C13 0.0322(17) 0.040(2) 0.023(2) -0.0062(17) 0.0048(16) -0.0059(16) C14 0.0175(15) 0.0227(18) 0.021(2) -0.0044(15) 0.0005(14) -0.0017(13) C15 0.0264(16) 0.029(2) 0.022(2) -0.0025(15) 0.0074(15) -0.0009(15) C16 0.0326(17) 0.0254(19) 0.027(2) 0.0031(16) 0.0024(15) -0.0004(15) C17 0.0285(17) 0.029(2) 0.031(2) -0.0041(17) 0.0017(16) 0.0048(14) C18 0.0355(18) 0.042(2) 0.025(2) -0.0083(17) 0.0067(16) 0.0089(17) C19 0.0330(17) 0.037(2) 0.021(2) 0.0012(16) 0.0030(15) 0.0080(16) P2 0.0228(4) 0.0217(4) 0.0176(5) -0.0027(4) 0.0041(3) -0.0006(4) C20 0.0245(15) 0.0246(18) 0.0229(19) -0.0024(14) 0.0027(14) -0.0029(13) C21 0.0331(17) 0.0177(18) 0.0136(18) -0.0020(14) 0.0008(14) 0.0024(14) C22 0.0349(18) 0.029(2) 0.021(2) 0.0011(15) 0.0085(15) 0.0018(15) C23 0.050(2) 0.0192(19) 0.024(2) 0.0028(15) 0.0085(17) -0.0055(16) O23 0.0561(15) 0.0318(15) 0.0481(18) -0.0016(12) 0.0175(13) -0.0007(12) C24 0.0357(19) 0.031(2) 0.027(2) -0.0020(16) 0.0072(16) 0.0074(16) O24 0.0499(14) 0.0309(15) 0.059(2) 0.0092(12) 0.0205(13) 0.0174(12) C25 0.0460(19) 0.023(2) 0.022(2) -0.0002(15) 0.0019(16) -0.0007(16) C26 0.0350(18) 0.0191(18) 0.0171(19) -0.0013(14) 0.0015(15) -0.0027(14) C27 0.0224(15) 0.0207(18) 0.0186(19) -0.0011(14) 0.0034(14) -0.0008(13) C28 0.0311(17) 0.028(2) 0.026(2) -0.0073(16) 0.0070(15) -0.0032(15) C29 0.0333(18) 0.030(2) 0.037(2) -0.0030(17) 0.0093(17) -0.0078(15) C30 0.043(2) 0.0214(19) 0.040(2) -0.0020(17) -0.0014(18) -0.0108(16) C31 0.048(2) 0.025(2) 0.031(2) -0.0109(16) 0.0063(17) -0.0101(16) C32 0.0289(16) 0.0270(19) 0.026(2) 0.0018(15) 0.0108(15) -0.0028(14) C33 0.0212(15) 0.0178(17) 0.0210(19) 0.0000(14) 0.0037(14) -0.0048(13) C34 0.0269(16) 0.0288(19) 0.022(2) 0.0002(15) 0.0021(15) -0.0019(14) C35 0.0336(18) 0.0266(19) 0.028(2) -0.0055(16) 0.0056(16) 0.0005(15) C36 0.0258(17) 0.0234(19) 0.049(3) -0.0016(17) 0.0031(17) 0.0049(14) C37 0.0329(18) 0.038(2) 0.035(2) -0.0012(18) -0.0071(16) 0.0087(16) C38 0.0368(18) 0.034(2) 0.023(2) -0.0064(16) -0.0002(16) 0.0049(16) S1 0.0325(4) 0.0244(5) 0.0219(5) -0.0001(4) 0.0044(4) -0.0058(4) O1 0.0503(13) 0.0428(14) 0.0227(14) -0.0020(11) -0.0004(11) -0.0211(11) O2 0.0595(13) 0.0264(13) 0.0254(14) 0.0104(10) 0.0038(11) -0.0081(11) O3 0.0405(12) 0.0314(13) 0.0439(16) -0.0015(11) 0.0157(11) 0.0030(10) C39 0.0317(18) 0.035(2) 0.025(2) 0.0002(17) 0.0039(16) -0.0017(16) F1 0.0400(10) 0.0394(12) 0.0398(13) 0.0155(10) 0.0059(9) -0.0104(9) F2 0.0466(11) 0.0599(13) 0.0305(13) -0.0005(10) -0.0064(10) -0.0200(9) F3 0.0389(10) 0.0555(13) 0.0510(14) -0.0004(11) 0.0123(10) 0.0132(10) O1T 0.0367(12) 0.0427(14) 0.0380(15) 0.0039(12) 0.0136(11) 0.0068(11) C1T 0.056(2) 0.032(2) 0.051(3) 0.0087(19) 0.015(2) 0.0036(18) C2T 0.087(3) 0.049(3) 0.048(3) 0.006(2) 0.029(2) 0.010(2) C3T 0.078(3) 0.065(3) 0.053(3) 0.007(2) 0.022(2) 0.024(2) C4T 0.052(2) 0.049(2) 0.045(3) 0.0048(19) 0.0092(19) 0.0171(18) O2T 0.0428(14) 0.0368(15) 0.064(2) 0.0089(13) 0.0087(13) 0.0040(12) C5T 0.0378(18) 0.043(2) 0.044(2) 0.0033(19) 0.0043(17) 0.0012(18) C6T 0.050(2) 0.039(2) 0.039(3) 0.0001(18) 0.0037(19) 0.0035(18) C7T 0.060(2) 0.065(3) 0.047(3) 0.016(2) 0.015(2) 0.028(2) C8T 0.033(2) 0.059(3) 0.083(3) 0.031(2) 0.012(2) 0.0025(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P2 2.3990(8) . ? Ag1 P1 2.4008(8) . ? Ag1 O1 2.5757(19) . ? P1 C14 1.824(3) . ? P1 C8 1.825(3) . ? P1 C1 1.841(2) . ? C1 C2 1.507(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.387(4) . ? C2 C3 1.393(3) . ? C3 C4 1.379(3) . ? C3 H3 0.9500 . ? C4 O4 1.382(3) . ? C4 C5 1.386(4) . ? O4 H4 0.831(12) . ? C5 O5 1.368(3) . ? C5 C6 1.388(3) . ? O5 H5 0.846(12) . ? C6 C7 1.383(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.382(4) . ? C8 C9 1.390(4) . ? C9 C10 1.383(4) . ? C9 H9 0.9500 . ? C10 C11 1.373(4) . ? C10 H10 0.9500 . ? C11 C12 1.380(4) . ? C11 H11 0.9500 . ? C12 C13 1.390(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.388(4) . ? C14 C19 1.396(4) . ? C15 C16 1.390(4) . ? C15 H15 0.9500 . ? C16 C17 1.370(4) . ? C16 H16 0.9500 . ? C17 C18 1.381(4) . ? C17 H17 0.9500 . ? C18 C19 1.384(4) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? P2 C33 1.818(3) . ? P2 C27 1.821(3) . ? P2 C20 1.836(3) . ? C20 C21 1.511(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.386(4) . ? C21 C26 1.393(3) . ? C22 C23 1.385(4) . ? C22 H22 0.9500 . ? C23 O23 1.387(3) . ? C23 C24 1.392(4) . ? O23 H23 0.856(13) . ? C24 C25 1.369(4) . ? C24 O24 1.378(3) . ? O24 H24 0.853(13) . ? C25 C26 1.395(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.382(4) . ? C27 C28 1.395(4) . ? C28 C29 1.380(4) . ? C28 H28 0.9500 . ? C29 C30 1.381(4) . ? C29 H29 0.9500 . ? C30 C31 1.380(4) . ? C30 H30 0.9500 . ? C31 C32 1.379(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.383(4) . ? C33 C38 1.394(4) . ? C34 C35 1.385(4) . ? C34 H34 0.9500 . ? C35 C36 1.374(4) . ? C35 H35 0.9500 . ? C36 C37 1.381(4) . ? C36 H36 0.9500 . ? C37 C38 1.383(4) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? S1 O2 1.4332(19) . ? S1 O1 1.438(2) . ? S1 O3 1.441(2) . ? S1 C39 1.827(3) . ? C39 F2 1.329(3) . ? C39 F1 1.332(3) . ? C39 F3 1.334(3) . ? O1T C4T 1.435(3) . ? O1T C1T 1.445(3) . ? C1T C2T 1.502(4) . ? C1T H1T1 0.9900 . ? C1T H1T2 0.9900 . ? C2T C3T 1.491(4) . ? C2T H2T1 0.9900 . ? C2T H2T2 0.9900 . ? C3T C4T 1.497(4) . ? C3T H3T1 0.9900 . ? C3T H3T2 0.9900 . ? C4T H4T1 0.9900 . ? C4T H4T2 0.9900 . ? O2T C8T 1.451(3) . ? O2T C5T 1.452(3) . ? C5T C6T 1.516(4) . ? C5T H5T1 0.9900 . ? C5T H5T2 0.9900 . ? C6T C7T 1.504(4) . ? C6T H6T1 0.9900 . ? C6T H6T2 0.9900 . ? C7T C8T 1.497(4) . ? C7T H7T1 0.9900 . ? C7T H7T2 0.9900 . ? C8T H8T1 0.9900 . ? C8T H8T2 0.9900 . ? 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 P2 Ag1 P1 159.23(3) . . ? P2 Ag1 O1 93.50(5) . . ? P1 Ag1 O1 106.99(5) . . ? C14 P1 C8 106.69(12) . . ? C14 P1 C1 107.12(13) . . ? C8 P1 C1 101.53(13) . . ? C14 P1 Ag1 107.08(10) . . ? C8 P1 Ag1 121.02(10) . . ? C1 P1 Ag1 112.56(9) . . ? C2 C1 P1 113.62(19) . . ? C2 C1 H1A 108.8 . . ? P1 C1 H1A 108.8 . . ? C2 C1 H1B 108.8 . . ? P1 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C7 C2 C3 118.8(2) . . ? C7 C2 C1 121.1(2) . . ? C3 C2 C1 120.0(2) . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 O4 117.7(3) . . ? C3 C4 C5 120.6(3) . . ? O4 C4 C5 121.7(2) . . ? C4 O4 H4 112.1(16) . . ? O5 C5 C4 116.4(2) . . ? O5 C5 C6 124.3(3) . . ? C4 C5 C6 119.3(2) . . ? C5 O5 H5 110.0(15) . . ? C7 C6 C5 120.1(3) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C2 120.8(3) . . ? C6 C7 H7 119.6 . . ? C2 C7 H7 119.6 . . ? C13 C8 C9 119.0(3) . . ? C13 C8 P1 122.5(2) . . ? C9 C8 P1 118.4(2) . . ? C10 C9 C8 120.0(3) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.6(3) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 120.1(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 119.4(3) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C8 C13 C12 120.9(3) . . ? C8 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C19 118.7(3) . . ? C15 C14 P1 118.6(2) . . ? C19 C14 P1 122.7(2) . . ? C14 C15 C16 120.9(3) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C17 C16 C15 119.4(3) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 120.8(3) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C19 119.9(3) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 C14 120.3(3) . . ? C18 C19 H19 119.9 . . ? C14 C19 H19 119.9 . . ? C33 P2 C27 105.81(12) . . ? C33 P2 C20 105.49(13) . . ? C27 P2 C20 103.76(13) . . ? C33 P2 Ag1 110.01(9) . . ? C27 P2 Ag1 115.82(10) . . ? C20 P2 Ag1 115.03(9) . . ? C21 C20 P2 110.99(19) . . ? C21 C20 H20A 109.4 . . ? P2 C20 H20A 109.4 . . ? C21 C20 H20B 109.4 . . ? P2 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C22 C21 C26 118.2(3) . . ? C22 C21 C20 120.8(3) . . ? C26 C21 C20 121.1(3) . . ? C23 C22 C21 120.5(3) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 O23 119.0(3) . . ? C22 C23 C24 120.7(3) . . ? O23 C23 C24 120.2(3) . . ? C23 O23 H23 107.7(17) . . ? C25 C24 O24 118.1(3) . . ? C25 C24 C23 119.4(3) . . ? O24 C24 C23 122.4(3) . . ? C24 O24 H24 108.9(16) . . ? C24 C25 C26 119.8(3) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C21 C26 C25 121.4(3) . . ? C21 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C32 C27 C28 119.1(3) . . ? C32 C27 P2 120.0(2) . . ? C28 C27 P2 120.9(2) . . ? C29 C28 C27 120.2(3) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 119.7(3) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C31 C30 C29 120.8(3) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C32 C31 C30 119.2(3) . . ? C32 C31 H31 120.4 . . ? C30 C31 H31 120.4 . . ? C31 C32 C27 121.0(3) . . ? C31 C32 H32 119.5 . . ? C27 C32 H32 119.5 . . ? C34 C33 C38 119.2(3) . . ? C34 C33 P2 123.2(2) . . ? C38 C33 P2 117.4(2) . . ? C33 C34 C35 120.5(3) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C36 C35 C34 119.9(3) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 120.3(3) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C36 C37 C38 120.0(3) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C37 C38 C33 120.1(3) . . ? C37 C38 H38 119.9 . . ? C33 C38 H38 119.9 . . ? O2 S1 O1 115.99(12) . . ? O2 S1 O3 114.71(13) . . ? O1 S1 O3 114.54(13) . . ? O2 S1 C39 103.46(13) . . ? O1 S1 C39 102.72(14) . . ? O3 S1 C39 102.87(13) . . ? S1 O1 Ag1 150.82(12) . . ? F2 C39 F1 107.8(2) . . ? F2 C39 F3 107.3(2) . . ? F1 C39 F3 107.4(3) . . ? F2 C39 S1 111.8(2) . . ? F1 C39 S1 111.30(19) . . ? F3 C39 S1 111.0(2) . . ? C4T O1T C1T 108.9(2) . . ? O1T C1T C2T 106.2(2) . . ? O1T C1T H1T1 110.5 . . ? C2T C1T H1T1 110.5 . . ? O1T C1T H1T2 110.5 . . ? C2T C1T H1T2 110.5 . . ? H1T1 C1T H1T2 108.7 . . ? C3T C2T C1T 102.8(3) . . ? C3T C2T H2T1 111.2 . . ? C1T C2T H2T1 111.2 . . ? C3T C2T H2T2 111.2 . . ? C1T C2T H2T2 111.2 . . ? H2T1 C2T H2T2 109.1 . . ? C2T C3T C4T 103.9(3) . . ? C2T C3T H3T1 111.0 . . ? C4T C3T H3T1 111.0 . . ? C2T C3T H3T2 111.0 . . ? C4T C3T H3T2 111.0 . . ? H3T1 C3T H3T2 109.0 . . ? O1T C4T C3T 106.6(3) . . ? O1T C4T H4T1 110.4 . . ? C3T C4T H4T1 110.4 . . ? O1T C4T H4T2 110.4 . . ? C3T C4T H4T2 110.4 . . ? H4T1 C4T H4T2 108.6 . . ? C8T O2T C5T 107.7(2) . . ? O2T C5T C6T 106.7(2) . . ? O2T C5T H5T1 110.4 . . ? C6T C5T H5T1 110.4 . . ? O2T C5T H5T2 110.4 . . ? C6T C5T H5T2 110.4 . . ? H5T1 C5T H5T2 108.6 . . ? C7T C6T C5T 102.7(3) . . ? C7T C6T H6T1 111.2 . . ? C5T C6T H6T1 111.2 . . ? C7T C6T H6T2 111.2 . . ? C5T C6T H6T2 111.2 . . ? H6T1 C6T H6T2 109.1 . . ? C8T C7T C6T 102.0(3) . . ? C8T C7T H7T1 111.4 . . ? C6T C7T H7T1 111.4 . . ? C8T C7T H7T2 111.4 . . ? C6T C7T H7T2 111.4 . . ? H7T1 C7T H7T2 109.2 . . ? O2T C8T C7T 105.7(2) . . ? O2T C8T H8T1 110.6 . . ? C7T C8T H8T1 110.6 . . ? O2T C8T H8T2 110.6 . . ? C7T C8T H8T2 110.6 . . ? H8T1 C8T H8T2 108.7 . . ? 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 P2 Ag1 P1 C14 -63.31(11) . . . . ? O1 Ag1 P1 C14 107.11(10) . . . . ? P2 Ag1 P1 C8 174.31(11) . . . . ? O1 Ag1 P1 C8 -15.27(11) . . . . ? P2 Ag1 P1 C1 54.15(13) . . . . ? O1 Ag1 P1 C1 -135.43(11) . . . . ? C14 P1 C1 C2 88.7(2) . . . . ? C8 P1 C1 C2 -159.6(2) . . . . ? Ag1 P1 C1 C2 -28.7(2) . . . . ? P1 C1 C2 C7 -90.4(3) . . . . ? P1 C1 C2 C3 91.3(3) . . . . ? C7 C2 C3 C4 -1.3(4) . . . . ? C1 C2 C3 C4 177.0(2) . . . . ? C2 C3 C4 O4 -176.5(2) . . . . ? C2 C3 C4 C5 1.5(4) . . . . ? C3 C4 C5 O5 179.3(2) . . . . ? O4 C4 C5 O5 -2.7(4) . . . . ? C3 C4 C5 C6 -0.4(4) . . . . ? O4 C4 C5 C6 177.6(2) . . . . ? O5 C5 C6 C7 179.4(3) . . . . ? C4 C5 C6 C7 -0.9(4) . . . . ? C5 C6 C7 C2 1.1(4) . . . . ? C3 C2 C7 C6 0.0(4) . . . . ? C1 C2 C7 C6 -178.3(2) . . . . ? C14 P1 C8 C13 82.3(2) . . . . ? C1 P1 C8 C13 -29.8(3) . . . . ? Ag1 P1 C8 C13 -155.2(2) . . . . ? C14 P1 C8 C9 -102.3(2) . . . . ? C1 P1 C8 C9 145.7(2) . . . . ? Ag1 P1 C8 C9 20.2(2) . . . . ? C13 C8 C9 C10 1.2(4) . . . . ? P1 C8 C9 C10 -174.4(2) . . . . ? C8 C9 C10 C11 -0.8(4) . . . . ? C9 C10 C11 C12 -0.1(4) . . . . ? C10 C11 C12 C13 0.6(4) . . . . ? C9 C8 C13 C12 -0.7(4) . . . . ? P1 C8 C13 C12 174.7(2) . . . . ? C11 C12 C13 C8 -0.2(4) . . . . ? C8 P1 C14 C15 119.9(2) . . . . ? C1 P1 C14 C15 -132.0(2) . . . . ? Ag1 P1 C14 C15 -11.1(2) . . . . ? C8 P1 C14 C19 -59.7(2) . . . . ? C1 P1 C14 C19 48.4(2) . . . . ? Ag1 P1 C14 C19 169.4(2) . . . . ? C19 C14 C15 C16 -0.3(4) . . . . ? P1 C14 C15 C16 -179.89(19) . . . . ? C14 C15 C16 C17 -0.5(4) . . . . ? C15 C16 C17 C18 0.7(4) . . . . ? C16 C17 C18 C19 0.0(4) . . . . ? C17 C18 C19 C14 -0.8(4) . . . . ? C15 C14 C19 C18 1.0(4) . . . . ? P1 C14 C19 C18 -179.5(2) . . . . ? P1 Ag1 P2 C33 -118.87(11) . . . . ? O1 Ag1 P2 C33 70.30(10) . . . . ? P1 Ag1 P2 C27 1.01(13) . . . . ? O1 Ag1 P2 C27 -169.82(10) . . . . ? P1 Ag1 P2 C20 122.19(11) . . . . ? O1 Ag1 P2 C20 -48.64(11) . . . . ? C33 P2 C20 C21 176.48(19) . . . . ? C27 P2 C20 C21 65.4(2) . . . . ? Ag1 P2 C20 C21 -62.1(2) . . . . ? P2 C20 C21 C22 -100.3(3) . . . . ? P2 C20 C21 C26 78.9(3) . . . . ? C26 C21 C22 C23 0.9(4) . . . . ? C20 C21 C22 C23 -179.9(3) . . . . ? C21 C22 C23 O23 177.8(3) . . . . ? C21 C22 C23 C24 0.7(4) . . . . ? C22 C23 C24 C25 -2.2(5) . . . . ? O23 C23 C24 C25 -179.3(3) . . . . ? C22 C23 C24 O24 178.9(3) . . . . ? O23 C23 C24 O24 1.9(5) . . . . ? O24 C24 C25 C26 -178.9(3) . . . . ? C23 C24 C25 C26 2.2(4) . . . . ? C22 C21 C26 C25 -0.9(4) . . . . ? C20 C21 C26 C25 179.9(2) . . . . ? C24 C25 C26 C21 -0.6(4) . . . . ? C33 P2 C27 C32 128.1(2) . . . . ? C20 P2 C27 C32 -121.1(2) . . . . ? Ag1 P2 C27 C32 5.9(3) . . . . ? C33 P2 C27 C28 -53.7(3) . . . . ? C20 P2 C27 C28 57.1(2) . . . . ? Ag1 P2 C27 C28 -175.86(19) . . . . ? C32 C27 C28 C29 0.1(4) . . . . ? P2 C27 C28 C29 -178.1(2) . . . . ? C27 C28 C29 C30 -0.5(4) . . . . ? C28 C29 C30 C31 0.7(5) . . . . ? C29 C30 C31 C32 -0.5(4) . . . . ? C30 C31 C32 C27 0.1(4) . . . . ? C28 C27 C32 C31 0.1(4) . . . . ? P2 C27 C32 C31 178.3(2) . . . . ? C27 P2 C33 C34 120.0(2) . . . . ? C20 P2 C33 C34 10.4(3) . . . . ? Ag1 P2 C33 C34 -114.2(2) . . . . ? C27 P2 C33 C38 -65.3(2) . . . . ? C20 P2 C33 C38 -174.9(2) . . . . ? Ag1 P2 C33 C38 60.5(2) . . . . ? C38 C33 C34 C35 0.3(4) . . . . ? P2 C33 C34 C35 174.9(2) . . . . ? C33 C34 C35 C36 -0.2(4) . . . . ? C34 C35 C36 C37 0.2(4) . . . . ? C35 C36 C37 C38 -0.3(5) . . . . ? C36 C37 C38 C33 0.3(4) . . . . ? C34 C33 C38 C37 -0.3(4) . . . . ? P2 C33 C38 C37 -175.3(2) . . . . ? O2 S1 O1 Ag1 21.8(3) . . . . ? O3 S1 O1 Ag1 -115.4(2) . . . . ? C39 S1 O1 Ag1 133.9(3) . . . . ? P2 Ag1 O1 S1 40.9(3) . . . . ? P1 Ag1 O1 S1 -135.7(2) . . . . ? O2 S1 C39 F2 -59.3(2) . . . . ? O1 S1 C39 F2 179.6(2) . . . . ? O3 S1 C39 F2 60.4(2) . . . . ? O2 S1 C39 F1 -180.0(2) . . . . ? O1 S1 C39 F1 59.0(2) . . . . ? O3 S1 C39 F1 -60.3(2) . . . . ? O2 S1 C39 F3 60.5(2) . . . . ? O1 S1 C39 F3 -60.6(2) . . . . ? O3 S1 C39 F3 -179.8(2) . . . . ? C4T O1T C1T C2T 13.4(3) . . . . ? O1T C1T C2T C3T -29.5(4) . . . . ? C1T C2T C3T C4T 33.9(4) . . . . ? C1T O1T C4T C3T 8.3(3) . . . . ? C2T C3T C4T O1T -26.7(4) . . . . ? C8T O2T C5T C6T 2.6(3) . . . . ? O2T C5T C6T C7T -25.3(3) . . . . ? C5T C6T C7T C8T 37.3(3) . . . . ? C5T O2T C8T C7T 21.5(3) . . . . ? C6T C7T C8T O2T -36.8(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 O4 H4 O1T 0.831(12) 1.895(14) 2.690(3) 160(3) . O5 H5 O3 0.846(12) 1.887(13) 2.730(3) 174(3) 2_645 O23 H23 O4 0.856(13) 1.987(17) 2.791(3) 156(3) 2_645 O24 H24 O2T 0.853(13) 1.927(15) 2.712(3) 152(2) . C1T H1T2 F1 0.99 2.55 3.460(4) 152.2 2_645 C18 H18 F2 0.95 2.52 3.273(4) 136.4 4_565 C9 H9 O1 0.95 2.59 3.475(4) 155.0 . C26 H26 O2 0.95 2.56 3.282(3) 132.6 . C1 H1B O2 0.99 2.37 3.353(3) 173.3 4_565 C19 H19 O2 0.95 2.55 3.291(4) 135.4 4_565 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.499 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.064 #============================================================================== data_gudat117_compound_6 _database_code_depnum_ccdc_archive 'CCDC 648047' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Triethylammonium Bisd-[(diphenylphosphine{benzo-(1,3)-dioxa-4- methyl}]-2-borate ; _chemical_name_common ;Triethylammonium Bisd-((diphenylphosphine(benzo-(1,3)-dioxa-4- methyl))-2-borate ; _chemical_melting_point ? _chemical_formula_moiety 'C38 H30 B O4 P2 - Et3NH - dme' _chemical_formula_sum 'C48 H56 B N O6 P2' _chemical_formula_weight 815.69 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' B B 0.0013 0.0007 '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' P P 0.1023 0.0942 '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 #(No.2) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.3386(2) _cell_length_b 16.3500(2) _cell_length_c 16.7372(2) _cell_angle_alpha 84.929(1) _cell_angle_beta 88.028(1) _cell_angle_gamma 89.833(1) _cell_volume 4450.97(9) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 13926 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description rods _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 0.146 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; dx = 40 mm, 90 sec./deg., 1 deg., 6 sets, 435 frames, mos.= 0.482(1) deg. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius kappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 1 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46944 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.48 _reflns_number_total 19875 _reflns_number_gt 13517 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. There are two crystallographic independent units in the asymmetric unit. Restraints (for geometry and displacmentparameters) were used for the refinement of the two kations (Et3NH), one of them is well defined and used as a model for the second one, as well as for the 4 dmf solvent molecules. 3 dmf miolecules are well defined and user as a model for the fourth one. Used are SADI, SAME and SIMU restraints. ; _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^)+(0.1438P)^2^+0.8736P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19875 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 353 _refine_ls_R_factor_all 0.1036 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.2398 _refine_ls_wR_factor_gt 0.2187 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.218 _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 B1 B 0.8193(2) 1.0350(2) 0.7623(2) 0.0239(7) Uani 1 1 d . . . O1 O 0.87305(13) 1.06563(13) 0.82234(12) 0.0241(5) Uani 1 1 d . . . O2 O 0.75829(13) 0.98159(13) 0.81268(12) 0.0245(5) Uani 1 1 d . . . C1 C 0.84632(18) 1.03314(18) 0.89667(17) 0.0203(6) Uani 1 1 d . . . C2 C 0.77813(18) 0.98317(18) 0.89100(18) 0.0217(6) Uani 1 1 d . . . C3 C 0.74078(19) 0.94284(19) 0.95812(19) 0.0255(7) Uani 1 1 d . . . H3 H 0.6945 0.9085 0.9543 0.031 Uiso 1 1 calc R . . C4 C 0.7737(2) 0.9545(2) 1.0320(2) 0.0281(7) Uani 1 1 d . . . H4 H 0.7495 0.9273 1.0795 0.034 Uiso 1 1 calc R . . C5 C 0.8406(2) 1.0047(2) 1.03780(19) 0.0265(7) Uani 1 1 d . . . H5 H 0.8612 1.0115 1.0892 0.032 Uiso 1 1 calc R . . C6 C 0.87942(18) 1.04635(18) 0.96890(18) 0.0216(6) Uani 1 1 d . . . C7 C 0.95189(18) 1.10235(19) 0.97276(19) 0.0245(7) Uani 1 1 d . . . H7A H 0.9799 1.1097 0.9192 0.029 Uiso 1 1 calc R . . H7B H 0.9911 1.0764 1.0110 0.029 Uiso 1 1 calc R . . P1 P 0.92190(5) 1.20442(5) 1.00462(5) 0.0234(2) Uani 1 1 d . . . C8 C 0.91770(18) 1.18697(19) 1.11472(19) 0.0244(7) Uani 1 1 d . . . C9 C 0.8633(2) 1.2333(2) 1.1572(2) 0.0379(9) Uani 1 1 d . . . H9 H 0.8266 1.2696 1.1290 0.046 Uiso 1 1 calc R . . C10 C 0.8616(3) 1.2277(3) 1.2404(2) 0.0452(10) Uani 1 1 d . . . H10 H 0.8238 1.2602 1.2682 0.054 Uiso 1 1 calc R . . C11 C 0.9134(2) 1.1759(2) 1.2829(2) 0.0394(9) Uani 1 1 d . . . H11 H 0.9122 1.1726 1.3399 0.047 Uiso 1 1 calc R . . C12 C 0.9676(3) 1.1283(3) 1.2414(2) 0.0456(10) Uani 1 1 d . . . H12 H 1.0035 1.0914 1.2700 0.055 Uiso 1 1 calc R . . C13 C 0.9696(2) 1.1343(2) 1.1587(2) 0.0403(9) Uani 1 1 d . . . H13 H 1.0074 1.1017 1.1312 0.048 Uiso 1 1 calc R . . C14 C 1.02063(19) 1.2591(2) 0.99152(18) 0.0261(7) Uani 1 1 d . . . C15 C 1.0191(2) 1.3438(2) 0.9768(2) 0.0319(8) Uani 1 1 d . . . H15 H 0.9681 1.3712 0.9702 0.038 Uiso 1 1 calc R . . C16 C 1.0909(2) 1.3892(2) 0.9716(2) 0.0395(9) Uani 1 1 d . . . H16 H 1.0887 1.4473 0.9615 0.047 Uiso 1 1 calc R . . C17 C 1.1650(2) 1.3505(2) 0.9811(2) 0.0408(9) Uani 1 1 d . . . H17 H 1.2142 1.3817 0.9782 0.049 Uiso 1 1 calc R . . C18 C 1.1678(2) 1.2665(2) 0.9948(2) 0.0421(9) Uani 1 1 d . . . H18 H 1.2192 1.2398 1.0009 0.050 Uiso 1 1 calc R . . C19 C 1.0962(2) 1.2200(2) 0.9997(2) 0.0360(8) Uani 1 1 d . . . H19 H 1.0989 1.1619 1.0086 0.043 Uiso 1 1 calc R . . O3 O 0.86389(13) 0.98657(13) 0.70393(12) 0.0239(5) Uani 1 1 d . . . O4 O 0.77843(13) 1.10085(13) 0.71428(12) 0.0246(5) Uani 1 1 d . . . C20 C 0.84622(18) 1.02147(18) 0.62952(18) 0.0210(6) Uani 1 1 d . . . C21 C 0.79522(18) 1.08979(18) 0.63578(18) 0.0229(6) Uani 1 1 d . . . C22 C 0.76669(19) 1.1339(2) 0.5691(2) 0.0290(7) Uani 1 1 d . . . H22 H 0.7319 1.1801 0.5733 0.035 Uiso 1 1 calc R . . C23 C 0.7912(2) 1.1078(2) 0.4940(2) 0.0303(7) Uani 1 1 d . . . H23 H 0.7719 1.1366 0.4466 0.036 Uiso 1 1 calc R . . C24 C 0.8425(2) 1.0417(2) 0.48771(19) 0.0289(7) Uani 1 1 d . . . H24 H 0.8586 1.0267 0.4359 0.035 Uiso 1 1 calc R . . C25 C 0.87179(18) 0.99553(19) 0.55640(18) 0.0220(6) Uani 1 1 d . . . C26 C 0.92711(19) 0.92169(19) 0.55171(19) 0.0250(7) Uani 1 1 d . . . H26A H 0.9502 0.9072 0.6050 0.030 Uiso 1 1 calc R . . H26B H 0.9732 0.9362 0.5132 0.030 Uiso 1 1 calc R . . P2 P 0.87332(5) 0.83143(5) 0.51998(5) 0.0251(2) Uani 1 1 d . . . C27 C 0.87196(19) 0.85217(19) 0.41016(19) 0.0253(7) Uani 1 1 d . . . C28 C 0.9355(2) 0.8883(2) 0.36140(19) 0.0314(8) Uani 1 1 d . . . H28 H 0.9838 0.9050 0.3855 0.038 Uiso 1 1 calc R . . C29 C 0.9298(2) 0.9002(2) 0.2789(2) 0.0382(9) Uani 1 1 d . . . H29 H 0.9738 0.9251 0.2471 0.046 Uiso 1 1 calc R . . C30 C 0.8604(3) 0.8762(3) 0.2430(3) 0.0508(11) Uani 1 1 d . . . H30 H 0.8564 0.8834 0.1864 0.061 Uiso 1 1 calc R . . C31 C 0.7965(3) 0.8415(3) 0.2905(3) 0.0610(13) Uani 1 1 d . . . H31 H 0.7483 0.8253 0.2660 0.073 Uiso 1 1 calc R . . C32 C 0.8015(2) 0.8299(2) 0.3737(3) 0.0435(9) Uani 1 1 d . . . H32 H 0.7566 0.8067 0.4054 0.052 Uiso 1 1 calc R . . C33 C 0.9550(2) 0.75400(19) 0.53482(18) 0.0248(7) Uani 1 1 d . . . C34 C 1.0352(2) 0.7646(2) 0.50472(19) 0.0289(7) Uani 1 1 d . . . H34 H 1.0500 0.8133 0.4724 0.035 Uiso 1 1 calc R . . C35 C 1.0936(2) 0.7041(2) 0.5218(2) 0.0308(7) Uani 1 1 d . . . H35 H 1.1484 0.7123 0.5019 0.037 Uiso 1 1 calc R . . C36 C 1.0726(2) 0.6321(2) 0.5677(2) 0.0352(8) Uani 1 1 d . . . H36 H 1.1124 0.5904 0.5782 0.042 Uiso 1 1 calc R . . C37 C 0.9934(2) 0.6213(2) 0.5982(2) 0.0396(9) Uani 1 1 d . . . H37 H 0.9788 0.5723 0.6303 0.048 Uiso 1 1 calc R . . C38 C 0.9349(2) 0.6817(2) 0.5819(2) 0.0345(8) Uani 1 1 d . . . H38 H 0.8805 0.6737 0.6031 0.041 Uiso 1 1 calc R . . N1 N 0.68425(19) 0.8506(2) 0.7512(2) 0.0682(12) Uani 1 1 d DU . . H1 H 0.7108 0.8946 0.7706 0.082 Uiso 1 1 calc R . . C39 C 0.6016(2) 0.8449(2) 0.7923(2) 0.0416(9) Uani 1 1 d DU . . H39A H 0.5723 0.8974 0.7805 0.050 Uiso 1 1 calc R . . H39B H 0.6085 0.8371 0.8511 0.050 Uiso 1 1 calc R . . C40 C 0.5502(3) 0.7762(3) 0.7676(3) 0.0624(13) Uani 1 1 d DU . . H40A H 0.4963 0.7771 0.7949 0.094 Uiso 1 1 calc R . . H40B H 0.5771 0.7236 0.7822 0.094 Uiso 1 1 calc R . . H40C H 0.5437 0.7830 0.7094 0.094 Uiso 1 1 calc R . . C41 C 0.6780(4) 0.8707(5) 0.6626(3) 0.135(3) Uani 1 1 d DU . . H41A H 0.7338 0.8735 0.6374 0.162 Uiso 1 1 calc R . . H41B H 0.6481 0.8260 0.6398 0.162 Uiso 1 1 calc R . . C42 C 0.6354(5) 0.9495(5) 0.6425(4) 0.183(5) Uani 1 1 d DU . . H42A H 0.6327 0.9598 0.5841 0.275 Uiso 1 1 calc R . . H42B H 0.6654 0.9941 0.6638 0.275 Uiso 1 1 calc R . . H42C H 0.5797 0.9466 0.6664 0.275 Uiso 1 1 calc R . . C43 C 0.7331(4) 0.7754(3) 0.7763(5) 0.151(3) Uani 1 1 d DU . . H43A H 0.7068 0.7514 0.8271 0.181 Uiso 1 1 calc R . . H43B H 0.7235 0.7361 0.7358 0.181 Uiso 1 1 calc R . . C44 C 0.8158(5) 0.7737(4) 0.7881(6) 0.153(4) Uani 1 1 d DU . . H44A H 0.8318 0.7185 0.8097 0.229 Uiso 1 1 calc R . . H44B H 0.8293 0.8134 0.8262 0.229 Uiso 1 1 calc R . . H44C H 0.8455 0.7879 0.7369 0.229 Uiso 1 1 calc R . . B1' B 0.7006(2) 0.5398(2) 0.7523(2) 0.0224(7) Uani 1 1 d . . . O1' O 0.64176(12) 0.57221(13) 0.81193(12) 0.0219(5) Uani 1 1 d . . . O2' O 0.76261(12) 0.49471(13) 0.80283(12) 0.0229(5) Uani 1 1 d . . . C1' C 0.66337(17) 0.54056(18) 0.88545(17) 0.0193(6) Uani 1 1 d . . . C2' C 0.73459(18) 0.49355(18) 0.88113(18) 0.0212(6) Uani 1 1 d . . . C3' C 0.76709(19) 0.45305(19) 0.94796(19) 0.0254(7) Uani 1 1 d . . . H3' H 0.8155 0.4210 0.9444 0.030 Uiso 1 1 calc R . . C4' C 0.7260(2) 0.46088(19) 1.02177(19) 0.0271(7) Uani 1 1 d . . . H4' H 0.7461 0.4328 1.0692 0.033 Uiso 1 1 calc R . . C5' C 0.65609(19) 0.50924(19) 1.02633(18) 0.0245(7) Uani 1 1 d . . . H5' H 0.6300 0.5143 1.0773 0.029 Uiso 1 1 calc R . . C6' C 0.62308(18) 0.55057(18) 0.95836(18) 0.0211(6) Uani 1 1 d . . . C7' C 0.54843(18) 0.60498(19) 0.96081(19) 0.0235(6) Uani 1 1 d . . . H7'1 H 0.5058 0.5778 0.9974 0.028 Uiso 1 1 calc R . . H7'2 H 0.5259 0.6134 0.9065 0.028 Uiso 1 1 calc R . . P1' P 0.57474(5) 0.70636(5) 0.99613(5) 0.02247(19) Uani 1 1 d . . . C8' C 0.57951(19) 0.67669(19) 1.10452(19) 0.0253(7) Uani 1 1 d . . . C9' C 0.5174(2) 0.6325(2) 1.14760(19) 0.0305(7) Uani 1 1 d . . . H9' H 0.4687 0.6205 1.1215 0.037 Uiso 1 1 calc R . . C10' C 0.5251(3) 0.6058(2) 1.2273(2) 0.0397(9) Uani 1 1 d . . . H10' H 0.4818 0.5762 1.2558 0.048 Uiso 1 1 calc R . . C11' C 0.5956(3) 0.6220(3) 1.2655(2) 0.0503(11) Uani 1 1 d . . . H11' H 0.6013 0.6026 1.3202 0.060 Uiso 1 1 calc R . . C12' C 0.6581(3) 0.6663(3) 1.2248(2) 0.0473(10) Uani 1 1 d . . . H12' H 0.7067 0.6777 1.2513 0.057 Uiso 1 1 calc R . . C13' C 0.6495(2) 0.6943(2) 1.1443(2) 0.0340(8) Uani 1 1 d . . . H13' H 0.6921 0.7257 1.1164 0.041 Uiso 1 1 calc R . . C14' C 0.4757(2) 0.7592(2) 0.99370(19) 0.0271(7) Uani 1 1 d . . . C15' C 0.4003(2) 0.7223(2) 0.9861(2) 0.0335(8) Uani 1 1 d . . . H15' H 0.3979 0.6653 0.9790 0.040 Uiso 1 1 calc R . . C16' C 0.3285(2) 0.7672(2) 0.9886(2) 0.0400(9) Uani 1 1 d . . . H16' H 0.2776 0.7410 0.9822 0.048 Uiso 1 1 calc R . . C17' C 0.3301(2) 0.8489(3) 1.0002(3) 0.0461(10) Uani 1 1 d . . . H17' H 0.2805 0.8791 1.0033 0.055 Uiso 1 1 calc R . . C18' C 0.4041(3) 0.8868(3) 1.0073(3) 0.0615(13) Uani 1 1 d . . . H18' H 0.4058 0.9437 1.0149 0.074 Uiso 1 1 calc R . . C19' C 0.4762(2) 0.8424(2) 1.0036(3) 0.0487(11) Uani 1 1 d . . . H19' H 0.5270 0.8695 1.0079 0.058 Uiso 1 1 calc R . . O3' O 0.66091(12) 0.48228(12) 0.70142(12) 0.0219(5) Uani 1 1 d . . . O4' O 0.73408(13) 0.60620(13) 0.69643(12) 0.0238(5) Uani 1 1 d . . . C20' C 0.66246(17) 0.52052(18) 0.62526(17) 0.0196(6) Uani 1 1 d . . . C21' C 0.70509(18) 0.59465(19) 0.62267(18) 0.0219(6) Uani 1 1 d . . . C22' C 0.71177(19) 0.6463(2) 0.55321(19) 0.0263(7) Uani 1 1 d . . . H22' H 0.7389 0.6977 0.5516 0.032 Uiso 1 1 calc R . . C23' C 0.6767(2) 0.6193(2) 0.48496(19) 0.0293(7) Uani 1 1 d . . . H23' H 0.6803 0.6534 0.4360 0.035 Uiso 1 1 calc R . . C24' C 0.63721(19) 0.5451(2) 0.48680(19) 0.0264(7) Uani 1 1 d . . . H24' H 0.6154 0.5287 0.4388 0.032 Uiso 1 1 calc R . . C25' C 0.62823(18) 0.49256(19) 0.55812(18) 0.0223(6) Uani 1 1 d . . . C26' C 0.58188(19) 0.41375(19) 0.56287(18) 0.0232(6) Uani 1 1 d . . . H26C H 0.5288 0.4236 0.5368 0.028 Uiso 1 1 calc R . . H26D H 0.5700 0.3952 0.6200 0.028 Uiso 1 1 calc R . . P2' P 0.63733(5) 0.33074(5) 0.51457(5) 0.0271(2) Uani 1 1 d . . . C27' C 0.62422(19) 0.3608(2) 0.40725(19) 0.0270(7) Uani 1 1 d . . . C28' C 0.5474(2) 0.3763(2) 0.3743(2) 0.0292(7) Uani 1 1 d . . . H28' H 0.4995 0.3731 0.4083 0.035 Uiso 1 1 calc R . . C29' C 0.5405(2) 0.3960(2) 0.2936(2) 0.0338(8) Uani 1 1 d . . . H29' H 0.4882 0.4071 0.2720 0.041 Uiso 1 1 calc R . . C30' C 0.6095(2) 0.3997(2) 0.2436(2) 0.0392(9) Uani 1 1 d . . . H30' H 0.6043 0.4124 0.1875 0.047 Uiso 1 1 calc R . . C31' C 0.6854(2) 0.3853(3) 0.2741(2) 0.0450(10) Uani 1 1 d . . . H31' H 0.7327 0.3885 0.2393 0.054 Uiso 1 1 calc R . . C32' C 0.6932(2) 0.3660(2) 0.3565(2) 0.0351(8) Uani 1 1 d . . . H32' H 0.7459 0.3564 0.3777 0.042 Uiso 1 1 calc R . . C33' C 0.5618(2) 0.2469(2) 0.5293(2) 0.0328(8) Uani 1 1 d . . . C34' C 0.5680(3) 0.1838(2) 0.4785(3) 0.0458(10) Uani 1 1 d . . . H34' H 0.6096 0.1857 0.4373 0.055 Uiso 1 1 calc R . . C35' C 0.5141(3) 0.1189(3) 0.4878(3) 0.0601(13) Uani 1 1 d . . . H35' H 0.5192 0.0761 0.4530 0.072 Uiso 1 1 calc R . . C36' C 0.4535(3) 0.1148(3) 0.5462(4) 0.0716(15) Uani 1 1 d . . . H36' H 0.4164 0.0699 0.5516 0.086 Uiso 1 1 calc R . . C37' C 0.4465(3) 0.1762(3) 0.5972(4) 0.0741(16) Uani 1 1 d . . . H37' H 0.4044 0.1739 0.6378 0.089 Uiso 1 1 calc R . . C38' C 0.5017(3) 0.2420(3) 0.5890(3) 0.0544(11) Uani 1 1 d . . . H38' H 0.4975 0.2836 0.6251 0.065 Uiso 1 1 calc R . . N1' N 0.82118(17) 0.34413(18) 0.75655(18) 0.0433(8) Uani 1 1 d DU . . H1' H 0.7986 0.3922 0.7734 0.052 Uiso 1 1 calc R . . C39' C 0.9047(2) 0.3391(2) 0.7884(2) 0.0377(8) Uani 1 1 d DU . . H39C H 0.9003 0.3353 0.8477 0.045 Uiso 1 1 calc R . . H39D H 0.9344 0.3905 0.7702 0.045 Uiso 1 1 calc R . . C40' C 0.9542(2) 0.2674(2) 0.7631(3) 0.0486(10) Uani 1 1 d DU . . H40D H 1.0087 0.2686 0.7858 0.073 Uiso 1 1 calc R . . H40E H 0.9597 0.2710 0.7044 0.073 Uiso 1 1 calc R . . H40F H 0.9265 0.2161 0.7826 0.073 Uiso 1 1 calc R . . C41' C 0.8153(3) 0.3512(3) 0.6686(2) 0.0537(11) Uani 1 1 d DU . . H41C H 0.7569 0.3541 0.6546 0.064 Uiso 1 1 calc R . . H41D H 0.8392 0.3016 0.6471 0.064 Uiso 1 1 calc R . . C42' C 0.8600(3) 0.4274(3) 0.6296(3) 0.0624(13) Uani 1 1 d DU . . H42D H 0.8550 0.4300 0.5712 0.094 Uiso 1 1 calc R . . H42E H 0.9179 0.4242 0.6427 0.094 Uiso 1 1 calc R . . H42F H 0.8356 0.4766 0.6499 0.094 Uiso 1 1 calc R . . C43' C 0.7683(3) 0.2740(2) 0.7976(3) 0.0541(11) Uani 1 1 d DU . . H43C H 0.7870 0.2217 0.7774 0.065 Uiso 1 1 calc R . . H43D H 0.7775 0.2702 0.8560 0.065 Uiso 1 1 calc R . . C44' C 0.6819(3) 0.2827(3) 0.7854(4) 0.0718(15) Uani 1 1 d DU . . H44D H 0.6528 0.2355 0.8132 0.108 Uiso 1 1 calc R . . H44E H 0.6718 0.2851 0.7279 0.108 Uiso 1 1 calc R . . H44F H 0.6622 0.3333 0.8068 0.108 Uiso 1 1 calc R . . C1D C 0.9632(3) 1.5905(3) 0.8181(3) 0.0668(14) Uani 1 1 d DU . . H1D1 H 0.9051 1.5793 0.8307 0.100 Uiso 1 1 calc R . . H1D2 H 0.9686 1.6324 0.7726 0.100 Uiso 1 1 calc R . . H1D3 H 0.9887 1.6104 0.8649 0.100 Uiso 1 1 calc R . . O1D O 1.00272(17) 1.51748(17) 0.79812(17) 0.0505(7) Uani 1 1 d DU . . C2D C 1.0868(2) 1.5289(3) 0.7796(3) 0.0494(10) Uani 1 1 d DU . . H2D1 H 1.1159 1.5386 0.8289 0.059 Uiso 1 1 calc R . . H2D2 H 1.0949 1.5776 0.7406 0.059 Uiso 1 1 calc R . . C3D C 1.1212(2) 1.4544(3) 0.7448(3) 0.0536(11) Uani 1 1 d DU . . H3D1 H 1.1811 1.4603 0.7358 0.064 Uiso 1 1 calc R . . H3D2 H 1.1104 1.4051 0.7824 0.064 Uiso 1 1 calc R . . O2D O 1.08376(19) 1.44571(18) 0.67137(17) 0.0541(8) Uani 1 1 d DU . . C4D C 1.1187(4) 1.3826(3) 0.6289(3) 0.0806(17) Uani 1 1 d DU . . H4D1 H 1.0904 1.3797 0.5785 0.121 Uiso 1 1 calc R . . H4D2 H 1.1130 1.3300 0.6615 0.121 Uiso 1 1 calc R . . H4D3 H 1.1769 1.3943 0.6171 0.121 Uiso 1 1 calc R . . C5D C 0.5613(5) 1.1013(5) 0.7803(7) 0.150(3) Uani 1 1 d DU . . H5D1 H 0.6149 1.0865 0.7578 0.225 Uiso 1 1 calc R . . H5D2 H 0.5671 1.1150 0.8357 0.225 Uiso 1 1 calc R . . H5D3 H 0.5396 1.1490 0.7481 0.225 Uiso 1 1 calc R . . O3D O 0.5075(3) 1.0352(3) 0.7794(5) 0.158(2) Uani 1 1 d DU . . C6D C 0.4318(4) 1.0394(5) 0.8062(7) 0.164(3) Uani 1 1 d DU . . H6D1 H 0.4115 1.0951 0.7892 0.197 Uiso 1 1 calc R . . H6D2 H 0.4327 1.0348 0.8655 0.197 Uiso 1 1 calc R . . C7D C 0.3706(4) 0.9806(4) 0.7838(6) 0.139(2) Uani 1 1 d DU . . H7D1 H 0.3373 0.9617 0.8324 0.167 Uiso 1 1 calc R . . H7D2 H 0.3335 1.0098 0.7454 0.167 Uiso 1 1 calc R . . O4D O 0.4012(4) 0.9127(4) 0.7501(5) 0.188(2) Uani 1 1 d DU . . C8D C 0.3433(7) 0.8496(6) 0.7429(8) 0.199(4) Uani 1 1 d DU . . H8D1 H 0.3701 0.8040 0.7182 0.298 Uiso 1 1 calc R . . H8D2 H 0.2988 0.8712 0.7092 0.298 Uiso 1 1 calc R . . H8D3 H 0.3209 0.8302 0.7962 0.298 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 B1 0.0268(18) 0.0205(17) 0.0257(18) -0.0092(14) -0.0014(14) -0.0028(14) O1 0.0247(11) 0.0271(12) 0.0215(11) -0.0082(9) 0.0016(9) -0.0060(9) O2 0.0253(11) 0.0267(12) 0.0229(11) -0.0082(9) -0.0032(9) -0.0053(9) C1 0.0197(14) 0.0183(14) 0.0234(15) -0.0044(12) 0.0011(12) 0.0029(11) C2 0.0196(14) 0.0209(15) 0.0254(15) -0.0059(12) -0.0015(12) 0.0022(11) C3 0.0199(15) 0.0236(16) 0.0332(17) -0.0039(13) 0.0005(13) -0.0003(12) C4 0.0259(16) 0.0277(17) 0.0292(17) 0.0038(14) 0.0031(13) 0.0004(13) C5 0.0267(16) 0.0304(17) 0.0229(15) -0.0038(13) -0.0041(13) 0.0031(13) C6 0.0192(14) 0.0222(15) 0.0244(15) -0.0065(12) -0.0021(12) 0.0015(11) C7 0.0175(14) 0.0311(17) 0.0266(16) -0.0101(13) -0.0037(12) 0.0003(12) P1 0.0202(4) 0.0259(4) 0.0248(4) -0.0049(3) -0.0053(3) 0.0016(3) C8 0.0191(15) 0.0275(17) 0.0275(16) -0.0075(13) -0.0021(12) -0.0018(12) C9 0.039(2) 0.041(2) 0.0340(19) -0.0057(16) 0.0009(16) 0.0139(16) C10 0.046(2) 0.054(3) 0.036(2) -0.0124(18) 0.0064(18) 0.0147(19) C11 0.047(2) 0.048(2) 0.0234(17) -0.0079(16) -0.0005(16) 0.0007(18) C12 0.053(2) 0.055(3) 0.0290(19) -0.0043(18) -0.0098(17) 0.016(2) C13 0.042(2) 0.051(2) 0.0288(18) -0.0102(17) -0.0067(16) 0.0175(18) C14 0.0257(16) 0.0313(18) 0.0218(15) -0.0032(13) -0.0044(13) -0.0024(13) C15 0.0340(18) 0.0314(19) 0.0311(18) -0.0053(15) -0.0059(15) 0.0000(14) C16 0.046(2) 0.034(2) 0.039(2) -0.0037(16) -0.0016(17) -0.0110(16) C17 0.033(2) 0.044(2) 0.046(2) -0.0053(18) 0.0023(17) -0.0145(16) C18 0.0240(18) 0.045(2) 0.056(2) -0.0012(19) 0.0001(17) -0.0065(15) C19 0.0265(17) 0.034(2) 0.047(2) -0.0007(16) 0.0006(16) -0.0040(14) O3 0.0317(12) 0.0215(11) 0.0188(10) -0.0036(9) -0.0022(9) 0.0030(9) O4 0.0273(11) 0.0231(11) 0.0244(11) -0.0079(9) -0.0006(9) 0.0024(9) C20 0.0194(14) 0.0204(15) 0.0232(15) -0.0017(12) -0.0030(12) -0.0029(11) C21 0.0208(15) 0.0224(16) 0.0263(16) -0.0068(13) -0.0005(12) -0.0025(12) C22 0.0230(16) 0.0274(17) 0.0367(18) -0.0022(14) -0.0035(14) 0.0040(13) C23 0.0297(17) 0.0323(19) 0.0285(17) 0.0013(14) -0.0053(14) 0.0050(14) C24 0.0303(17) 0.0318(18) 0.0250(16) -0.0044(14) -0.0008(13) 0.0012(14) C25 0.0200(15) 0.0245(16) 0.0220(15) -0.0048(12) -0.0011(12) -0.0004(12) C26 0.0259(16) 0.0270(17) 0.0232(15) -0.0077(13) -0.0017(13) 0.0032(13) P2 0.0234(4) 0.0241(4) 0.0274(4) -0.0025(3) 0.0042(3) -0.0017(3) C27 0.0257(16) 0.0208(16) 0.0300(16) -0.0042(13) -0.0061(13) 0.0023(12) C28 0.0261(17) 0.042(2) 0.0264(17) -0.0070(15) -0.0006(14) 0.0030(14) C29 0.043(2) 0.042(2) 0.0292(18) -0.0027(16) -0.0012(16) 0.0152(17) C30 0.078(3) 0.038(2) 0.038(2) -0.0030(18) -0.021(2) 0.002(2) C31 0.074(3) 0.050(3) 0.059(3) 0.010(2) -0.044(3) -0.019(2) C32 0.041(2) 0.034(2) 0.055(2) 0.0099(18) -0.0209(18) -0.0118(16) C33 0.0303(17) 0.0219(16) 0.0228(15) -0.0051(13) -0.0005(13) -0.0001(13) C34 0.0341(18) 0.0256(17) 0.0270(16) -0.0040(13) 0.0048(14) 0.0025(13) C35 0.0328(18) 0.0317(18) 0.0283(17) -0.0061(14) 0.0023(14) 0.0054(14) C36 0.040(2) 0.0324(19) 0.0329(18) -0.0015(15) -0.0064(16) 0.0070(15) C37 0.041(2) 0.032(2) 0.044(2) 0.0119(16) -0.0084(17) -0.0033(16) C38 0.0321(18) 0.035(2) 0.0350(19) 0.0067(15) -0.0046(15) -0.0032(15) N1 0.043(2) 0.068(2) 0.103(3) -0.068(2) 0.017(2) -0.0228(17) C39 0.042(2) 0.039(2) 0.044(2) -0.0040(17) 0.0006(17) -0.0142(17) C40 0.062(3) 0.057(3) 0.069(3) 0.000(2) -0.011(2) -0.031(2) C41 0.106(5) 0.230(7) 0.082(4) -0.103(5) 0.057(4) -0.117(5) C42 0.184(9) 0.311(12) 0.048(3) 0.051(6) -0.044(5) -0.199(9) C43 0.088(4) 0.059(3) 0.321(8) -0.108(5) 0.013(6) -0.003(3) C44 0.231(10) 0.069(4) 0.172(8) -0.048(5) -0.118(7) 0.048(6) B1' 0.0232(17) 0.0203(17) 0.0251(17) -0.0097(14) 0.0000(14) 0.0012(13) O1' 0.0216(11) 0.0241(11) 0.0211(10) -0.0071(9) -0.0038(8) 0.0056(8) O2' 0.0229(11) 0.0253(11) 0.0217(11) -0.0079(9) -0.0010(9) 0.0053(9) C1' 0.0187(14) 0.0203(15) 0.0195(14) -0.0039(12) -0.0044(11) -0.0014(11) C2' 0.0212(15) 0.0194(15) 0.0241(15) -0.0074(12) -0.0023(12) 0.0001(11) C3' 0.0216(15) 0.0216(16) 0.0339(17) -0.0064(13) -0.0064(13) 0.0048(12) C4' 0.0341(18) 0.0215(16) 0.0260(16) -0.0001(13) -0.0096(14) 0.0002(13) C5' 0.0273(16) 0.0241(16) 0.0222(15) -0.0036(13) 0.0005(13) -0.0036(12) C6' 0.0197(14) 0.0195(15) 0.0247(15) -0.0063(12) -0.0001(12) -0.0018(11) C7' 0.0184(14) 0.0263(16) 0.0265(16) -0.0067(13) 0.0011(12) 0.0001(12) P1' 0.0193(4) 0.0236(4) 0.0246(4) -0.0035(3) 0.0019(3) -0.0003(3) C8' 0.0251(16) 0.0251(16) 0.0265(16) -0.0075(13) 0.0011(13) 0.0017(12) C9' 0.0282(17) 0.0380(19) 0.0255(16) -0.0056(14) 0.0052(14) -0.0009(14) C10' 0.048(2) 0.044(2) 0.0266(18) -0.0011(16) 0.0069(16) -0.0046(17) C11' 0.066(3) 0.056(3) 0.0284(19) -0.0014(18) -0.0035(19) -0.002(2) C12' 0.049(2) 0.056(3) 0.039(2) -0.0105(19) -0.0185(19) -0.003(2) C13' 0.0310(18) 0.038(2) 0.0339(19) -0.0051(15) -0.0019(15) -0.0034(15) C14' 0.0269(16) 0.0260(17) 0.0283(17) -0.0040(13) 0.0030(13) 0.0036(13) C15' 0.0265(17) 0.0330(19) 0.042(2) -0.0106(16) -0.0045(15) 0.0050(14) C16' 0.0267(18) 0.047(2) 0.046(2) -0.0042(18) -0.0067(16) 0.0091(16) C17' 0.032(2) 0.044(2) 0.062(3) -0.004(2) 0.0015(18) 0.0166(17) C18' 0.045(2) 0.031(2) 0.110(4) -0.017(2) 0.000(3) 0.0115(18) C19' 0.031(2) 0.028(2) 0.088(3) -0.013(2) 0.002(2) 0.0015(15) O3' 0.0247(11) 0.0232(11) 0.0185(10) -0.0052(9) -0.0003(8) -0.0043(8) O4' 0.0274(11) 0.0224(11) 0.0224(11) -0.0060(9) -0.0034(9) -0.0025(9) C20' 0.0174(14) 0.0237(15) 0.0177(14) -0.0026(12) -0.0001(11) 0.0023(11) C21' 0.0195(14) 0.0240(16) 0.0229(15) -0.0063(12) -0.0002(12) -0.0001(12) C22' 0.0253(16) 0.0247(16) 0.0286(17) -0.0016(13) -0.0001(13) -0.0043(12) C23' 0.0302(17) 0.0330(18) 0.0237(16) 0.0024(14) 0.0000(13) 0.0001(14) C24' 0.0258(16) 0.0323(18) 0.0213(15) -0.0030(13) -0.0039(13) 0.0022(13) C25' 0.0190(14) 0.0252(16) 0.0235(15) -0.0068(13) -0.0002(12) 0.0015(12) C26' 0.0238(15) 0.0257(16) 0.0212(15) -0.0074(12) -0.0028(12) -0.0025(12) P2' 0.0247(4) 0.0286(5) 0.0299(4) -0.0096(4) -0.0089(3) 0.0045(3) C27' 0.0253(16) 0.0274(17) 0.0303(17) -0.0132(14) -0.0038(13) 0.0026(13) C28' 0.0236(16) 0.0342(18) 0.0319(17) -0.0126(15) -0.0066(13) 0.0046(13) C29' 0.0359(19) 0.0316(19) 0.0351(19) -0.0065(15) -0.0122(15) 0.0018(15) C30' 0.048(2) 0.036(2) 0.0329(19) -0.0011(16) -0.0051(17) -0.0020(17) C31' 0.040(2) 0.056(3) 0.039(2) -0.0057(19) 0.0075(17) 0.0007(18) C32' 0.0259(17) 0.043(2) 0.038(2) -0.0119(16) -0.0022(15) 0.0028(15) C33' 0.0337(18) 0.0246(17) 0.041(2) -0.0054(15) -0.0145(16) 0.0026(14) C34' 0.048(2) 0.032(2) 0.061(3) -0.0166(19) -0.018(2) 0.0052(17) C35' 0.065(3) 0.034(2) 0.087(4) -0.023(2) -0.032(3) -0.001(2) C36' 0.071(3) 0.035(3) 0.110(5) -0.008(3) -0.022(3) -0.015(2) C37' 0.072(3) 0.051(3) 0.100(4) -0.014(3) 0.016(3) -0.026(3) C38' 0.067(3) 0.035(2) 0.062(3) -0.014(2) 0.003(2) -0.017(2) N1' 0.0487(19) 0.0321(16) 0.0534(19) -0.0226(15) -0.0154(15) 0.0144(14) C39' 0.038(2) 0.0309(19) 0.045(2) -0.0087(16) -0.0079(16) 0.0069(15) C40' 0.039(2) 0.041(2) 0.068(3) -0.013(2) -0.008(2) 0.0129(18) C41' 0.058(3) 0.058(3) 0.049(2) -0.024(2) -0.009(2) 0.016(2) C42' 0.059(3) 0.074(3) 0.058(3) -0.034(2) 0.024(2) -0.005(2) C43' 0.067(3) 0.033(2) 0.063(3) -0.0102(19) 0.012(2) -0.004(2) C44' 0.077(4) 0.049(3) 0.087(4) 0.010(3) 0.001(3) -0.006(3) C1D 0.074(3) 0.065(3) 0.065(3) -0.031(2) 0.021(3) -0.014(2) O1D 0.0480(16) 0.0474(16) 0.0566(17) -0.0108(14) 0.0072(14) -0.0170(13) C2D 0.045(2) 0.054(2) 0.049(2) -0.0008(19) -0.0104(18) -0.0171(18) C3D 0.037(2) 0.057(3) 0.065(3) 0.010(2) -0.0096(19) -0.0041(18) O2D 0.0591(18) 0.0525(17) 0.0509(17) -0.0061(14) -0.0020(14) 0.0184(14) C4D 0.079(4) 0.075(3) 0.087(4) -0.018(3) 0.033(3) 0.016(3) C5D 0.098(5) 0.107(5) 0.241(8) 0.009(6) 0.006(6) -0.046(4) O3D 0.077(3) 0.094(3) 0.299(6) 0.002(4) 0.000(4) -0.017(3) C6D 0.105(5) 0.131(5) 0.256(7) -0.035(5) 0.041(5) -0.039(4) C7D 0.087(4) 0.090(4) 0.247(6) -0.079(4) 0.082(4) -0.039(3) O4D 0.122(4) 0.157(5) 0.283(6) -0.027(5) 0.019(4) -0.036(4) C8D 0.149(7) 0.171(7) 0.277(9) -0.036(7) 0.022(7) -0.058(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O4 1.460(4) . ? B1 O1 1.478(4) . ? B1 O3 1.481(4) . ? B1 O2 1.511(4) . ? O1 C1 1.367(4) . ? O2 C2 1.364(4) . ? C1 C6 1.375(4) . ? C1 C2 1.394(4) . ? C2 C3 1.376(4) . ? C3 C4 1.395(5) . ? C3 H3 0.9500 . ? C4 C5 1.380(5) . ? C4 H4 0.9500 . ? C5 C6 1.417(4) . ? C5 H5 0.9500 . ? C6 C7 1.506(4) . ? C7 P1 1.856(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? P1 C8 1.839(3) . ? P1 C14 1.843(3) . ? C8 C9 1.385(4) . ? C8 C13 1.389(5) . ? C9 C10 1.386(5) . ? C9 H9 0.9500 . ? C10 C11 1.368(6) . ? C10 H10 0.9500 . ? C11 C12 1.387(5) . ? C11 H11 0.9500 . ? C12 C13 1.377(5) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.386(5) . ? C14 C19 1.394(5) . ? C15 C16 1.385(5) . ? C15 H15 0.9500 . ? C16 C17 1.373(6) . ? C16 H16 0.9500 . ? C17 C18 1.373(6) . ? C17 H17 0.9500 . ? C18 C19 1.393(5) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? O3 C20 1.363(4) . ? O4 C21 1.361(4) . ? C20 C25 1.381(4) . ? C20 C21 1.401(4) . ? C21 C22 1.369(5) . ? C22 C23 1.407(5) . ? C22 H22 0.9500 . ? C23 C24 1.373(4) . ? C23 H23 0.9500 . ? C24 C25 1.416(4) . ? C24 H24 0.9500 . ? C25 C26 1.512(4) . ? C26 P2 1.847(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? P2 C27 1.840(3) . ? P2 C33 1.844(3) . ? C27 C32 1.385(5) . ? C27 C28 1.398(5) . ? C28 C29 1.383(5) . ? C28 H28 0.9500 . ? C29 C30 1.376(6) . ? C29 H29 0.9500 . ? C30 C31 1.381(7) . ? C30 H30 0.9500 . ? C31 C32 1.395(6) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.393(4) . ? C33 C38 1.395(5) . ? C34 C35 1.391(5) . ? C34 H34 0.9500 . ? C35 C36 1.386(5) . ? C35 H35 0.9500 . ? C36 C37 1.380(5) . ? C36 H36 0.9500 . ? C37 C38 1.389(5) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? N1 C39 1.494(4) . ? N1 C41 1.498(5) . ? N1 C43 1.500(5) . ? N1 H1 0.9300 . ? C39 C40 1.500(5) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.481(7) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.372(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? B1' O4' 1.464(4) . ? B1' O3' 1.488(4) . ? B1' O1' 1.492(4) . ? B1' O2' 1.493(4) . ? O1' C1' 1.350(4) . ? O2' C2' 1.372(3) . ? C1' C6' 1.389(4) . ? C1' C2' 1.396(4) . ? C2' C3' 1.371(4) . ? C3' C4' 1.402(4) . ? C3' H3' 0.9500 . ? C4' C5' 1.391(4) . ? C4' H4' 0.9500 . ? C5' C6' 1.395(4) . ? C5' H5' 0.9500 . ? C6' C7' 1.509(4) . ? C7' P1' 1.865(3) . ? C7' H7'1 0.9900 . ? C7' H7'2 0.9900 . ? P1' C14' 1.833(3) . ? P1' C8' 1.840(3) . ? C8' C13' 1.386(5) . ? C8' C9' 1.391(5) . ? C9' C10' 1.376(5) . ? C9' H9' 0.9500 . ? C10' C11' 1.375(6) . ? C10' H10' 0.9500 . ? C11' C12' 1.379(6) . ? C11' H11' 0.9500 . ? C12' C13' 1.396(5) . ? C12' H12' 0.9500 . ? C13' H13' 0.9500 . ? C14' C19' 1.385(5) . ? C14' C15' 1.388(5) . ? C15' C16' 1.383(5) . ? C15' H15' 0.9500 . ? C16' C17' 1.368(6) . ? C16' H16' 0.9500 . ? C17' C18' 1.375(6) . ? C17' H17' 0.9500 . ? C18' C19' 1.384(5) . ? C18' H18' 0.9500 . ? C19' H19' 0.9500 . ? O3' C20' 1.369(4) . ? O4' C21' 1.366(4) . ? C20' C25' 1.386(4) . ? C20' C21' 1.396(4) . ? C21' C22' 1.376(4) . ? C22' C23' 1.401(5) . ? C22' H22' 0.9500 . ? C23' C24' 1.374(5) . ? C23' H23' 0.9500 . ? C24' C25' 1.411(4) . ? C24' H24' 0.9500 . ? C25' C26' 1.491(4) . ? C26' P2' 1.858(3) . ? C26' H26C 0.9900 . ? C26' H26D 0.9900 . ? P2' C27' 1.840(3) . ? P2' C33' 1.842(4) . ? C27' C32' 1.387(5) . ? C27' C28' 1.402(4) . ? C28' C29' 1.369(5) . ? C28' H28' 0.9500 . ? C29' C30' 1.379(5) . ? C29' H29' 0.9500 . ? C30' C31' 1.369(6) . ? C30' H30' 0.9500 . ? C31' C32' 1.398(5) . ? C31' H31' 0.9500 . ? C32' H32' 0.9500 . ? C33' C38' 1.373(6) . ? C33' C34' 1.396(5) . ? C34' C35' 1.376(6) . ? C34' H34' 0.9500 . ? C35' C36' 1.364(8) . ? C35' H35' 0.9500 . ? C36' C37' 1.376(7) . ? C36' H36' 0.9500 . ? C37' C38' 1.399(6) . ? C37' H37' 0.9500 . ? C38' H38' 0.9500 . ? N1' C41' 1.473(4) . ? N1' C39' 1.481(4) . ? N1' C43' 1.536(4) . ? N1' H1' 0.9300 . ? C39' C40' 1.505(4) . ? C39' H39C 0.9900 . ? C39' H39D 0.9900 . ? C40' H40D 0.9800 . ? C40' H40E 0.9800 . ? C40' H40F 0.9800 . ? C41' C42' 1.529(5) . ? C41' H41C 0.9900 . ? C41' H41D 0.9900 . ? C42' H42D 0.9800 . ? C42' H42E 0.9800 . ? C42' H42F 0.9800 . ? C43' C44' 1.439(5) . ? C43' H43C 0.9900 . ? C43' H43D 0.9900 . ? C44' H44D 0.9800 . ? C44' H44E 0.9800 . ? C44' H44F 0.9800 . ? C1D O1D 1.416(4) . ? C1D H1D1 0.9800 . ? C1D H1D2 0.9800 . ? C1D H1D3 0.9800 . ? O1D C2D 1.408(4) . ? C2D C3D 1.496(6) . ? C2D H2D1 0.9900 . ? C2D H2D2 0.9900 . ? C3D O2D 1.409(4) . ? C3D H3D1 0.9900 . ? C3D H3D2 0.9900 . ? O2D C4D 1.412(4) . ? C4D H4D1 0.9800 . ? C4D H4D2 0.9800 . ? C4D H4D3 0.9800 . ? C5D O3D 1.397(6) . ? C5D H5D1 0.9800 . ? C5D H5D2 0.9800 . ? C5D H5D3 0.9800 . ? O3D C6D 1.304(6) . ? C6D C7D 1.469(8) . ? C6D H6D1 0.9900 . ? C6D H6D2 0.9900 . ? C7D O4D 1.374(6) . ? C7D H7D1 0.9900 . ? C7D H7D2 0.9900 . ? O4D C8D 1.418(7) . ? C8D H8D1 0.9800 . ? C8D H8D2 0.9800 . ? C8D H8D3 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 B1 O1 112.9(3) . . ? O4 B1 O3 105.7(2) . . ? O1 B1 O3 113.1(3) . . ? O4 B1 O2 111.3(3) . . ? O1 B1 O2 103.4(2) . . ? O3 B1 O2 110.6(2) . . ? C1 O1 B1 108.1(2) . . ? C2 O2 B1 107.6(2) . . ? O1 C1 C6 126.7(3) . . ? O1 C1 C2 110.7(3) . . ? C6 C1 C2 122.6(3) . . ? O2 C2 C3 128.5(3) . . ? O2 C2 C1 110.1(3) . . ? C3 C2 C1 121.4(3) . . ? C2 C3 C4 117.2(3) . . ? C2 C3 H3 121.4 . . ? C4 C3 H3 121.4 . . ? C5 C4 C3 121.5(3) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 121.6(3) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C1 C6 C5 115.8(3) . . ? C1 C6 C7 121.0(3) . . ? C5 C6 C7 123.2(3) . . ? C6 C7 P1 112.3(2) . . ? C6 C7 H7A 109.1 . . ? P1 C7 H7A 109.1 . . ? C6 C7 H7B 109.1 . . ? P1 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? C8 P1 C14 98.78(14) . . ? C8 P1 C7 102.97(14) . . ? C14 P1 C7 100.67(14) . . ? C9 C8 C13 117.4(3) . . ? C9 C8 P1 118.2(3) . . ? C13 C8 P1 124.3(2) . . ? C8 C9 C10 121.0(3) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C11 C10 C9 121.0(3) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 118.8(3) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C13 C12 C11 120.2(4) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C8 121.7(3) . . ? C12 C13 H13 119.2 . . ? C8 C13 H13 119.2 . . ? C15 C14 C19 118.5(3) . . ? C15 C14 P1 118.0(2) . . ? C19 C14 P1 123.4(3) . . ? C16 C15 C14 121.0(3) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C17 C16 C15 120.2(4) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C18 C17 C16 119.6(4) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 120.9(4) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C18 C19 C14 119.8(3) . . ? C18 C19 H19 120.1 . . ? C14 C19 H19 120.1 . . ? C20 O3 B1 106.5(2) . . ? C21 O4 B1 107.3(2) . . ? O3 C20 C25 127.3(3) . . ? O3 C20 C21 110.3(2) . . ? C25 C20 C21 122.4(3) . . ? O4 C21 C22 128.3(3) . . ? O4 C21 C20 110.3(3) . . ? C22 C21 C20 121.4(3) . . ? C21 C22 C23 117.0(3) . . ? C21 C22 H22 121.5 . . ? C23 C22 H22 121.5 . . ? C24 C23 C22 121.6(3) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C23 C24 C25 121.7(3) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? C20 C25 C24 115.8(3) . . ? C20 C25 C26 121.1(3) . . ? C24 C25 C26 123.1(3) . . ? C25 C26 P2 112.8(2) . . ? C25 C26 H26A 109.0 . . ? P2 C26 H26A 109.0 . . ? C25 C26 H26B 109.0 . . ? P2 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? C27 P2 C33 103.38(14) . . ? C27 P2 C26 103.17(15) . . ? C33 P2 C26 99.40(14) . . ? C32 C27 C28 118.1(3) . . ? C32 C27 P2 116.5(3) . . ? C28 C27 P2 125.5(3) . . ? C29 C28 C27 121.5(3) . . ? C29 C28 H28 119.2 . . ? C27 C28 H28 119.2 . . ? C30 C29 C28 120.0(4) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 119.1(4) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C30 C31 C32 121.2(4) . . ? C30 C31 H31 119.4 . . ? C32 C31 H31 119.4 . . ? C27 C32 C31 120.0(4) . . ? C27 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C38 118.6(3) . . ? C34 C33 P2 124.3(2) . . ? C38 C33 P2 117.0(2) . . ? C35 C34 C33 120.3(3) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C36 C35 C34 120.5(3) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C37 C36 C35 119.6(3) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C36 C37 C38 120.2(3) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C37 C38 C33 120.8(3) . . ? C37 C38 H38 119.6 . . ? C33 C38 H38 119.6 . . ? C39 N1 C41 111.4(3) . . ? C39 N1 C43 109.6(4) . . ? C41 N1 C43 115.7(4) . . ? C39 N1 H1 106.5 . . ? C41 N1 H1 106.5 . . ? C43 N1 H1 106.5 . . ? N1 C39 C40 113.4(3) . . ? N1 C39 H39A 108.9 . . ? C40 C39 H39A 108.9 . . ? N1 C39 H39B 108.9 . . ? C40 C39 H39B 108.9 . . ? H39A C39 H39B 107.7 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 N1 112.5(4) . . ? C42 C41 H41A 109.1 . . ? N1 C41 H41A 109.1 . . ? C42 C41 H41B 109.1 . . ? N1 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 N1 125.5(5) . . ? C44 C43 H43A 105.9 . . ? N1 C43 H43A 105.9 . . ? C44 C43 H43B 105.9 . . ? N1 C43 H43B 105.9 . . ? H43A C43 H43B 106.3 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O4' B1' O3' 105.5(2) . . ? O4' B1' O1' 111.0(2) . . ? O3' B1' O1' 112.2(3) . . ? O4' B1' O2' 114.6(3) . . ? O3' B1' O2' 109.7(2) . . ? O1' B1' O2' 103.9(2) . . ? C1' O1' B1' 107.3(2) . . ? C2' O2' B1' 107.2(2) . . ? O1' C1' C6' 127.2(3) . . ? O1' C1' C2' 111.3(2) . . ? C6' C1' C2' 121.4(3) . . ? C3' C2' O2' 128.2(3) . . ? C3' C2' C1' 122.0(3) . . ? O2' C2' C1' 109.8(3) . . ? C2' C3' C4' 117.2(3) . . ? C2' C3' H3' 121.4 . . ? C4' C3' H3' 121.4 . . ? C5' C4' C3' 120.8(3) . . ? C5' C4' H4' 119.6 . . ? C3' C4' H4' 119.6 . . ? C4' C5' C6' 122.0(3) . . ? C4' C5' H5' 119.0 . . ? C6' C5' H5' 119.0 . . ? C1' C6' C5' 116.5(3) . . ? C1' C6' C7' 119.8(3) . . ? C5' C6' C7' 123.7(3) . . ? C6' C7' P1' 110.8(2) . . ? C6' C7' H7'1 109.5 . . ? P1' C7' H7'1 109.5 . . ? C6' C7' H7'2 109.5 . . ? P1' C7' H7'2 109.5 . . ? H7'1 C7' H7'2 108.1 . . ? C14' P1' C8' 99.86(14) . . ? C14' P1' C7' 102.01(14) . . ? C8' P1' C7' 99.57(14) . . ? C13' C8' C9' 118.2(3) . . ? C13' C8' P1' 119.2(3) . . ? C9' C8' P1' 122.4(3) . . ? C10' C9' C8' 121.2(3) . . ? C10' C9' H9' 119.4 . . ? C8' C9' H9' 119.4 . . ? C11' C10' C9' 120.0(4) . . ? C11' C10' H10' 120.0 . . ? C9' C10' H10' 120.0 . . ? C10' C11' C12' 120.2(4) . . ? C10' C11' H11' 119.9 . . ? C12' C11' H11' 119.9 . . ? C11' C12' C13' 119.6(4) . . ? C11' C12' H12' 120.2 . . ? C13' C12' H12' 120.2 . . ? C8' C13' C12' 120.7(3) . . ? C8' C13' H13' 119.7 . . ? C12' C13' H13' 119.7 . . ? C19' C14' C15' 117.5(3) . . ? C19' C14' P1' 116.9(3) . . ? C15' C14' P1' 125.5(2) . . ? C16' C15' C14' 121.0(3) . . ? C16' C15' H15' 119.5 . . ? C14' C15' H15' 119.5 . . ? C17' C16' C15' 120.7(4) . . ? C17' C16' H16' 119.7 . . ? C15' C16' H16' 119.7 . . ? C16' C17' C18' 119.3(3) . . ? C16' C17' H17' 120.4 . . ? C18' C17' H17' 120.4 . . ? C17' C18' C19' 120.2(4) . . ? C17' C18' H18' 119.9 . . ? C19' C18' H18' 119.9 . . ? C18' C19' C14' 121.3(4) . . ? C18' C19' H19' 119.4 . . ? C14' C19' H19' 119.4 . . ? C20' O3' B1' 106.2(2) . . ? C21' O4' B1' 106.8(2) . . ? O3' C20' C25' 127.1(3) . . ? O3' C20' C21' 110.3(3) . . ? C25' C20' C21' 122.6(3) . . ? O4' C21' C22' 128.3(3) . . ? O4' C21' C20' 110.5(3) . . ? C22' C21' C20' 121.2(3) . . ? C21' C22' C23' 116.9(3) . . ? C21' C22' H22' 121.6 . . ? C23' C22' H22' 121.6 . . ? C24' C23' C22' 121.9(3) . . ? C24' C23' H23' 119.0 . . ? C22' C23' H23' 119.0 . . ? C23' C24' C25' 121.7(3) . . ? C23' C24' H24' 119.1 . . ? C25' C24' H24' 119.1 . . ? C20' C25' C24' 115.6(3) . . ? C20' C25' C26' 121.5(3) . . ? C24' C25' C26' 122.8(3) . . ? C25' C26' P2' 113.5(2) . . ? C25' C26' H26C 108.9 . . ? P2' C26' H26C 108.9 . . ? C25' C26' H26D 108.9 . . ? P2' C26' H26D 108.9 . . ? H26C C26' H26D 107.7 . . ? C27' P2' C33' 99.37(16) . . ? C27' P2' C26' 102.21(14) . . ? C33' P2' C26' 101.01(15) . . ? C32' C27' C28' 118.7(3) . . ? C32' C27' P2' 118.4(3) . . ? C28' C27' P2' 122.9(2) . . ? C29' C28' C27' 120.7(3) . . ? C29' C28' H28' 119.6 . . ? C27' C28' H28' 119.6 . . ? C28' C29' C30' 120.0(3) . . ? C28' C29' H29' 120.0 . . ? C30' C29' H29' 120.0 . . ? C31' C30' C29' 120.6(4) . . ? C31' C30' H30' 119.7 . . ? C29' C30' H30' 119.7 . . ? C30' C31' C32' 119.9(3) . . ? C30' C31' H31' 120.0 . . ? C32' C31' H31' 120.0 . . ? C27' C32' C31' 120.1(3) . . ? C27' C32' H32' 120.0 . . ? C31' C32' H32' 120.0 . . ? C38' C33' C34' 118.5(4) . . ? C38' C33' P2' 123.6(3) . . ? C34' C33' P2' 117.8(3) . . ? C35' C34' C33' 120.3(4) . . ? C35' C34' H34' 119.9 . . ? C33' C34' H34' 119.9 . . ? C36' C35' C34' 121.1(4) . . ? C36' C35' H35' 119.5 . . ? C34' C35' H35' 119.5 . . ? C35' C36' C37' 119.6(5) . . ? C35' C36' H36' 120.2 . . ? C37' C36' H36' 120.2 . . ? C36' C37' C38' 119.8(5) . . ? C36' C37' H37' 120.1 . . ? C38' C37' H37' 120.1 . . ? C33' C38' C37' 120.7(4) . . ? C33' C38' H38' 119.7 . . ? C37' C38' H38' 119.7 . . ? C41' N1' C39' 116.7(3) . . ? C41' N1' C43' 112.4(3) . . ? C39' N1' C43' 109.6(3) . . ? C41' N1' H1' 105.7 . . ? C39' N1' H1' 105.7 . . ? C43' N1' H1' 105.7 . . ? N1' C39' C40' 114.2(3) . . ? N1' C39' H39C 108.7 . . ? C40' C39' H39C 108.7 . . ? N1' C39' H39D 108.7 . . ? C40' C39' H39D 108.7 . . ? H39C C39' H39D 107.6 . . ? C39' C40' H40D 109.5 . . ? C39' C40' H40E 109.5 . . ? H40D C40' H40E 109.5 . . ? C39' C40' H40F 109.5 . . ? H40D C40' H40F 109.5 . . ? H40E C40' H40F 109.5 . . ? N1' C41' C42' 111.6(3) . . ? N1' C41' H41C 109.3 . . ? C42' C41' H41C 109.3 . . ? N1' C41' H41D 109.3 . . ? C42' C41' H41D 109.3 . . ? H41C C41' H41D 108.0 . . ? C41' C42' H42D 109.5 . . ? C41' C42' H42E 109.5 . . ? H42D C42' H42E 109.5 . . ? C41' C42' H42F 109.5 . . ? H42D C42' H42F 109.5 . . ? H42E C42' H42F 109.5 . . ? C44' C43' N1' 114.7(3) . . ? C44' C43' H43C 108.6 . . ? N1' C43' H43C 108.6 . . ? C44' C43' H43D 108.6 . . ? N1' C43' H43D 108.6 . . ? H43C C43' H43D 107.6 . . ? C43' C44' H44D 109.5 . . ? C43' C44' H44E 109.5 . . ? H44D C44' H44E 109.5 . . ? C43' C44' H44F 109.5 . . ? H44D C44' H44F 109.5 . . ? H44E C44' H44F 109.5 . . ? O1D C1D H1D1 109.5 . . ? O1D C1D H1D2 109.5 . . ? H1D1 C1D H1D2 109.5 . . ? O1D C1D H1D3 109.5 . . ? H1D1 C1D H1D3 109.5 . . ? H1D2 C1D H1D3 109.5 . . ? C2D O1D C1D 112.6(3) . . ? O1D C2D C3D 109.7(3) . . ? O1D C2D H2D1 109.7 . . ? C3D C2D H2D1 109.7 . . ? O1D C2D H2D2 109.7 . . ? C3D C2D H2D2 109.7 . . ? H2D1 C2D H2D2 108.2 . . ? O2D C3D C2D 108.7(3) . . ? O2D C3D H3D1 109.9 . . ? C2D C3D H3D1 109.9 . . ? O2D C3D H3D2 109.9 . . ? C2D C3D H3D2 109.9 . . ? H3D1 C3D H3D2 108.3 . . ? C3D O2D C4D 113.2(4) . . ? O2D C4D H4D1 109.5 . . ? O2D C4D H4D2 109.5 . . ? H4D1 C4D H4D2 109.5 . . ? O2D C4D H4D3 109.5 . . ? H4D1 C4D H4D3 109.5 . . ? H4D2 C4D H4D3 109.5 . . ? O3D C5D H5D1 109.5 . . ? O3D C5D H5D2 109.5 . . ? H5D1 C5D H5D2 109.5 . . ? O3D C5D H5D3 109.5 . . ? H5D1 C5D H5D3 109.5 . . ? H5D2 C5D H5D3 109.5 . . ? C6D O3D C5D 121.6(6) . . ? O3D C6D C7D 120.3(6) . . ? O3D C6D H6D1 107.3 . . ? C7D C6D H6D1 107.3 . . ? O3D C6D H6D2 107.3 . . ? C7D C6D H6D2 107.3 . . ? H6D1 C6D H6D2 106.9 . . ? O4D C7D C6D 115.8(5) . . ? O4D C7D H7D1 108.3 . . ? C6D C7D H7D1 108.3 . . ? O4D C7D H7D2 108.3 . . ? C6D C7D H7D2 108.3 . . ? H7D1 C7D H7D2 107.4 . . ? C7D O4D C8D 114.9(6) . . ? O4D C8D H8D1 109.5 . . ? O4D C8D H8D2 109.5 . . ? H8D1 C8D H8D2 109.5 . . ? O4D C8D H8D3 109.5 . . ? H8D1 C8D H8D3 109.5 . . ? H8D2 C8D H8D3 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 B1 O1 C1 121.0(3) . . . . ? O3 B1 O1 C1 -119.1(3) . . . . ? O2 B1 O1 C1 0.6(3) . . . . ? O4 B1 O2 C2 -122.0(3) . . . . ? O1 B1 O2 C2 -0.6(3) . . . . ? O3 B1 O2 C2 120.8(3) . . . . ? B1 O1 C1 C6 -179.9(3) . . . . ? B1 O1 C1 C2 -0.4(3) . . . . ? B1 O2 C2 C3 -178.9(3) . . . . ? B1 O2 C2 C1 0.4(3) . . . . ? O1 C1 C2 O2 0.0(3) . . . . ? C6 C1 C2 O2 179.6(3) . . . . ? O1 C1 C2 C3 179.3(3) . . . . ? C6 C1 C2 C3 -1.1(4) . . . . ? O2 C2 C3 C4 179.6(3) . . . . ? C1 C2 C3 C4 0.4(4) . . . . ? C2 C3 C4 C5 0.3(4) . . . . ? C3 C4 C5 C6 -0.4(5) . . . . ? O1 C1 C6 C5 -179.5(3) . . . . ? C2 C1 C6 C5 1.0(4) . . . . ? O1 C1 C6 C7 1.0(4) . . . . ? C2 C1 C6 C7 -178.5(3) . . . . ? C4 C5 C6 C1 -0.3(4) . . . . ? C4 C5 C6 C7 179.3(3) . . . . ? C1 C6 C7 P1 102.0(3) . . . . ? C5 C6 C7 P1 -77.5(3) . . . . ? C6 C7 P1 C8 84.5(2) . . . . ? C6 C7 P1 C14 -173.8(2) . . . . ? C14 P1 C8 C9 106.7(3) . . . . ? C7 P1 C8 C9 -150.1(3) . . . . ? C14 P1 C8 C13 -68.5(3) . . . . ? C7 P1 C8 C13 34.6(3) . . . . ? C13 C8 C9 C10 0.6(6) . . . . ? P1 C8 C9 C10 -175.0(3) . . . . ? C8 C9 C10 C11 -0.2(7) . . . . ? C9 C10 C11 C12 -0.5(7) . . . . ? C10 C11 C12 C13 0.9(7) . . . . ? C11 C12 C13 C8 -0.6(7) . . . . ? C9 C8 C13 C12 -0.2(6) . . . . ? P1 C8 C13 C12 175.1(3) . . . . ? C8 P1 C14 C15 -101.2(3) . . . . ? C7 P1 C14 C15 153.7(3) . . . . ? C8 P1 C14 C19 75.4(3) . . . . ? C7 P1 C14 C19 -29.7(3) . . . . ? C19 C14 C15 C16 -1.1(5) . . . . ? P1 C14 C15 C16 175.7(3) . . . . ? C14 C15 C16 C17 0.0(5) . . . . ? C15 C16 C17 C18 0.8(6) . . . . ? C16 C17 C18 C19 -0.4(6) . . . . ? C17 C18 C19 C14 -0.7(6) . . . . ? C15 C14 C19 C18 1.4(5) . . . . ? P1 C14 C19 C18 -175.2(3) . . . . ? O4 B1 O3 C20 -2.1(3) . . . . ? O1 B1 O3 C20 -126.0(3) . . . . ? O2 B1 O3 C20 118.5(3) . . . . ? O1 B1 O4 C21 126.1(3) . . . . ? O3 B1 O4 C21 2.1(3) . . . . ? O2 B1 O4 C21 -118.1(3) . . . . ? B1 O3 C20 C25 -177.6(3) . . . . ? B1 O3 C20 C21 1.4(3) . . . . ? B1 O4 C21 C22 176.3(3) . . . . ? B1 O4 C21 C20 -1.3(3) . . . . ? O3 C20 C21 O4 -0.1(3) . . . . ? C25 C20 C21 O4 179.0(3) . . . . ? O3 C20 C21 C22 -177.9(3) . . . . ? C25 C20 C21 C22 1.2(5) . . . . ? O4 C21 C22 C23 -177.7(3) . . . . ? C20 C21 C22 C23 -0.3(5) . . . . ? C21 C22 C23 C24 -0.9(5) . . . . ? C22 C23 C24 C25 1.3(5) . . . . ? O3 C20 C25 C24 178.2(3) . . . . ? C21 C20 C25 C24 -0.7(4) . . . . ? O3 C20 C25 C26 -1.3(5) . . . . ? C21 C20 C25 C26 179.8(3) . . . . ? C23 C24 C25 C20 -0.5(5) . . . . ? C23 C24 C25 C26 179.0(3) . . . . ? C20 C25 C26 P2 107.5(3) . . . . ? C24 C25 C26 P2 -71.9(4) . . . . ? C25 C26 P2 C27 80.9(2) . . . . ? C25 C26 P2 C33 -172.8(2) . . . . ? C33 P2 C27 C32 114.9(3) . . . . ? C26 P2 C27 C32 -141.9(3) . . . . ? C33 P2 C27 C28 -65.2(3) . . . . ? C26 P2 C27 C28 38.0(3) . . . . ? C32 C27 C28 C29 -1.3(5) . . . . ? P2 C27 C28 C29 178.8(3) . . . . ? C27 C28 C29 C30 -0.2(5) . . . . ? C28 C29 C30 C31 1.1(6) . . . . ? C29 C30 C31 C32 -0.6(7) . . . . ? C28 C27 C32 C31 1.8(6) . . . . ? P2 C27 C32 C31 -178.3(3) . . . . ? C30 C31 C32 C27 -0.9(7) . . . . ? C27 P2 C33 C34 55.6(3) . . . . ? C26 P2 C33 C34 -50.5(3) . . . . ? C27 P2 C33 C38 -126.9(3) . . . . ? C26 P2 C33 C38 127.0(3) . . . . ? C38 C33 C34 C35 -0.2(5) . . . . ? P2 C33 C34 C35 177.2(3) . . . . ? C33 C34 C35 C36 1.2(5) . . . . ? C34 C35 C36 C37 -1.5(5) . . . . ? C35 C36 C37 C38 0.9(6) . . . . ? C36 C37 C38 C33 0.0(6) . . . . ? C34 C33 C38 C37 -0.4(5) . . . . ? P2 C33 C38 C37 -178.0(3) . . . . ? C41 N1 C39 C40 64.2(5) . . . . ? C43 N1 C39 C40 -65.2(5) . . . . ? C39 N1 C41 C42 59.1(6) . . . . ? C43 N1 C41 C42 -174.8(5) . . . . ? C39 N1 C43 C44 -143.7(8) . . . . ? C41 N1 C43 C44 89.3(9) . . . . ? O4' B1' O1' C1' -130.2(3) . . . . ? O3' B1' O1' C1' 112.0(3) . . . . ? O2' B1' O1' C1' -6.5(3) . . . . ? O4' B1' O2' C2' 128.5(3) . . . . ? O3' B1' O2' C2' -113.1(3) . . . . ? O1' B1' O2' C2' 7.1(3) . . . . ? B1' O1' C1' C6' -176.3(3) . . . . ? B1' O1' C1' C2' 3.6(3) . . . . ? B1' O2' C2' C3' 173.7(3) . . . . ? B1' O2' C2' C1' -5.3(3) . . . . ? O1' C1' C2' C3' -178.0(3) . . . . ? C6' C1' C2' C3' 1.9(5) . . . . ? O1' C1' C2' O2' 1.1(3) . . . . ? C6' C1' C2' O2' -179.0(3) . . . . ? O2' C2' C3' C4' -179.2(3) . . . . ? C1' C2' C3' C4' -0.3(5) . . . . ? C2' C3' C4' C5' -1.2(5) . . . . ? C3' C4' C5' C6' 1.2(5) . . . . ? O1' C1' C6' C5' 177.9(3) . . . . ? C2' C1' C6' C5' -1.9(4) . . . . ? O1' C1' C6' C7' -2.9(5) . . . . ? C2' C1' C6' C7' 177.3(3) . . . . ? C4' C5' C6' C1' 0.4(5) . . . . ? C4' C5' C6' C7' -178.7(3) . . . . ? C1' C6' C7' P1' -102.2(3) . . . . ? C5' C6' C7' P1' 76.9(3) . . . . ? C6' C7' P1' C14' -179.9(2) . . . . ? C6' C7' P1' C8' -77.6(2) . . . . ? C14' P1' C8' C13' -130.0(3) . . . . ? C7' P1' C8' C13' 125.9(3) . . . . ? C14' P1' C8' C9' 54.1(3) . . . . ? C7' P1' C8' C9' -50.0(3) . . . . ? C13' C8' C9' C10' -0.8(5) . . . . ? P1' C8' C9' C10' 175.1(3) . . . . ? C8' C9' C10' C11' -0.7(5) . . . . ? C9' C10' C11' C12' 1.3(6) . . . . ? C10' C11' C12' C13' -0.3(6) . . . . ? C9' C8' C13' C12' 1.7(5) . . . . ? P1' C8' C13' C12' -174.3(3) . . . . ? C11' C12' C13' C8' -1.2(6) . . . . ? C8' P1' C14' C19' 88.7(3) . . . . ? C7' P1' C14' C19' -169.2(3) . . . . ? C8' P1' C14' C15' -88.5(3) . . . . ? C7' P1' C14' C15' 13.6(3) . . . . ? C19' C14' C15' C16' -0.2(5) . . . . ? P1' C14' C15' C16' 177.0(3) . . . . ? C14' C15' C16' C17' -1.2(6) . . . . ? C15' C16' C17' C18' 1.6(6) . . . . ? C16' C17' C18' C19' -0.6(7) . . . . ? C17' C18' C19' C14' -0.8(8) . . . . ? C15' C14' C19' C18' 1.2(6) . . . . ? P1' C14' C19' C18' -176.2(4) . . . . ? O4' B1' O3' C20' -7.9(3) . . . . ? O1' B1' O3' C20' 113.1(3) . . . . ? O2' B1' O3' C20' -131.9(2) . . . . ? O3' B1' O4' C21' 8.7(3) . . . . ? O1' B1' O4' C21' -113.1(3) . . . . ? O2' B1' O4' C21' 129.5(2) . . . . ? B1' O3' C20' C25' -176.0(3) . . . . ? B1' O3' C20' C21' 4.3(3) . . . . ? B1' O4' C21' C22' 171.7(3) . . . . ? B1' O4' C21' C20' -6.4(3) . . . . ? O3' C20' C21' O4' 1.3(3) . . . . ? C25' C20' C21' O4' -178.4(2) . . . . ? O3' C20' C21' C22' -177.0(3) . . . . ? C25' C20' C21' C22' 3.3(4) . . . . ? O4' C21' C22' C23' 179.6(3) . . . . ? C20' C21' C22' C23' -2.5(4) . . . . ? C21' C22' C23' C24' 0.2(5) . . . . ? C22' C23' C24' C25' 1.4(5) . . . . ? O3' C20' C25' C24' 178.7(3) . . . . ? C21' C20' C25' C24' -1.7(4) . . . . ? O3' C20' C25' C26' 1.3(4) . . . . ? C21' C20' C25' C26' -179.0(3) . . . . ? C23' C24' C25' C20' -0.6(4) . . . . ? C23' C24' C25' C26' 176.7(3) . . . . ? C20' C25' C26' P2' -108.4(3) . . . . ? C24' C25' C26' P2' 74.5(3) . . . . ? C25' C26' P2' C27' -76.1(3) . . . . ? C25' C26' P2' C33' -178.3(2) . . . . ? C33' P2' C27' C32' -128.3(3) . . . . ? C26' P2' C27' C32' 128.2(3) . . . . ? C33' P2' C27' C28' 49.7(3) . . . . ? C26' P2' C27' C28' -53.8(3) . . . . ? C32' C27' C28' C29' 0.1(5) . . . . ? P2' C27' C28' C29' -177.9(3) . . . . ? C27' C28' C29' C30' 0.9(5) . . . . ? C28' C29' C30' C31' -1.2(6) . . . . ? C29' C30' C31' C32' 0.5(6) . . . . ? C28' C27' C32' C31' -0.7(5) . . . . ? P2' C27' C32' C31' 177.4(3) . . . . ? C30' C31' C32' C27' 0.4(6) . . . . ? C27' P2' C33' C38' -128.3(4) . . . . ? C26' P2' C33' C38' -23.8(4) . . . . ? C27' P2' C33' C34' 53.9(3) . . . . ? C26' P2' C33' C34' 158.4(3) . . . . ? C38' C33' C34' C35' 0.9(6) . . . . ? P2' C33' C34' C35' 178.8(3) . . . . ? C33' C34' C35' C36' 0.3(7) . . . . ? C34' C35' C36' C37' -0.6(8) . . . . ? C35' C36' C37' C38' -0.3(9) . . . . ? C34' C33' C38' C37' -1.8(7) . . . . ? P2' C33' C38' C37' -179.5(4) . . . . ? C36' C37' C38' C33' 1.5(8) . . . . ? C41' N1' C39' C40' -59.1(4) . . . . ? C43' N1' C39' C40' 70.1(4) . . . . ? C39' N1' C41' C42' -58.9(4) . . . . ? C43' N1' C41' C42' 173.2(3) . . . . ? C41' N1' C43' C44' -61.8(5) . . . . ? C39' N1' C43' C44' 166.7(4) . . . . ? C1D O1D C2D C3D -169.7(4) . . . . ? O1D C2D C3D O2D 64.2(4) . . . . ? C2D C3D O2D C4D 173.1(4) . . . . ? C5D O3D C6D C7D 162.0(10) . . . . ? O3D C6D C7D O4D 14.2(16) . . . . ? C6D C7D O4D C8D 168.6(10) . . . . ? 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 O2 0.93 1.83 2.757(4) 176.9 . N1' H1' O2' 0.93 1.87 2.802(3) 174.1 . C43' H43C O4 0.99 2.33 3.266(5) 157.6 1_545 C43 H43B O4' 0.99 2.28 3.177(6) 149.5 . _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.813 _refine_diff_density_min -1.281 _refine_diff_density_rms 0.085 #============================================================================== #_eof # End of Crystallographic Information File # Attachment '648430mod.cif' data_c:\crystal\x-red\scjan07 _database_code_depnum_ccdc_archive 'CCDC 648430' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H37 Ag B N O5 P2' _chemical_formula_weight 804.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ag Ag -0.8971 1.1015 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' N N 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 18.8664(8) _cell_length_b 15.1936(5) _cell_length_c 15.0136(5) _cell_angle_alpha 90.00 _cell_angle_beta 124.062(2) _cell_angle_gamma 90.00 _cell_volume 3565.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.8mm _exptl_crystal_size_mid 0.5mm _exptl_crystal_size_min 0.5mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.703 _exptl_absorpt_correction_type ;numerically with the help of the X-SHAPE soft ware by STOE, based on the program HABITUS by W. Herrendorf, Univ. Giessen, 1995 ; _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa CCD (Nonius)' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20576 _diffrn_reflns_av_R_equivalents 0.0989 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 5.54 _diffrn_reflns_theta_max 28.29 _reflns_number_total 8102 _reflns_number_gt 6931 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+11.5874P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.64(3) _refine_ls_number_reflns 8102 _refine_ls_number_parameters 458 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1292 _refine_ls_wR_factor_gt 0.1217 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Ag Ag 0.47286(2) 0.30748(2) 0.15037(2) 0.01932(10) Uani 1 1 d . . . P1 P 0.44075(10) 0.25573(10) -0.02290(12) 0.0181(3) Uani 1 1 d . . . P2 P 0.49662(8) 0.28904(9) 0.32736(11) 0.0133(3) Uani 1 1 d . . . C1 C 0.3406(4) 0.5388(4) -0.0533(5) 0.0212(11) Uani 1 1 d . . . C2 C 0.3952(4) 0.4705(4) -0.0443(5) 0.0200(11) Uani 1 1 d . . . C3 C 0.3734(4) 0.4153(4) -0.1291(5) 0.0206(11) Uani 1 1 d . . . C4 C 0.2952(4) 0.4324(4) -0.2264(5) 0.0294(14) Uani 1 1 d . . . H4A H 0.2781 0.3969 -0.2857 0.035 Uiso 1 1 calc R . . C5 C 0.2428(4) 0.5014(5) -0.2360(5) 0.0321(14) Uani 1 1 d . . . H5A H 0.1914 0.5114 -0.3017 0.039 Uiso 1 1 calc R . . C6 C 0.2659(4) 0.5555(4) -0.1491(5) 0.0290(13) Uani 1 1 d . . . H6A H 0.2310 0.6020 -0.1563 0.035 Uiso 1 1 calc R . . C7 C 0.4329(4) 0.3427(4) -0.1138(4) 0.0176(10) Uani 1 1 d . . . H7B H 0.4894 0.3671 -0.0846 0.021 Uiso 1 1 calc R . . H7A H 0.4131 0.3169 -0.1831 0.021 Uiso 1 1 calc R . . C8 C 0.3386(4) 0.1996(4) -0.0964(5) 0.0211(11) Uani 1 1 d . . . C9 C 0.2882(4) 0.1920(4) -0.2072(5) 0.0316(14) Uani 1 1 d . . . H9A H 0.3060 0.2179 -0.2475 0.038 Uiso 1 1 calc R . . C10 C 0.2112(5) 0.1461(5) -0.2591(7) 0.0384(19) Uani 1 1 d . . . H10A H 0.1782 0.1414 -0.3336 0.046 Uiso 1 1 calc R . . C11 C 0.1837(4) 0.1075(4) -0.2004(7) 0.0373(17) Uani 1 1 d . . . H11A H 0.1325 0.0764 -0.2356 0.045 Uiso 1 1 calc R . . C12 C 0.2312(5) 0.1147(5) -0.0912(7) 0.0370(17) Uani 1 1 d . . . H12A H 0.2124 0.0890 -0.0517 0.044 Uiso 1 1 calc R . . C13 C 0.3097(4) 0.1617(4) -0.0383(6) 0.0295(14) Uani 1 1 d . . . H13A H 0.3421 0.1671 0.0362 0.035 Uiso 1 1 calc R . . C14 C 0.5147(4) 0.1773(4) -0.0236(5) 0.0190(12) Uani 1 1 d . . . C15 C 0.4958(4) 0.0892(4) -0.0465(5) 0.0294(13) Uani 1 1 d . . . H15A H 0.4440 0.0671 -0.0623 0.035 Uiso 1 1 calc R . . C16 C 0.5548(5) 0.0334(5) -0.0457(6) 0.0355(15) Uani 1 1 d . . . H16A H 0.5423 -0.0261 -0.0607 0.043 Uiso 1 1 calc R . . C17 C 0.6319(5) 0.0661(5) -0.0226(6) 0.0306(16) Uani 1 1 d . . . H17A H 0.6710 0.0285 -0.0223 0.037 Uiso 1 1 calc R . . C18 C 0.6509(4) 0.1541(5) -0.0001(5) 0.0306(14) Uani 1 1 d . . . H18A H 0.7027 0.1758 0.0151 0.037 Uiso 1 1 calc R . . C19 C 0.5933(4) 0.2102(4) 0.0000(5) 0.0247(12) Uani 1 1 d . . . H19A H 0.6064 0.2696 0.0157 0.030 Uiso 1 1 calc R . . C20 C 0.5157(4) 0.5031(4) 0.2990(5) 0.0192(11) Uani 1 1 d . . . C21 C 0.5623(4) 0.5702(4) 0.2907(6) 0.0242(13) Uani 1 1 d . . . C22 C 0.6342(4) 0.6037(4) 0.3830(6) 0.0285(13) Uani 1 1 d . . . H22A H 0.6655 0.6494 0.3797 0.034 Uiso 1 1 calc R . . C23 C 0.6583(4) 0.5665(4) 0.4817(5) 0.0277(13) Uani 1 1 d . . . H23A H 0.7065 0.5881 0.5447 0.033 Uiso 1 1 calc R . . C24 C 0.6124(3) 0.4985(4) 0.4877(5) 0.0228(12) Uani 1 1 d . . . H24A H 0.6296 0.4759 0.5546 0.027 Uiso 1 1 calc R . . C25 C 0.5398(3) 0.4629(4) 0.3940(5) 0.0183(11) Uani 1 1 d . . . C26 C 0.4887(3) 0.3871(4) 0.3927(4) 0.0162(10) Uani 1 1 d . . . H26B H 0.4291 0.4045 0.3552 0.019 Uiso 1 1 calc R . . H26A H 0.5085 0.3724 0.4661 0.019 Uiso 1 1 calc R . . C27 C 0.5999(3) 0.2385(4) 0.4230(4) 0.0161(10) Uani 1 1 d . . . C28 C 0.6407(4) 0.2443(4) 0.5345(5) 0.0249(12) Uani 1 1 d . . . H28A H 0.6168 0.2784 0.5627 0.030 Uiso 1 1 calc R . . C29 C 0.7165(4) 0.1993(4) 0.6033(5) 0.0293(13) Uani 1 1 d . . . H29A H 0.7431 0.2027 0.6773 0.035 Uiso 1 1 calc R . . C30 C 0.7524(4) 0.1491(4) 0.5607(6) 0.0263(14) Uani 1 1 d . . . H30A H 0.8031 0.1187 0.6067 0.032 Uiso 1 1 calc R . . C31 C 0.7140(4) 0.1439(4) 0.4517(5) 0.0267(13) Uani 1 1 d . . . H31A H 0.7388 0.1106 0.4240 0.032 Uiso 1 1 calc R . . C32 C 0.6376(4) 0.1889(4) 0.3826(5) 0.0193(11) Uani 1 1 d . . . H32A H 0.6117 0.1855 0.3087 0.023 Uiso 1 1 calc R . . C33 C 0.4201(4) 0.2126(4) 0.3250(5) 0.0158(11) Uani 1 1 d . . . C34 C 0.3840(4) 0.2284(4) 0.3834(5) 0.0235(12) Uani 1 1 d . . . H34A H 0.4001 0.2778 0.4272 0.028 Uiso 1 1 calc R . . C35 C 0.3240(4) 0.1703(5) 0.3757(5) 0.0311(14) Uani 1 1 d . . . H35A H 0.2996 0.1810 0.4140 0.037 Uiso 1 1 calc R . . C36 C 0.3006(5) 0.0966(5) 0.3112(6) 0.0312(16) Uani 1 1 d . . . H36A H 0.2598 0.0582 0.3053 0.037 Uiso 1 1 calc R . . C37 C 0.3377(4) 0.0793(4) 0.2547(5) 0.0271(12) Uani 1 1 d . . . H37A H 0.3224 0.0290 0.2124 0.033 Uiso 1 1 calc R . . C38 C 0.3971(4) 0.1371(4) 0.2616(5) 0.0221(11) Uani 1 1 d . . . H38A H 0.4218 0.1257 0.2239 0.027 Uiso 1 1 calc R . . C39 C 0.4012(4) 0.2149(5) -0.3647(6) 0.0275(14) Uani 1 1 d . . . H39A H 0.4197 0.2731 -0.3540 0.033 Uiso 1 1 calc R . . C40 C 0.5423(5) 0.1751(6) -0.3162(8) 0.049(2) Uani 1 1 d . . . H40C H 0.5580 0.1396 -0.3554 0.059 Uiso 1 1 calc R . . H40B H 0.5813 0.1643 -0.2406 0.059 Uiso 1 1 calc R . . H40A H 0.5446 0.2362 -0.3308 0.059 Uiso 1 1 calc R . . C41 C 0.4322(6) 0.0602(5) -0.3676(8) 0.052(2) Uani 1 1 d . . . H41C H 0.4428 0.0365 -0.4184 0.062 Uiso 1 1 calc R . . H41B H 0.3726 0.0543 -0.3955 0.062 Uiso 1 1 calc R . . H41A H 0.4656 0.0285 -0.3010 0.062 Uiso 1 1 calc R . . B B 0.4543(4) 0.5331(4) 0.1211(5) 0.0226(14) Uani 1 1 d . . . O1 O 0.3760(3) 0.5812(3) 0.0416(4) 0.0248(9) Uani 1 1 d . . . O2 O 0.4680(3) 0.4688(3) 0.0561(3) 0.0194(8) Uani 1 1 d . . . O3 O 0.4460(3) 0.4806(3) 0.1989(3) 0.0189(8) Uani 1 1 d . . . O4 O 0.5278(3) 0.5923(3) 0.1867(4) 0.0278(9) Uani 1 1 d . . . O5 O 0.3266(3) 0.2007(4) -0.3928(4) 0.0398(11) Uani 1 1 d . . . N N 0.4561(3) 0.1529(4) -0.3491(5) 0.0293(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.02573(19) 0.01773(17) 0.02036(16) -0.0005(2) 0.01650(14) 0.0001(2) P1 0.0247(7) 0.0158(7) 0.0202(7) -0.0015(6) 0.0164(6) -0.0034(6) P2 0.0123(6) 0.0147(6) 0.0149(6) -0.0013(5) 0.0088(5) 0.0006(5) C1 0.025(3) 0.016(3) 0.030(3) 0.006(2) 0.020(3) 0.004(2) C2 0.024(3) 0.017(3) 0.030(3) 0.006(2) 0.022(3) -0.002(2) C3 0.020(3) 0.020(3) 0.026(3) 0.005(2) 0.016(2) -0.004(2) C4 0.034(3) 0.032(3) 0.023(3) 0.004(3) 0.016(3) -0.006(3) C5 0.025(3) 0.033(3) 0.033(3) 0.009(3) 0.013(3) 0.003(3) C6 0.027(3) 0.027(3) 0.038(3) 0.016(3) 0.022(3) 0.012(3) C7 0.022(3) 0.014(2) 0.021(3) -0.002(2) 0.014(2) -0.003(2) C8 0.030(3) 0.015(3) 0.034(3) -0.001(2) 0.028(3) 0.001(2) C9 0.034(3) 0.029(3) 0.038(3) -0.011(3) 0.024(3) -0.016(3) C10 0.031(4) 0.034(4) 0.042(4) -0.012(3) 0.015(3) -0.012(3) C11 0.025(3) 0.017(3) 0.072(5) -0.003(3) 0.029(3) -0.005(2) C12 0.041(4) 0.024(3) 0.072(5) 0.003(3) 0.047(4) -0.001(3) C13 0.042(4) 0.020(3) 0.042(4) 0.003(3) 0.033(3) 0.001(3) C14 0.025(3) 0.018(3) 0.020(3) -0.002(2) 0.017(2) -0.006(2) C15 0.027(3) 0.022(3) 0.037(3) -0.007(3) 0.017(3) -0.005(2) C16 0.038(4) 0.022(3) 0.040(4) -0.004(3) 0.018(3) 0.000(3) C17 0.031(4) 0.031(4) 0.031(3) 0.001(3) 0.018(3) 0.012(3) C18 0.026(3) 0.029(3) 0.038(4) 0.004(3) 0.019(3) 0.001(3) C19 0.021(3) 0.019(3) 0.033(3) 0.001(2) 0.015(2) -0.003(2) C20 0.014(3) 0.018(3) 0.027(3) -0.007(2) 0.011(2) -0.004(2) C21 0.024(3) 0.019(3) 0.042(4) -0.009(3) 0.027(3) -0.003(2) C22 0.020(3) 0.023(3) 0.049(4) -0.009(3) 0.024(3) -0.004(2) C23 0.014(3) 0.024(3) 0.038(3) -0.010(3) 0.011(3) -0.001(2) C24 0.017(3) 0.022(3) 0.027(3) -0.007(2) 0.011(2) 0.004(2) C25 0.008(2) 0.019(3) 0.027(3) -0.010(2) 0.009(2) 0.0004(19) C26 0.016(2) 0.019(3) 0.015(2) -0.001(2) 0.010(2) 0.003(2) C27 0.009(2) 0.016(3) 0.022(3) 0.000(2) 0.008(2) -0.0016(19) C28 0.018(3) 0.029(3) 0.028(3) 0.000(2) 0.013(2) 0.002(2) C29 0.020(3) 0.035(3) 0.023(3) 0.003(3) 0.006(2) -0.003(3) C30 0.021(3) 0.020(3) 0.041(4) 0.009(3) 0.019(3) 0.004(2) C31 0.014(3) 0.021(3) 0.044(4) 0.000(3) 0.016(3) 0.004(2) C32 0.017(3) 0.019(3) 0.023(3) -0.005(2) 0.012(2) -0.003(2) C33 0.012(2) 0.015(3) 0.014(2) 0.001(2) 0.004(2) 0.003(2) C34 0.018(3) 0.032(3) 0.021(3) -0.004(2) 0.011(2) -0.007(2) C35 0.023(3) 0.047(4) 0.030(3) -0.008(3) 0.019(3) -0.014(3) C36 0.028(3) 0.036(4) 0.031(3) 0.004(3) 0.017(3) -0.012(3) C37 0.028(3) 0.023(3) 0.030(3) -0.003(2) 0.017(3) -0.007(2) C38 0.023(3) 0.020(3) 0.024(3) 0.000(2) 0.014(2) -0.002(2) C39 0.028(3) 0.029(3) 0.029(3) -0.003(3) 0.018(3) -0.007(3) C40 0.029(4) 0.051(5) 0.064(6) 0.012(4) 0.024(4) 0.008(4) C41 0.067(5) 0.031(4) 0.076(6) 0.007(4) 0.052(5) 0.001(4) B 0.030(4) 0.017(3) 0.028(4) 0.000(2) 0.021(3) 0.000(2) O1 0.030(2) 0.020(2) 0.033(2) 0.0049(18) 0.024(2) 0.0052(17) O2 0.020(2) 0.0171(19) 0.025(2) -0.0003(16) 0.0144(18) 0.0019(16) O3 0.019(2) 0.019(2) 0.0180(19) -0.0050(16) 0.0101(17) -0.0066(16) O4 0.037(2) 0.016(2) 0.045(3) -0.0099(19) 0.032(2) -0.0109(18) O5 0.036(3) 0.050(3) 0.044(3) -0.006(2) 0.029(2) -0.010(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 Ag P1 2.4468(16) . ? Ag P2 2.4508(14) . ? P1 C8 1.811(6) . ? P1 C14 1.840(6) . ? P1 C7 1.844(6) . ? P2 C27 1.821(5) . ? P2 C26 1.835(6) . ? P2 C33 1.837(6) . ? C1 O1 1.351(8) . ? C1 C6 1.360(9) . ? C1 C2 1.414(8) . ? C2 O2 1.356(7) . ? C2 C3 1.381(9) . ? C3 C4 1.401(8) . ? C3 C7 1.498(8) . ? C4 C5 1.393(10) . ? C5 C6 1.390(10) . ? C8 C9 1.383(9) . ? C8 C13 1.386(9) . ? C9 C10 1.390(9) . ? C10 C11 1.378(12) . ? C11 C12 1.363(11) . ? C12 C13 1.420(10) . ? C14 C15 1.379(8) . ? C14 C19 1.408(8) . ? C15 C16 1.394(10) . ? C16 C17 1.385(10) . ? C17 C18 1.376(10) . ? C18 C19 1.383(9) . ? C20 C25 1.374(9) . ? C20 O3 1.376(6) . ? C20 C21 1.397(8) . ? C21 O4 1.355(8) . ? C21 C22 1.384(9) . ? C22 C23 1.403(10) . ? C23 C24 1.384(9) . ? C24 C25 1.410(7) . ? C25 C26 1.495(8) . ? C27 C32 1.388(8) . ? C27 C28 1.400(8) . ? C28 C29 1.387(8) . ? C29 C30 1.391(10) . ? C30 C31 1.372(10) . ? C31 C32 1.395(8) . ? C33 C38 1.394(8) . ? C33 C34 1.401(8) . ? C34 C35 1.388(8) . ? C35 C36 1.382(10) . ? C36 C37 1.394(10) . ? C37 C38 1.381(8) . ? C39 O5 1.241(8) . ? C39 N 1.319(9) . ? C40 N 1.451(10) . ? C41 N 1.458(9) . ? B O1 1.471(8) . ? B O4 1.474(8) . ? B O3 1.493(8) . ? B O2 1.503(8) . ? 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 P1 Ag P2 154.43(6) . . ? C8 P1 C14 104.1(3) . . ? C8 P1 C7 105.7(3) . . ? C14 P1 C7 101.9(3) . . ? C8 P1 Ag 110.1(2) . . ? C14 P1 Ag 118.5(2) . . ? C7 P1 Ag 115.20(18) . . ? C27 P2 C26 107.0(3) . . ? C27 P2 C33 103.3(2) . . ? C26 P2 C33 103.0(3) . . ? C27 P2 Ag 111.60(19) . . ? C26 P2 Ag 117.83(18) . . ? C33 P2 Ag 112.73(19) . . ? O1 C1 C6 129.3(6) . . ? O1 C1 C2 110.2(5) . . ? C6 C1 C2 120.4(6) . . ? O2 C2 C3 127.3(5) . . ? O2 C2 C1 110.5(5) . . ? C3 C2 C1 122.2(6) . . ? C2 C3 C4 116.4(6) . . ? C2 C3 C7 119.7(5) . . ? C4 C3 C7 123.9(6) . . ? C5 C4 C3 121.3(6) . . ? C6 C5 C4 121.1(6) . . ? C1 C6 C5 118.5(6) . . ? C3 C7 P1 112.5(4) . . ? C9 C8 C13 118.3(6) . . ? C9 C8 P1 123.5(5) . . ? C13 C8 P1 118.1(5) . . ? C8 C9 C10 121.0(7) . . ? C11 C10 C9 120.2(8) . . ? C12 C11 C10 120.4(6) . . ? C11 C12 C13 119.3(6) . . ? C8 C13 C12 120.7(7) . . ? C15 C14 C19 119.8(6) . . ? C15 C14 P1 122.6(5) . . ? C19 C14 P1 117.6(5) . . ? C14 C15 C16 119.6(6) . . ? C17 C16 C15 120.4(6) . . ? C18 C17 C16 120.2(7) . . ? C17 C18 C19 120.2(6) . . ? C18 C19 C14 119.9(6) . . ? C25 C20 O3 125.6(5) . . ? C25 C20 C21 124.0(5) . . ? O3 C20 C21 110.3(5) . . ? O4 C21 C22 129.1(6) . . ? O4 C21 C20 111.4(5) . . ? C22 C21 C20 119.5(6) . . ? C21 C22 C23 117.7(6) . . ? C24 C23 C22 121.8(5) . . ? C23 C24 C25 121.0(6) . . ? C20 C25 C24 115.9(5) . . ? C20 C25 C26 119.6(5) . . ? C24 C25 C26 124.5(6) . . ? C25 C26 P2 112.8(4) . . ? C32 C27 C28 118.9(5) . . ? C32 C27 P2 118.0(4) . . ? C28 C27 P2 123.0(4) . . ? C29 C28 C27 120.4(6) . . ? C28 C29 C30 119.6(6) . . ? C31 C30 C29 120.8(6) . . ? C30 C31 C32 119.6(6) . . ? C27 C32 C31 120.7(6) . . ? C38 C33 C34 119.5(6) . . ? C38 C33 P2 118.4(5) . . ? C34 C33 P2 122.1(4) . . ? C35 C34 C33 120.0(6) . . ? C36 C35 C34 119.9(6) . . ? C35 C36 C37 120.5(6) . . ? C38 C37 C36 119.8(6) . . ? C37 C38 C33 120.3(6) . . ? O5 C39 N 124.3(7) . . ? O1 B O4 112.4(5) . . ? O1 B O3 113.7(5) . . ? O4 B O3 106.0(5) . . ? O1 B O2 104.8(4) . . ? O4 B O2 113.0(5) . . ? O3 B O2 107.0(5) . . ? C1 O1 B 107.3(4) . . ? C2 O2 B 105.9(4) . . ? C20 O3 B 105.5(4) . . ? C21 O4 B 106.4(5) . . ? C39 N C40 120.8(6) . . ? C39 N C41 121.9(6) . . ? C40 N C41 117.2(6) . . ? 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 P2 Ag P1 C8 57.5(3) . . . . ? P2 Ag P1 C14 -62.2(3) . . . . ? P2 Ag P1 C7 176.8(2) . . . . ? P1 Ag P2 C27 74.0(2) . . . . ? P1 Ag P2 C26 -161.7(2) . . . . ? P1 Ag P2 C33 -41.8(2) . . . . ? O1 C1 C2 O2 -1.5(6) . . . . ? C6 C1 C2 O2 176.5(5) . . . . ? O1 C1 C2 C3 178.3(5) . . . . ? C6 C1 C2 C3 -3.7(9) . . . . ? O2 C2 C3 C4 -178.0(5) . . . . ? C1 C2 C3 C4 2.2(8) . . . . ? O2 C2 C3 C7 1.3(9) . . . . ? C1 C2 C3 C7 -178.4(5) . . . . ? C2 C3 C4 C5 -0.2(9) . . . . ? C7 C3 C4 C5 -179.5(6) . . . . ? C3 C4 C5 C6 -0.4(10) . . . . ? O1 C1 C6 C5 -179.5(6) . . . . ? C2 C1 C6 C5 3.0(9) . . . . ? C4 C5 C6 C1 -1.0(10) . . . . ? C2 C3 C7 P1 68.4(6) . . . . ? C4 C3 C7 P1 -112.3(5) . . . . ? C8 P1 C7 C3 70.2(4) . . . . ? C14 P1 C7 C3 178.7(4) . . . . ? Ag P1 C7 C3 -51.6(4) . . . . ? C14 P1 C8 C9 -76.9(6) . . . . ? C7 P1 C8 C9 30.1(6) . . . . ? Ag P1 C8 C9 155.1(5) . . . . ? C14 P1 C8 C13 102.6(5) . . . . ? C7 P1 C8 C13 -150.5(5) . . . . ? Ag P1 C8 C13 -25.5(5) . . . . ? C13 C8 C9 C10 -1.1(10) . . . . ? P1 C8 C9 C10 178.3(6) . . . . ? C8 C9 C10 C11 0.2(11) . . . . ? C9 C10 C11 C12 0.7(11) . . . . ? C10 C11 C12 C13 -0.5(10) . . . . ? C9 C8 C13 C12 1.3(9) . . . . ? P1 C8 C13 C12 -178.2(5) . . . . ? C11 C12 C13 C8 -0.5(10) . . . . ? C8 P1 C14 C15 -17.5(6) . . . . ? C7 P1 C14 C15 -127.2(5) . . . . ? Ag P1 C14 C15 105.3(5) . . . . ? C8 P1 C14 C19 162.4(5) . . . . ? C7 P1 C14 C19 52.6(5) . . . . ? Ag P1 C14 C19 -74.9(5) . . . . ? C19 C14 C15 C16 0.1(10) . . . . ? P1 C14 C15 C16 180.0(5) . . . . ? C14 C15 C16 C17 -0.3(10) . . . . ? C15 C16 C17 C18 0.1(11) . . . . ? C16 C17 C18 C19 0.3(11) . . . . ? C17 C18 C19 C14 -0.4(10) . . . . ? C15 C14 C19 C18 0.2(9) . . . . ? P1 C14 C19 C18 -179.6(5) . . . . ? C25 C20 C21 O4 174.7(5) . . . . ? O3 C20 C21 O4 -2.0(7) . . . . ? C25 C20 C21 C22 -4.7(9) . . . . ? O3 C20 C21 C22 178.7(5) . . . . ? O4 C21 C22 C23 -177.5(6) . . . . ? C20 C21 C22 C23 1.7(8) . . . . ? C21 C22 C23 C24 0.0(9) . . . . ? C22 C23 C24 C25 1.0(9) . . . . ? O3 C20 C25 C24 -178.4(5) . . . . ? C21 C20 C25 C24 5.4(8) . . . . ? O3 C20 C25 C26 0.8(8) . . . . ? C21 C20 C25 C26 -175.3(5) . . . . ? C23 C24 C25 C20 -3.5(8) . . . . ? C23 C24 C25 C26 177.3(5) . . . . ? C20 C25 C26 P2 67.6(6) . . . . ? C24 C25 C26 P2 -113.3(5) . . . . ? C27 P2 C26 C25 77.1(4) . . . . ? C33 P2 C26 C25 -174.3(4) . . . . ? Ag P2 C26 C25 -49.5(4) . . . . ? C26 P2 C27 C32 -153.1(4) . . . . ? C33 P2 C27 C32 98.6(5) . . . . ? Ag P2 C27 C32 -22.8(5) . . . . ? C26 P2 C27 C28 29.9(5) . . . . ? C33 P2 C27 C28 -78.4(5) . . . . ? Ag P2 C27 C28 160.2(4) . . . . ? C32 C27 C28 C29 -1.5(9) . . . . ? P2 C27 C28 C29 175.5(5) . . . . ? C27 C28 C29 C30 0.7(9) . . . . ? C28 C29 C30 C31 0.4(10) . . . . ? C29 C30 C31 C32 -0.6(10) . . . . ? C28 C27 C32 C31 1.2(8) . . . . ? P2 C27 C32 C31 -175.9(4) . . . . ? C30 C31 C32 C27 -0.2(9) . . . . ? C27 P2 C33 C38 -81.2(5) . . . . ? C26 P2 C33 C38 167.5(4) . . . . ? Ag P2 C33 C38 39.5(5) . . . . ? C27 P2 C33 C34 99.6(5) . . . . ? C26 P2 C33 C34 -11.7(5) . . . . ? Ag P2 C33 C34 -139.7(4) . . . . ? C38 C33 C34 C35 -1.6(9) . . . . ? P2 C33 C34 C35 177.5(5) . . . . ? C33 C34 C35 C36 0.5(10) . . . . ? C34 C35 C36 C37 0.9(11) . . . . ? C35 C36 C37 C38 -1.2(10) . . . . ? C36 C37 C38 C33 0.0(9) . . . . ? C34 C33 C38 C37 1.4(8) . . . . ? P2 C33 C38 C37 -177.8(5) . . . . ? C6 C1 O1 B 176.4(6) . . . . ? C2 C1 O1 B -5.9(6) . . . . ? O4 B O1 C1 133.3(5) . . . . ? O3 B O1 C1 -106.2(5) . . . . ? O2 B O1 C1 10.3(6) . . . . ? C3 C2 O2 B -171.8(6) . . . . ? C1 C2 O2 B 8.0(6) . . . . ? O1 B O2 C2 -11.0(6) . . . . ? O4 B O2 C2 -133.7(5) . . . . ? O3 B O2 C2 110.0(5) . . . . ? C25 C20 O3 B -171.6(6) . . . . ? C21 C20 O3 B 5.0(6) . . . . ? O1 B O3 C20 -129.9(5) . . . . ? O4 B O3 C20 -6.0(6) . . . . ? O2 B O3 C20 114.8(5) . . . . ? C22 C21 O4 B 177.2(6) . . . . ? C20 C21 O4 B -2.0(6) . . . . ? O1 B O4 C21 129.7(5) . . . . ? O3 B O4 C21 4.9(6) . . . . ? O2 B O4 C21 -111.9(5) . . . . ? O5 C39 N C40 -180.0(7) . . . . ? O5 C39 N C41 2.3(11) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.772 _refine_diff_density_min -1.063 _refine_diff_density_rms 0.104 # Attachment '648431mod.cif' data_c:\crystal\x-red\scnov05 _database_code_depnum_ccdc_archive 'CCDC 648431' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H46 B N O4 P2' _chemical_formula_weight 725.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.1023 0.0942 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 8.1733(2) _cell_length_b 43.2770(10) _cell_length_c 11.0401(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.894(2) _cell_angle_gamma 90.00 _cell_volume 3890.82(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.155 _exptl_absorpt_correction_type ;numerically with the help of the X-SHAPE soft ware by STOE, based on the program HABITUS by W. Herrendorf, Univ. Giessen, 1995 ; _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa CCD (Nonius)' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32901 _diffrn_reflns_av_R_equivalents 0.0896 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -57 _diffrn_reflns_limit_k_max 57 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 28.27 _reflns_number_total 9084 _reflns_number_gt 7638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+7.4395P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(8) _refine_ls_number_reflns 9084 _refine_ls_number_parameters 476 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 P1 P 0.16578(9) 0.067706(16) 0.86026(6) 0.01552(15) Uani 1 1 d . . . P2 P 0.14025(9) 0.374558(17) 0.83405(7) 0.01751(16) Uani 1 1 d . . . O1 O 0.2026(2) 0.19397(4) 0.77248(18) 0.0164(4) Uani 1 1 d . . . O2 O 0.2033(2) 0.24976(4) 0.81806(17) 0.0149(4) Uani 1 1 d . . . O3 O -0.0084(2) 0.21472(4) 0.88205(18) 0.0165(4) Uani 1 1 d . . . C1 C -0.0710(3) 0.37301(7) 0.8795(3) 0.0184(6) Uani 1 1 d . . . C2 C -0.0583(4) 0.06959(7) 0.8268(3) 0.0180(6) Uani 1 1 d . . . C3 C 0.1527(4) 0.17316(6) 0.8553(2) 0.0131(5) Uani 1 1 d . . . C4 C -0.0556(4) 0.28094(7) 0.5723(2) 0.0172(6) Uani 1 1 d . . . H4A H -0.1306 0.2732 0.5117 0.021 Uiso 1 1 calc R . . C5 C 0.1446(3) 0.12608(7) 0.9680(2) 0.0160(6) Uani 1 1 d . . . C6 C -0.1161(4) 0.06725(7) 0.7041(3) 0.0201(6) Uani 1 1 d . . . H6A H -0.0413 0.0662 0.6453 0.024 Uiso 1 1 calc R . . O4 O 0.0023(2) 0.23051(4) 0.67090(17) 0.0154(4) Uani 1 1 d . . . C7 C 0.2118(3) 0.14358(6) 0.8757(2) 0.0148(6) Uani 1 1 d . . . H7A H 0.2926 0.1354 0.8306 0.018 Uiso 1 1 calc R . . C8 C 0.1940(4) 0.02992(6) 0.9371(3) 0.0177(6) Uani 1 1 d . . . C9 C 0.2019(4) 0.09355(7) 0.9945(3) 0.0174(6) Uani 1 1 d . . . H9B H 0.1446 0.0853 1.0609 0.021 Uiso 1 1 calc R . . H9A H 0.3183 0.0938 1.0205 0.021 Uiso 1 1 calc R . . C10 C -0.2829(4) 0.06651(8) 0.6686(3) 0.0262(7) Uani 1 1 d . . . H10A H -0.3195 0.0639 0.5872 0.031 Uiso 1 1 calc R . . C11 C -0.0344(4) 0.16907(7) 1.0119(3) 0.0182(6) Uani 1 1 d . . . H11A H -0.1150 0.1775 1.0566 0.022 Uiso 1 1 calc R . . C12 C 0.1197(4) 0.35894(7) 0.6775(3) 0.0183(6) Uani 1 1 d . . . H12B H 0.0285 0.3692 0.6320 0.022 Uiso 1 1 calc R . . H12A H 0.2185 0.3638 0.6386 0.022 Uiso 1 1 calc R . . C13 C 0.0318(3) 0.18554(6) 0.9211(2) 0.0144(5) Uani 1 1 d . . . C14 C 0.0443(4) 0.43305(7) 0.7336(3) 0.0241(7) Uani 1 1 d . . . H14A H -0.0576 0.4242 0.7115 0.029 Uiso 1 1 calc R . . C15 C 0.1410(3) 0.27310(7) 0.7449(2) 0.0130(5) Uani 1 1 d . . . C16 C 0.0917(3) 0.32430(7) 0.6704(3) 0.0155(6) Uani 1 1 d . . . C17 C 0.1771(3) 0.30400(7) 0.7534(2) 0.0153(6) Uani 1 1 d . . . H17A H 0.2556 0.3114 0.8122 0.018 Uiso 1 1 calc R . . C18 C 0.0258(4) 0.13900(7) 1.0337(2) 0.0183(6) Uani 1 1 d . . . H18A H -0.0160 0.1274 1.0948 0.022 Uiso 1 1 calc R . . C19 C -0.0952(4) 0.38325(7) 0.9968(3) 0.0238(7) Uani 1 1 d . . . H19A H -0.0072 0.3917 1.0448 0.029 Uiso 1 1 calc R . . C20 C 0.0240(3) 0.26169(6) 0.6557(2) 0.0148(5) Uani 1 1 d . . . C21 C 0.3385(4) -0.01864(8) 0.9535(3) 0.0296(8) Uani 1 1 d . . . H21A H 0.4171 -0.0319 0.9264 0.035 Uiso 1 1 calc R . . C22 C -0.0211(3) 0.31259(7) 0.5806(3) 0.0179(6) Uani 1 1 d . . . H22A H -0.0747 0.3261 0.5249 0.021 Uiso 1 1 calc R . . C23 C 0.0740(5) 0.46388(8) 0.7019(3) 0.0310(8) Uani 1 1 d . . . H23A H -0.0073 0.4753 0.6579 0.037 Uiso 1 1 calc R . . C24 C -0.3401(4) 0.07263(9) 0.8761(3) 0.0320(8) Uani 1 1 d . . . H24A H -0.4155 0.0746 0.9341 0.038 Uiso 1 1 calc R . . C25 C 0.1660(4) 0.41569(7) 0.7976(3) 0.0192(6) Uani 1 1 d . . . C26 C -0.1728(4) 0.07269(8) 0.9122(3) 0.0259(7) Uani 1 1 d . . . H26A H -0.1373 0.0748 0.9940 0.031 Uiso 1 1 calc R . . C27 C -0.3950(4) 0.06964(8) 0.7552(3) 0.0299(8) Uani 1 1 d . . . H27A H -0.5070 0.0697 0.7317 0.036 Uiso 1 1 calc R . . C28 C 0.3166(4) 0.42949(7) 0.8299(3) 0.0279(7) Uani 1 1 d . . . H28A H 0.3991 0.4181 0.8724 0.034 Uiso 1 1 calc R . . C29 C 0.1350(4) -0.00738(7) 1.0896(3) 0.0277(7) Uani 1 1 d . . . H29A H 0.0764 -0.0130 1.1547 0.033 Uiso 1 1 calc R . . C30 C 0.1068(4) 0.02095(7) 1.0340(3) 0.0261(7) Uani 1 1 d . . . H30A H 0.0285 0.0342 1.0618 0.031 Uiso 1 1 calc R . . C31 C -0.2469(4) 0.38120(8) 1.0432(3) 0.0281(7) Uani 1 1 d . . . H31A H -0.2607 0.3886 1.1208 0.034 Uiso 1 1 calc R . . C32 C -0.2047(4) 0.36018(7) 0.8105(3) 0.0219(6) Uani 1 1 d . . . H32A H -0.1928 0.3533 0.7319 0.026 Uiso 1 1 calc R . . C33 C 0.3466(5) 0.46007(8) 0.8001(4) 0.0361(8) Uani 1 1 d . . . H33A H 0.4480 0.4690 0.8227 0.043 Uiso 1 1 calc R . . B1 B 0.1027(4) 0.22200(7) 0.7857(3) 0.0143(6) Uani 1 1 d . . . C34 C 0.3108(4) 0.00979(7) 0.8982(3) 0.0237(7) Uani 1 1 d . . . H34A H 0.3713 0.0155 0.8341 0.028 Uiso 1 1 calc R . . C35 C -0.3555(4) 0.35760(8) 0.8584(3) 0.0280(7) Uani 1 1 d . . . H35A H -0.4430 0.3486 0.8120 0.034 Uiso 1 1 calc R . . C36 C -0.3779(4) 0.36813(8) 0.9734(3) 0.0284(7) Uani 1 1 d . . . H36A H -0.4801 0.3665 1.0041 0.034 Uiso 1 1 calc R . . C37 C 0.2499(4) -0.02741(8) 1.0487(3) 0.0273(7) Uani 1 1 d . . . H37A H 0.2674 -0.0466 1.0851 0.033 Uiso 1 1 calc R . . C38 C 0.2236(5) 0.47716(8) 0.7362(3) 0.0358(8) Uani 1 1 d . . . H38A H 0.2427 0.4977 0.7166 0.043 Uiso 1 1 calc R . . N1 N -0.3318(3) 0.21309(6) 0.7013(2) 0.0187(5) Uani 1 1 d . . . H45 H -0.218(5) 0.2179(8) 0.705(3) 0.027(9) Uiso 1 1 d . . . C39 C -0.3443(4) 0.18027(8) 0.7434(3) 0.0249(7) Uani 1 1 d . . . H39B H -0.4577 0.1736 0.7304 0.030 Uiso 1 1 calc R . . H39A H -0.3124 0.1793 0.8300 0.030 Uiso 1 1 calc R . . C40 C -0.4093(4) 0.23409(8) 0.7900(3) 0.0233(7) Uani 1 1 d . . . H40B H -0.5233 0.2282 0.7932 0.028 Uiso 1 1 calc R . . H40A H -0.3542 0.2310 0.8704 0.028 Uiso 1 1 calc R . . C41 C -0.3940(4) 0.21784(9) 0.5702(3) 0.0287(7) Uani 1 1 d . . . H41B H -0.3703 0.2389 0.5475 0.034 Uiso 1 1 calc R . . H41A H -0.3338 0.2042 0.5202 0.034 Uiso 1 1 calc R . . C42 C -0.5748(4) 0.21203(10) 0.5423(3) 0.0346(8) Uani 1 1 d . . . H42C H -0.6052 0.2165 0.4582 0.042 Uiso 1 1 calc R . . H42B H -0.6359 0.2251 0.5924 0.042 Uiso 1 1 calc R . . H42A H -0.5986 0.1908 0.5583 0.042 Uiso 1 1 calc R . . C43 C -0.2371(5) 0.15837(9) 0.6776(4) 0.0373(9) Uani 1 1 d . . . H43C H -0.2369 0.1384 0.7155 0.045 Uiso 1 1 calc R . . H43B H -0.1270 0.1663 0.6816 0.045 Uiso 1 1 calc R . . H43A H -0.2795 0.1566 0.5941 0.045 Uiso 1 1 calc R . . C44 C -0.4021(5) 0.26795(8) 0.7588(4) 0.0357(8) Uani 1 1 d . . . H44C H -0.4421 0.2799 0.8232 0.043 Uiso 1 1 calc R . . H44B H -0.4691 0.2718 0.6846 0.043 Uiso 1 1 calc R . . H44A H -0.2907 0.2737 0.7486 0.043 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 P1 0.0171(4) 0.0128(3) 0.0169(4) 0.0019(3) 0.0028(3) 0.0009(3) P2 0.0186(4) 0.0151(3) 0.0186(4) 0.0012(3) 0.0000(3) -0.0008(3) O1 0.0177(10) 0.0142(10) 0.0184(10) 0.0031(8) 0.0073(8) -0.0002(8) O2 0.0162(10) 0.0119(9) 0.0164(9) 0.0024(7) 0.0004(7) 0.0001(7) O3 0.0172(10) 0.0150(10) 0.0181(9) 0.0037(8) 0.0058(8) 0.0020(8) C1 0.0196(15) 0.0172(14) 0.0188(14) 0.0013(11) 0.0036(11) -0.0005(12) C2 0.0189(15) 0.0135(14) 0.0218(14) 0.0027(11) 0.0026(11) 0.0009(11) C3 0.0147(13) 0.0138(12) 0.0111(12) 0.0007(11) 0.0018(10) -0.0055(11) C4 0.0187(14) 0.0226(15) 0.0102(12) 0.0015(11) 0.0015(10) -0.0003(12) C5 0.0180(14) 0.0136(13) 0.0155(13) -0.0007(10) -0.0045(11) 0.0006(11) C6 0.0224(15) 0.0169(14) 0.0210(14) 0.0028(12) 0.0025(12) 0.0035(12) O4 0.0169(10) 0.0141(10) 0.0149(9) 0.0013(8) -0.0002(7) -0.0023(8) C7 0.0159(14) 0.0154(14) 0.0131(12) -0.0020(10) 0.0010(10) -0.0002(10) C8 0.0212(15) 0.0095(13) 0.0222(15) 0.0032(11) -0.0003(12) 0.0023(11) C9 0.0184(15) 0.0159(14) 0.0172(14) 0.0022(11) -0.0023(11) 0.0002(11) C10 0.0295(18) 0.0254(17) 0.0226(16) 0.0022(13) -0.0045(13) 0.0013(14) C11 0.0212(15) 0.0179(14) 0.0167(13) 0.0000(11) 0.0079(11) 0.0012(12) C12 0.0219(15) 0.0173(14) 0.0165(13) 0.0020(11) 0.0050(11) 0.0010(12) C13 0.0143(13) 0.0149(14) 0.0138(12) -0.0002(10) -0.0001(10) -0.0003(11) C14 0.0311(18) 0.0201(16) 0.0208(15) -0.0022(12) 0.0012(13) 0.0021(13) C15 0.0093(13) 0.0200(14) 0.0103(12) 0.0004(10) 0.0043(10) 0.0039(10) C16 0.0170(14) 0.0143(14) 0.0163(13) 0.0024(10) 0.0082(11) 0.0036(11) C17 0.0138(14) 0.0172(14) 0.0152(13) -0.0003(11) 0.0027(11) -0.0006(11) C18 0.0218(15) 0.0185(15) 0.0152(14) 0.0021(11) 0.0046(11) -0.0016(12) C19 0.0277(17) 0.0247(16) 0.0184(15) -0.0043(12) -0.0011(12) -0.0007(13) C20 0.0150(14) 0.0161(14) 0.0140(13) -0.0021(11) 0.0054(10) -0.0005(11) C21 0.037(2) 0.0245(17) 0.0273(17) 0.0001(13) 0.0035(14) 0.0151(15) C22 0.0183(14) 0.0208(15) 0.0147(13) 0.0062(11) 0.0028(11) 0.0057(12) C23 0.044(2) 0.0273(18) 0.0227(16) 0.0034(13) 0.0071(14) 0.0108(16) C24 0.0209(16) 0.045(2) 0.0311(18) 0.0086(15) 0.0081(13) 0.0027(16) C25 0.0257(16) 0.0142(14) 0.0185(14) -0.0027(11) 0.0065(12) 0.0006(12) C26 0.0229(16) 0.0344(19) 0.0202(15) 0.0029(13) 0.0010(12) -0.0002(13) C27 0.0173(16) 0.0335(19) 0.0377(19) 0.0100(15) -0.0049(14) -0.0019(14) C28 0.0280(17) 0.0209(16) 0.0344(18) 0.0069(13) -0.0001(14) -0.0022(13) C29 0.0369(19) 0.0204(17) 0.0270(17) 0.0073(13) 0.0103(14) -0.0048(14) C30 0.0265(17) 0.0197(16) 0.0334(18) 0.0034(13) 0.0106(14) 0.0035(13) C31 0.0384(19) 0.0306(18) 0.0156(14) -0.0008(13) 0.0053(13) 0.0085(15) C32 0.0227(16) 0.0254(16) 0.0178(14) -0.0023(12) 0.0036(12) -0.0011(12) C33 0.033(2) 0.0274(19) 0.048(2) -0.0005(16) 0.0074(17) -0.0122(15) B1 0.0146(15) 0.0127(15) 0.0160(15) -0.0004(12) 0.0029(12) 0.0010(12) C34 0.0278(17) 0.0248(16) 0.0190(15) 0.0022(12) 0.0055(12) 0.0051(13) C35 0.0237(17) 0.0328(17) 0.0273(17) 0.0017(14) 0.0018(14) -0.0020(15) C36 0.0243(17) 0.0336(19) 0.0286(17) 0.0092(14) 0.0092(13) 0.0071(14) C37 0.0378(19) 0.0182(16) 0.0248(16) 0.0046(12) -0.0033(14) 0.0015(14) C38 0.055(2) 0.0158(16) 0.039(2) 0.0035(14) 0.0158(17) -0.0019(16) N1 0.0130(12) 0.0282(14) 0.0154(12) 0.0020(10) 0.0041(9) -0.0028(10) C39 0.0224(16) 0.0273(17) 0.0243(16) 0.0073(13) -0.0034(13) -0.0035(13) C40 0.0166(15) 0.0343(18) 0.0196(15) 0.0010(13) 0.0062(12) 0.0021(13) C41 0.0237(17) 0.045(2) 0.0178(15) 0.0100(14) 0.0050(12) -0.0022(15) C42 0.0269(18) 0.055(2) 0.0206(16) 0.0096(15) -0.0031(13) -0.0072(16) C43 0.039(2) 0.0290(19) 0.043(2) -0.0114(16) -0.0059(16) -0.0018(16) C44 0.0289(19) 0.031(2) 0.048(2) -0.0035(16) 0.0092(16) 0.0073(15) _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 C2 1.839(3) . ? P1 C8 1.848(3) . ? P1 C9 1.860(3) . ? P2 C1 1.839(3) . ? P2 C25 1.841(3) . ? P2 C12 1.850(3) . ? O1 C3 1.370(3) . ? O1 B1 1.476(4) . ? O2 C15 1.365(3) . ? O2 B1 1.482(4) . ? O3 C13 1.366(3) . ? O3 B1 1.490(4) . ? C1 C32 1.393(4) . ? C1 C19 1.399(4) . ? C2 C26 1.391(4) . ? C2 C6 1.400(4) . ? C3 C7 1.380(4) . ? C3 C13 1.384(4) . ? C4 C20 1.365(4) . ? C4 C22 1.400(4) . ? C5 C18 1.379(4) . ? C5 C7 1.418(4) . ? C5 C9 1.504(4) . ? C6 C10 1.387(4) . ? O4 C20 1.373(3) . ? O4 B1 1.496(4) . ? C8 C34 1.387(4) . ? C8 C30 1.391(4) . ? C10 C27 1.386(5) . ? C11 C13 1.378(4) . ? C11 C18 1.405(4) . ? C12 C16 1.518(4) . ? C14 C25 1.391(4) . ? C14 C23 1.406(5) . ? C15 C17 1.371(4) . ? C15 C20 1.403(4) . ? C16 C22 1.390(4) . ? C16 C17 1.411(4) . ? C19 C31 1.384(5) . ? C21 C37 1.379(5) . ? C21 C34 1.384(5) . ? C23 C38 1.375(6) . ? C24 C27 1.377(5) . ? C24 C26 1.391(5) . ? C25 C28 1.386(4) . ? C28 C33 1.391(5) . ? C29 C30 1.381(4) . ? C29 C37 1.382(5) . ? C31 C36 1.385(5) . ? C32 C35 1.386(5) . ? C33 C38 1.390(5) . ? C35 C36 1.376(5) . ? N1 C39 1.501(4) . ? N1 C41 1.506(4) . ? N1 C40 1.514(4) . ? C39 C43 1.517(5) . ? C40 C44 1.508(5) . ? C41 C42 1.504(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 P1 C8 102.41(13) . . ? C2 P1 C9 102.77(13) . . ? C8 P1 C9 99.28(13) . . ? C1 P2 C25 102.85(14) . . ? C1 P2 C12 103.22(13) . . ? C25 P2 C12 98.74(13) . . ? C3 O1 B1 106.0(2) . . ? C15 O2 B1 106.6(2) . . ? C13 O3 B1 106.0(2) . . ? C32 C1 C19 117.7(3) . . ? C32 C1 P2 125.2(2) . . ? C19 C1 P2 116.8(2) . . ? C26 C2 C6 118.1(3) . . ? C26 C2 P1 125.8(2) . . ? C6 C2 P1 116.1(2) . . ? O1 C3 C7 126.8(3) . . ? O1 C3 C13 111.3(2) . . ? C7 C3 C13 121.9(3) . . ? C20 C4 C22 118.1(3) . . ? C18 C5 C7 119.7(3) . . ? C18 C5 C9 119.9(3) . . ? C7 C5 C9 120.4(3) . . ? C10 C6 C2 121.1(3) . . ? C20 O4 B1 106.2(2) . . ? C3 C7 C5 117.5(3) . . ? C34 C8 C30 118.3(3) . . ? C34 C8 P1 118.4(2) . . ? C30 C8 P1 123.2(2) . . ? C5 C9 P1 112.46(19) . . ? C27 C10 C6 119.7(3) . . ? C13 C11 C18 116.8(3) . . ? C16 C12 P2 114.2(2) . . ? O3 C13 C11 127.5(3) . . ? O3 C13 C3 110.8(2) . . ? C11 C13 C3 121.6(3) . . ? C25 C14 C23 120.5(3) . . ? O2 C15 C17 127.9(2) . . ? O2 C15 C20 110.6(2) . . ? C17 C15 C20 121.4(3) . . ? C22 C16 C17 119.8(3) . . ? C22 C16 C12 119.0(2) . . ? C17 C16 C12 121.2(3) . . ? C15 C17 C16 118.1(3) . . ? C5 C18 C11 122.5(3) . . ? C31 C19 C1 121.6(3) . . ? C4 C20 O4 128.6(3) . . ? C4 C20 C15 121.0(3) . . ? O4 C20 C15 110.3(2) . . ? C37 C21 C34 120.3(3) . . ? C16 C22 C4 121.4(3) . . ? C38 C23 C14 119.8(3) . . ? C27 C24 C26 120.6(3) . . ? C28 C25 C14 118.6(3) . . ? C28 C25 P2 118.4(2) . . ? C14 C25 P2 122.9(2) . . ? C2 C26 C24 120.5(3) . . ? C24 C27 C10 119.8(3) . . ? C25 C28 C33 121.3(3) . . ? C30 C29 C37 120.3(3) . . ? C29 C30 C8 120.8(3) . . ? C19 C31 C36 119.7(3) . . ? C35 C32 C1 120.4(3) . . ? C38 C33 C28 119.5(3) . . ? O1 B1 O2 113.0(2) . . ? O1 B1 O3 105.8(2) . . ? O2 B1 O3 111.0(2) . . ? O1 B1 O4 112.7(2) . . ? O2 B1 O4 104.9(2) . . ? O3 B1 O4 109.4(2) . . ? C21 C34 C8 120.8(3) . . ? C36 C35 C32 121.2(3) . . ? C35 C36 C31 119.4(3) . . ? C21 C37 C29 119.5(3) . . ? C23 C38 C33 120.3(3) . . ? C39 N1 C41 113.6(3) . . ? C39 N1 C40 108.9(2) . . ? C41 N1 C40 114.4(2) . . ? N1 C39 C43 112.7(3) . . ? C44 C40 N1 114.1(3) . . ? C42 C41 N1 114.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C25 P2 C1 C32 107.3(3) . . . . ? C12 P2 C1 C32 5.0(3) . . . . ? C25 P2 C1 C19 -78.3(3) . . . . ? C12 P2 C1 C19 179.4(2) . . . . ? C8 P1 C2 C26 68.8(3) . . . . ? C9 P1 C2 C26 -33.9(3) . . . . ? C8 P1 C2 C6 -110.3(2) . . . . ? C9 P1 C2 C6 147.0(2) . . . . ? B1 O1 C3 C7 180.0(3) . . . . ? B1 O1 C3 C13 -0.8(3) . . . . ? C26 C2 C6 C10 -3.1(4) . . . . ? P1 C2 C6 C10 176.1(2) . . . . ? O1 C3 C7 C5 178.8(2) . . . . ? C13 C3 C7 C5 -0.4(4) . . . . ? C18 C5 C7 C3 -0.5(4) . . . . ? C9 C5 C7 C3 179.4(2) . . . . ? C2 P1 C8 C34 131.0(2) . . . . ? C9 P1 C8 C34 -123.7(3) . . . . ? C2 P1 C8 C30 -50.7(3) . . . . ? C9 P1 C8 C30 54.7(3) . . . . ? C18 C5 C9 P1 120.1(3) . . . . ? C7 C5 C9 P1 -59.8(3) . . . . ? C2 P1 C9 C5 -59.8(2) . . . . ? C8 P1 C9 C5 -164.9(2) . . . . ? C2 C6 C10 C27 3.1(5) . . . . ? C1 P2 C12 C16 -73.2(2) . . . . ? C25 P2 C12 C16 -178.7(2) . . . . ? B1 O3 C13 C11 178.1(3) . . . . ? B1 O3 C13 C3 -2.6(3) . . . . ? C18 C11 C13 O3 178.7(3) . . . . ? C18 C11 C13 C3 -0.5(4) . . . . ? O1 C3 C13 O3 2.3(3) . . . . ? C7 C3 C13 O3 -178.5(2) . . . . ? O1 C3 C13 C11 -178.4(3) . . . . ? C7 C3 C13 C11 0.9(4) . . . . ? B1 O2 C15 C17 169.4(3) . . . . ? B1 O2 C15 C20 -8.7(3) . . . . ? P2 C12 C16 C22 139.0(2) . . . . ? P2 C12 C16 C17 -40.6(3) . . . . ? O2 C15 C17 C16 -177.2(2) . . . . ? C20 C15 C17 C16 0.7(4) . . . . ? C22 C16 C17 C15 -2.2(4) . . . . ? C12 C16 C17 C15 177.4(2) . . . . ? C7 C5 C18 C11 0.9(4) . . . . ? C9 C5 C18 C11 -179.0(3) . . . . ? C13 C11 C18 C5 -0.4(4) . . . . ? C32 C1 C19 C31 -0.8(5) . . . . ? P2 C1 C19 C31 -175.7(3) . . . . ? C22 C4 C20 O4 175.1(3) . . . . ? C22 C4 C20 C15 -2.0(4) . . . . ? B1 O4 C20 C4 -172.0(3) . . . . ? B1 O4 C20 C15 5.4(3) . . . . ? O2 C15 C20 C4 179.7(2) . . . . ? C17 C15 C20 C4 1.5(4) . . . . ? O2 C15 C20 O4 2.1(3) . . . . ? C17 C15 C20 O4 -176.1(2) . . . . ? C17 C16 C22 C4 1.7(4) . . . . ? C12 C16 C22 C4 -177.9(3) . . . . ? C20 C4 C22 C16 0.5(4) . . . . ? C25 C14 C23 C38 -1.1(5) . . . . ? C23 C14 C25 C28 0.3(4) . . . . ? C23 C14 C25 P2 -176.2(2) . . . . ? C1 P2 C25 C28 141.6(2) . . . . ? C12 P2 C25 C28 -112.5(3) . . . . ? C1 P2 C25 C14 -41.8(3) . . . . ? C12 P2 C25 C14 64.0(3) . . . . ? C6 C2 C26 C24 1.6(5) . . . . ? P1 C2 C26 C24 -177.4(3) . . . . ? C27 C24 C26 C2 -0.3(5) . . . . ? C26 C24 C27 C10 0.3(6) . . . . ? C6 C10 C27 C24 -1.7(5) . . . . ? C14 C25 C28 C33 0.3(5) . . . . ? P2 C25 C28 C33 177.0(3) . . . . ? C37 C29 C30 C8 -0.6(5) . . . . ? C34 C8 C30 C29 -0.4(5) . . . . ? P1 C8 C30 C29 -178.8(3) . . . . ? C1 C19 C31 C36 1.4(5) . . . . ? C19 C1 C32 C35 -0.5(4) . . . . ? P2 C1 C32 C35 173.8(2) . . . . ? C25 C28 C33 C38 -0.3(5) . . . . ? C3 O1 B1 O2 121.0(2) . . . . ? C3 O1 B1 O3 -0.7(3) . . . . ? C3 O1 B1 O4 -120.3(2) . . . . ? C15 O2 B1 O1 134.6(2) . . . . ? C15 O2 B1 O3 -106.7(2) . . . . ? C15 O2 B1 O4 11.5(3) . . . . ? C13 O3 B1 O1 2.0(3) . . . . ? C13 O3 B1 O2 -120.9(2) . . . . ? C13 O3 B1 O4 123.7(2) . . . . ? C20 O4 B1 O1 -133.5(2) . . . . ? C20 O4 B1 O2 -10.2(3) . . . . ? C20 O4 B1 O3 109.0(2) . . . . ? C37 C21 C34 C8 0.0(5) . . . . ? C30 C8 C34 C21 0.7(5) . . . . ? P1 C8 C34 C21 179.2(3) . . . . ? C1 C32 C35 C36 1.4(5) . . . . ? C32 C35 C36 C31 -0.8(5) . . . . ? C19 C31 C36 C35 -0.5(5) . . . . ? C34 C21 C37 C29 -0.9(5) . . . . ? C30 C29 C37 C21 1.2(5) . . . . ? C14 C23 C38 C33 1.2(5) . . . . ? C28 C33 C38 C23 -0.5(6) . . . . ? C41 N1 C39 C43 64.3(3) . . . . ? C40 N1 C39 C43 -166.9(3) . . . . ? C39 N1 C40 C44 179.1(3) . . . . ? C41 N1 C40 C44 -52.6(4) . . . . ? C39 N1 C41 C42 64.8(4) . . . . ? C40 N1 C41 C42 -61.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.292 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.062