#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/40/2104073.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2104073 loop_ _publ_author_name 'van der Lee, A.' 'Rolland, M.' 'Marat, X.' 'Virieux, D.' 'Volle, J.-N.' 'Pirat, J.-L.' _publ_section_title ; Structure-directing weak phosphoryl XH···O=P (X = C, N) hydrogen bonds in cyclic oxazaphospholidines and oxazaphosphinanes ; _journal_coeditor_code GP5020 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 196 _journal_page_last 205 _journal_volume 64 _journal_year 2008 _chemical_formula_moiety 'C20 H26 N O2 P' _chemical_formula_sum 'C20 H26 N O2 P' _chemical_formula_weight 343.39 _chemical_name_systematic ; (2S,4S,5R)and(2R,4R,5S)-3-tert-butyl-2-ethyl-4,5- diphenyl-[1,3,2]-oxazaphospholidine2-oxide ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_method CRYSTALS_ver_12.84 _cell_angle_alpha 97.644(3) _cell_angle_beta 93.038(2) _cell_angle_gamma 98.742(2) _cell_formula_units_Z 4 _cell_length_a 6.7231(5) _cell_length_b 11.9766(6) _cell_length_c 23.6865(16) _cell_measurement_reflns_used 11434 _cell_measurement_temperature 120 _cell_measurement_theta_max 16.54 _cell_measurement_theta_min 2.49 _cell_volume 1863.1(2) _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_collection 'SMART (Siemens, 1993)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _diffrn_ambient_temperature 120 _diffrn_measured_fraction_theta_full 0.953 _diffrn_measured_fraction_theta_max 0.930 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.50606 _diffrn_reflns_av_R_equivalents 0.073 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_number 32894 _diffrn_reflns_theta_full 15.660 _diffrn_reflns_theta_max 20.880 _diffrn_reflns_theta_min 1.179 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_crystal_colour 'translucent pale white' _exptl_crystal_density_diffrn 1.224 _exptl_crystal_description needle _exptl_crystal_F_000 736 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.48 _refine_diff_density_min -0.58 _refine_ls_extinction_coef 66E1(9) _refine_ls_extinction_method 'Larson (1970), Equation 22' _refine_ls_goodness_of_fit_ref 1.0621 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 434 _refine_ls_number_reflns 7201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0497 _refine_ls_shift/su_max 0.000874 _refine_ls_structure_factor_coef F _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.507 0.574 0.220 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0783 _refine_ls_wR_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.0533 _reflns_number_gt 7201 _reflns_number_total 11718 _reflns_threshold_expression I>2.0\s(I) _[local]_cod_data_source_file gp5020.cif _[local]_cod_data_source_block II _[local]_cod_cif_authors_sg_H-M 'P -1 ' _cod_database_code 2104073 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0010 0.0007 ; International Tables Vol C 4.2.6.8 and 6.1.1.4, dispersion factors from Interpolated values from CXRO/LLNL data ; H 0.0000 0.0000 ; International Tables Vol C 4.2.6.8 and 6.1.1.4, dispersion factors from Interpolated values from CXRO/LLNL data ; N 0.0028 0.0016 ; International Tables Vol C 4.2.6.8 and 6.1.1.4, dispersion factors from Interpolated values from CXRO/LLNL data ; O 0.0046 0.0029 ; International Tables Vol C 4.2.6.8 and 6.1.1.4, dispersion factors from Interpolated values from CXRO/LLNL data ; P 0.0561 0.0483 ; International Tables Vol C 4.2.6.8 and 6.1.1.4, dispersion factors from Interpolated values from CXRO/LLNL data ; loop_ _atom_site_type_symbol _atom_site_label _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 O O1 0.77651(15) 0.31881(9) 0.42493(5) 0.0209 Uani 1.0000 P P2 0.81472(5) 0.18934(3) 0.410737(16) 0.0171 Uani 1.0000 N N3 0.59819(16) 0.14115(10) 0.37339(5) 0.0160 Uani 1.0000 C C4 0.47693(18) 0.23247(11) 0.36808(6) 0.0144 Uani 1.0000 C C5 0.56125(19) 0.32181(11) 0.42069(6) 0.0167 Uani 1.0000 O O6 1.00407(15) 0.17922(11) 0.38347(5) 0.0285 Uani 1.0000 C C7 0.5095(2) 0.02075(12) 0.35146(7) 0.0197 Uani 1.0000 C C8 0.6752(2) -0.05377(13) 0.34813(7) 0.0266 Uani 1.0000 C C9 0.3515(3) -0.02224(14) 0.39119(9) 0.0346 Uani 1.0000 C C10 0.4092(3) 0.01434(14) 0.29150(8) 0.0321 Uani 1.0000 C C11 0.8173(2) 0.13664(14) 0.47865(7) 0.0249 Uani 1.0000 C C12 1.0154(3) 0.17880(18) 0.51469(8) 0.0358 Uani 1.0000 C C13 0.4924(2) 0.28161(11) 0.31219(6) 0.0161 Uani 1.0000 C C14 0.3241(2) 0.31951(13) 0.28902(7) 0.0220 Uani 1.0000 C C15 0.3346(3) 0.37081(14) 0.23960(7) 0.0290 Uani 1.0000 C C16 0.5133(3) 0.38401(15) 0.21295(7) 0.0326 Uani 1.0000 C C17 0.6823(3) 0.34621(16) 0.23553(7) 0.0315 Uani 1.0000 C C18 0.6713(2) 0.29432(14) 0.28493(6) 0.0233 Uani 1.0000 C C19 0.5196(2) 0.44037(12) 0.41757(6) 0.0194 Uani 1.0000 C C20 0.3338(3) 0.46618(14) 0.43280(7) 0.0279 Uani 1.0000 C C21 0.2833(3) 0.57296(16) 0.42753(9) 0.0380 Uani 1.0000 C C22 0.4205(3) 0.65441(15) 0.40754(8) 0.0389 Uani 1.0000 C C23 0.6063(3) 0.62959(14) 0.39270(8) 0.0346 Uani 1.0000 C C24 0.6570(3) 0.52238(13) 0.39744(7) 0.0260 Uani 1.0000 O O25 0.75529(14) 0.70375(8) 0.06658(4) 0.0184 Uani 1.0000 P P26 0.71085(5) 0.83190(3) 0.081143(15) 0.0150 Uani 1.0000 N N27 0.93126(16) 0.88544(9) 0.11615(5) 0.0147 Uani 1.0000 C C28 1.05303(18) 0.79439(11) 0.12373(5) 0.0134 Uani 1.0000 C C29 0.97127(18) 0.70373(11) 0.07130(6) 0.0150 Uani 1.0000 O O30 0.52514(15) 0.84066(10) 0.11036(5) 0.0249 Uani 1.0000 C C31 0.9832(2) 1.00090(11) 0.15068(6) 0.0174 Uani 1.0000 C C32 0.8722(3) 1.08434(13) 0.12286(8) 0.0282 Uani 1.0000 C C33 1.2104(2) 1.04049(13) 0.15114(7) 0.0243 Uani 1.0000 C C34 0.9180(2) 0.99958(14) 0.21169(7) 0.0257 Uani 1.0000 C C35 0.6924(2) 0.87958(13) 0.01208(6) 0.0218 Uani 1.0000 C C36 0.5017(2) 0.81638(14) -0.02358(7) 0.0278 Uani 1.0000 C C37 1.03775(19) 0.74499(11) 0.17934(6) 0.0149 Uani 1.0000 C C38 0.8540(2) 0.71596(13) 0.20296(6) 0.0219 Uani 1.0000 C C39 0.8468(2) 0.66298(15) 0.25174(7) 0.0280 Uani 1.0000 C C40 1.0230(3) 0.63861(15) 0.27774(7) 0.0307 Uani 1.0000 C C41 1.2053(3) 0.66725(15) 0.25460(7) 0.0278 Uani 1.0000 C C42 1.2132(2) 0.72004(12) 0.20559(6) 0.0194 Uani 1.0000 C C43 1.01773(19) 0.58654(11) 0.07508(6) 0.0155 Uani 1.0000 C C44 0.8778(2) 0.50090(12) 0.09169(6) 0.0200 Uani 1.0000 C C45 0.9311(2) 0.39454(12) 0.09658(7) 0.0232 Uani 1.0000 C C46 1.1236(2) 0.37327(13) 0.08559(7) 0.0248 Uani 1.0000 C C47 1.2625(2) 0.45848(13) 0.06876(7) 0.0256 Uani 1.0000 C C48 1.2102(2) 0.56452(12) 0.06352(7) 0.0212 Uani 1.0000 H H49 0.5067 0.2949 0.4547 0.0500 Uiso 1.0000 H H50 0.3427 0.2031 0.3734 0.0500 Uiso 1.0000 H H51 0.7123 0.1664 0.4985 0.0500 Uiso 1.0000 H H52 0.7881 0.0561 0.4723 0.0500 Uiso 1.0000 H H53 1.0061 0.1512 0.5494 0.0500 Uiso 1.0000 H H54 1.1204 0.1496 0.4948 0.0500 Uiso 1.0000 H H55 1.0397 0.2584 0.5195 0.0500 Uiso 1.0000 H H56 0.7747 -0.0282 0.3249 0.0500 Uiso 1.0000 H H57 0.7314 -0.0561 0.3854 0.0500 Uiso 1.0000 H H58 0.6129 -0.1289 0.3309 0.0500 Uiso 1.0000 H H59 0.4197 -0.0239 0.4270 0.0500 Uiso 1.0000 H H60 0.2881 -0.0976 0.3762 0.0500 Uiso 1.0000 H H61 0.2553 0.0259 0.3961 0.0500 Uiso 1.0000 H H62 0.3508 -0.0588 0.2784 0.0500 Uiso 1.0000 H H63 0.3056 0.0581 0.2930 0.0500 Uiso 1.0000 H H64 0.5016 0.0385 0.2661 0.0500 Uiso 1.0000 H H65 0.7841 0.2681 0.3001 0.0500 Uiso 1.0000 H H66 0.2091 0.3113 0.3069 0.0500 Uiso 1.0000 H H67 0.2261 0.3963 0.2251 0.0500 Uiso 1.0000 H H68 0.5223 0.4172 0.1808 0.0500 Uiso 1.0000 H H69 0.8037 0.3530 0.2173 0.0500 Uiso 1.0000 H H70 0.2423 0.4113 0.4465 0.0500 Uiso 1.0000 H H71 0.1634 0.5892 0.4376 0.0500 Uiso 1.0000 H H72 0.3899 0.7249 0.4046 0.0500 Uiso 1.0000 H H73 0.6953 0.6818 0.3778 0.0500 Uiso 1.0000 H H74 0.7775 0.5052 0.3870 0.0500 Uiso 1.0000 H H75 1.1868 0.8207 0.1181 0.0500 Uiso 1.0000 H H76 1.0266 0.7294 0.0382 0.0500 Uiso 1.0000 H H77 0.8092 0.8672 -0.0068 0.0500 Uiso 1.0000 H H78 0.6885 0.9579 0.0180 0.0500 Uiso 1.0000 H H79 0.3885 0.8352 -0.0054 0.0500 Uiso 1.0000 H H80 0.5021 0.8392 -0.0594 0.0500 Uiso 1.0000 H H81 0.4990 0.7369 -0.0273 0.0500 Uiso 1.0000 H H82 0.7346 1.0637 0.1208 0.0500 Uiso 1.0000 H H83 0.9141 1.0894 0.0857 0.0500 Uiso 1.0000 H H84 0.9062 1.1575 0.1442 0.0500 Uiso 1.0000 H H85 1.2826 0.9936 0.1693 0.0500 Uiso 1.0000 H H86 1.2411 1.1166 0.1704 0.0500 Uiso 1.0000 H H87 1.2526 1.0401 0.1136 0.0500 Uiso 1.0000 H H88 0.9412 1.0745 0.2313 0.0500 Uiso 1.0000 H H89 0.9919 0.9516 0.2306 0.0500 Uiso 1.0000 H H90 0.7801 0.9710 0.2117 0.0500 Uiso 1.0000 H H91 1.3328 0.7363 0.1895 0.0500 Uiso 1.0000 H H92 1.3209 0.6502 0.2719 0.0500 Uiso 1.0000 H H93 1.0153 0.6023 0.3099 0.0500 Uiso 1.0000 H H94 0.7259 0.6464 0.2676 0.0500 Uiso 1.0000 H H95 0.7379 0.7323 0.1862 0.0500 Uiso 1.0000 H H96 1.3032 0.6215 0.0529 0.0500 Uiso 1.0000 H H97 1.3853 0.4454 0.0605 0.0500 Uiso 1.0000 H H98 1.1606 0.3049 0.0900 0.0500 Uiso 1.0000 H H99 0.8351 0.3376 0.1090 0.0500 Uiso 1.0000 H H100 0.7517 0.5152 0.1007 0.0500 Uiso 1.0000 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0148(5) 0.0197(5) 0.0279(5) 0.0016(4) -0.0040(4) 0.0055(4) P2 0.01208(16) 0.02038(18) 0.02088(18) 0.00461(13) 0.00099(13) 0.00844(15) N3 0.0135(5) 0.0147(5) 0.0215(6) 0.0052(4) 0.0004(4) 0.0056(5) C4 0.0110(5) 0.0139(6) 0.0193(6) 0.0035(4) 0.0019(5) 0.0048(5) C5 0.0154(6) 0.0178(6) 0.0180(6) 0.0044(5) 0.0004(5) 0.0049(5) O6 0.0135(5) 0.0382(7) 0.0373(7) 0.0073(4) 0.0053(4) 0.0138(6) C7 0.0196(6) 0.0143(6) 0.0263(7) 0.0047(5) 0.0025(5) 0.0042(6) C8 0.0310(8) 0.0228(7) 0.0295(8) 0.0145(6) 0.0022(6) 0.0044(7) C9 0.0289(8) 0.0210(7) 0.0569(12) 0.0029(6) 0.0141(8) 0.0138(8) C10 0.0366(9) 0.0200(7) 0.0369(9) 0.0071(6) -0.0140(7) -0.0024(7) C11 0.0259(7) 0.0284(8) 0.0231(7) 0.0075(6) -0.0016(6) 0.0109(7) C12 0.0329(9) 0.0445(11) 0.0314(9) 0.0122(8) -0.0108(7) 0.0094(8) C13 0.0165(6) 0.0138(6) 0.0179(6) 0.0022(5) -0.0015(5) 0.0035(5) C14 0.0207(7) 0.0218(7) 0.0239(7) 0.0060(5) -0.0039(5) 0.0049(6) C15 0.0335(9) 0.0272(8) 0.0279(8) 0.0089(7) -0.0075(7) 0.0096(7) C16 0.0441(10) 0.0303(9) 0.0248(8) 0.0019(7) -0.0024(7) 0.0151(7) C17 0.0310(8) 0.0400(10) 0.0253(8) 0.0014(7) 0.0057(6) 0.0152(8) C18 0.0197(7) 0.0292(8) 0.0229(7) 0.0043(6) 0.0029(5) 0.0103(6) C19 0.0246(7) 0.0165(6) 0.0167(6) 0.0049(5) -0.0027(5) 0.0012(5) C20 0.0295(8) 0.0251(8) 0.0305(8) 0.0112(6) 0.0016(6) 0.0019(7) C21 0.0464(11) 0.0317(9) 0.0388(10) 0.0245(8) -0.0028(8) -0.0031(8) C22 0.0655(14) 0.0214(8) 0.0316(9) 0.0197(8) -0.0090(9) 0.0009(7) C23 0.0564(12) 0.0176(7) 0.0282(8) 0.0026(7) -0.0063(8) 0.0051(7) C24 0.0328(8) 0.0182(7) 0.0270(8) 0.0030(6) -0.0021(6) 0.0057(6) O25 0.0137(4) 0.0160(5) 0.0252(5) 0.0019(4) -0.0023(4) 0.0045(4) P26 0.00939(15) 0.01635(16) 0.02064(18) 0.00295(12) 0.00081(12) 0.00666(14) N27 0.0117(5) 0.0124(5) 0.0208(5) 0.0029(4) 0.0006(4) 0.0043(4) C28 0.0098(5) 0.0136(5) 0.0180(6) 0.0036(4) 0.0015(4) 0.0047(5) C29 0.0109(5) 0.0160(6) 0.0187(6) 0.0025(4) 0.0013(5) 0.0037(5) O30 0.0119(5) 0.0308(6) 0.0343(6) 0.0054(4) 0.0061(4) 0.0090(5) C31 0.0173(6) 0.0131(6) 0.0226(7) 0.0035(5) 0.0014(5) 0.0038(5) C32 0.0332(9) 0.0174(7) 0.0357(9) 0.0100(6) -0.0041(7) 0.0051(7) C33 0.0189(7) 0.0199(7) 0.0316(8) -0.0031(5) 0.0017(6) 0.0023(6) C34 0.0289(8) 0.0255(7) 0.0231(7) 0.0072(6) 0.0070(6) -0.0002(6) C35 0.0196(7) 0.0230(7) 0.0240(7) 0.0025(5) -0.0018(5) 0.0099(6) C36 0.0245(7) 0.0290(8) 0.0304(8) 0.0045(6) -0.0091(6) 0.0099(7) C37 0.0145(6) 0.0133(6) 0.0173(6) 0.0030(5) 0.0001(5) 0.0033(5) C38 0.0174(6) 0.0279(7) 0.0223(7) 0.0032(5) 0.0038(5) 0.0103(6) C39 0.0280(8) 0.0330(9) 0.0254(8) 0.0013(7) 0.0060(6) 0.0150(7) C40 0.0377(9) 0.0318(9) 0.0257(8) 0.0057(7) 0.0014(7) 0.0152(7) C41 0.0279(8) 0.0308(8) 0.0264(8) 0.0081(6) -0.0053(6) 0.0097(7) C42 0.0166(6) 0.0195(6) 0.0233(7) 0.0057(5) -0.0021(5) 0.0053(6) C43 0.0161(6) 0.0133(6) 0.0175(6) 0.0038(5) 0.0004(5) 0.0029(5) C44 0.0182(6) 0.0173(6) 0.0253(7) 0.0021(5) 0.0004(5) 0.0070(6) C45 0.0268(7) 0.0174(7) 0.0256(7) 0.0019(6) -0.0013(6) 0.0066(6) C46 0.0306(8) 0.0166(6) 0.0278(8) 0.0089(6) -0.0040(6) 0.0017(6) C47 0.0207(7) 0.0198(7) 0.0366(9) 0.0087(5) 0.0002(6) -0.0005(7) C48 0.0183(6) 0.0166(6) 0.0289(7) 0.0045(5) 0.0035(5) 0.0017(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag P2 O1 1.605(2) yes P2 O6 1.472(2) yes P2 N3 1.645(2) yes P2 C11 1.805(3) yes P26 O30 1.470(2) yes P26 N27 1.654(2) yes P26 O25 1.605(2) yes P26 C35 1.807(3) yes O1 C5 1.451(3) yes O25 C29 1.450(3) yes N3 C4 1.475(3) yes N3 C7 1.486(3) yes N27 C31 1.491(3) yes N27 C28 1.483(3) yes C4 C13 1.521(3) no C4 C5 1.551(3) no C5 C19 1.498(3) no C7 C10 1.527(4) no C7 C8 1.529(4) no C7 C9 1.532(5) no C11 C12 1.522(4) no C13 C14 1.396(4) no C13 C18 1.392(4) no C14 C15 1.392(4) no C15 C16 1.384(5) no C16 C17 1.391(5) no C17 C18 1.397(4) no C19 C20 1.387(4) no C19 C24 1.394(4) no C20 C21 1.392(5) no C21 C22 1.388(6) no C22 C23 1.380(6) no C23 C24 1.395(4) no C4 H50 0.9400 no C5 H49 0.9800 no C8 H57 0.9500 no C8 H56 0.9300 no C8 H58 0.9600 no C9 H59 0.9500 no C9 H60 0.9500 no C9 H61 0.9300 no C10 H62 0.9100 no C10 H63 0.9300 no C10 H64 0.9300 no C11 H51 0.9600 no C11 H52 0.9500 no C12 H53 0.9300 no C12 H54 0.9500 no C12 H55 0.9300 no C14 H66 0.9000 no C15 H67 0.9000 no C16 H68 0.9100 no C17 H69 0.9400 no C18 H65 0.9400 no C20 H70 0.9300 no C21 H71 0.8900 no C22 H72 0.9100 no C23 H73 0.9200 no C24 H74 0.9000 no C28 C29 1.553(3) no C28 C37 1.516(3) no C29 C43 1.498(3) no C31 C32 1.529(4) no C31 C33 1.529(4) no C31 C34 1.534(4) no C35 C36 1.533(4) no C37 C38 1.400(4) no C37 C42 1.395(4) no C38 C39 1.390(4) no C39 C40 1.395(5) no C40 C41 1.384(5) no C41 C42 1.394(4) no C43 C44 1.395(4) no C43 C48 1.393(4) no C44 C45 1.393(3) no C45 C46 1.388(4) no C46 C47 1.389(4) no C47 C48 1.387(3) no C28 H75 0.9300 no C29 H76 0.9500 no C32 H82 0.9200 no C32 H83 0.9500 no C32 H84 0.9400 no C33 H85 0.9300 no C33 H86 0.9500 no C33 H87 0.9500 no C34 H88 0.9400 no C34 H89 0.9500 no C34 H90 0.9400 no C35 H77 0.9500 no C35 H78 0.9300 no C36 H79 0.9400 no C36 H80 0.9300 no C36 H81 0.9400 no C38 H95 0.9200 no C39 H94 0.9200 no C40 H93 0.9300 no C41 H92 0.9200 no C42 H91 0.9100 no C44 H100 0.9200 no C45 H99 0.9500 no C46 H98 0.9100 no C47 H97 0.8900 no C48 H96 0.9200 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O1 P2 O6 113.21(13) yes O1 P2 N3 96.02(11) yes O1 P2 C11 105.03(14) yes O6 P2 N3 119.21(12) yes O6 P2 C11 111.04(13) yes N3 P2 C11 110.67(12) yes N27 P26 C35 111.18(12) yes O25 P26 N27 96.46(11) yes O25 P26 C35 103.73(11) yes O25 P26 O30 113.94(12) yes O30 P26 C35 110.75(13) yes O30 P26 N27 119.06(12) yes P2 O1 C5 109.54(16) yes P26 O25 C29 109.59(15) yes P2 N3 C7 128.14(18) yes P2 N3 C4 111.97(16) yes C4 N3 C7 119.54(19) yes C28 N27 C31 121.12(19) yes P26 N27 C31 125.57(17) yes P26 N27 C28 111.09(15) yes C5 C4 C13 112.6(2) no N3 C4 C13 114.38(19) yes N3 C4 C5 102.21(18) yes O1 C5 C4 104.65(19) yes O1 C5 C19 111.3(2) yes C4 C5 C19 115.1(2) no N3 C7 C10 109.4(2) yes C8 C7 C9 110.2(2) no C8 C7 C10 108.4(2) no C9 C7 C10 109.4(3) no N3 C7 C8 110.1(2) yes N3 C7 C9 109.3(2) yes P2 C11 C12 112.6(2) yes C14 C13 C18 119.3(2) no C4 C13 C14 118.6(2) no C4 C13 C18 122.1(2) no C13 C14 C15 120.6(3) no C14 C15 C16 119.9(3) no C15 C16 C17 120.1(3) no C16 C17 C18 120.0(3) no C13 C18 C17 120.2(3) no C5 C19 C20 118.1(2) no C5 C19 C24 122.2(2) no C20 C19 C24 119.6(3) no C19 C20 C21 120.4(3) no C20 C21 C22 119.8(4) no C21 C22 C23 120.1(3) no C22 C23 C24 120.4(3) no C19 C24 C23 119.8(3) no C5 C4 H50 108.00 no N3 C4 H50 108.00 no C13 C4 H50 111.00 no C19 C5 H49 110.00 no C4 C5 H49 108.00 no O1 C5 H49 107.00 no C7 C8 H56 112.00 no C7 C8 H57 110.00 no C7 C8 H58 107.00 no H57 C8 H58 110.00 no H56 C8 H57 111.00 no H56 C8 H58 107.00 no C7 C9 H59 108.00 no H59 C9 H60 109.00 no C7 C9 H60 110.00 no C7 C9 H61 111.00 no H60 C9 H61 110.00 no H59 C9 H61 109.00 no C7 C10 H64 112.00 no C7 C10 H63 109.00 no H63 C10 H64 111.00 no H62 C10 H63 107.00 no H62 C10 H64 109.00 no C7 C10 H62 110.00 no P2 C11 H52 109.00 no C12 C11 H51 108.00 no C12 C11 H52 112.00 no H51 C11 H52 110.00 no P2 C11 H51 106.00 no C11 C12 H53 109.00 no C11 C12 H54 108.00 no H54 C12 H55 110.00 no H53 C12 H55 112.00 no C11 C12 H55 109.00 no H53 C12 H54 110.00 no C15 C14 H66 121.00 no C13 C14 H66 119.00 no C14 C15 H67 120.00 no C16 C15 H67 120.00 no C15 C16 H68 121.00 no C17 C16 H68 119.00 no C18 C17 H69 119.00 no C16 C17 H69 121.00 no C13 C18 H65 119.00 no C17 C18 H65 120.00 no C21 C20 H70 120.00 no C19 C20 H70 120.00 no C22 C21 H71 120.00 no C20 C21 H71 120.00 no C21 C22 H72 120.00 no C23 C22 H72 119.00 no C22 C23 H73 121.00 no C24 C23 H73 119.00 no C19 C24 H74 120.00 no C23 C24 H74 121.00 no N27 C28 C29 101.51(17) yes N27 C28 C37 116.56(19) yes C29 C28 C37 112.0(2) no O25 C29 C28 104.99(18) yes O25 C29 C43 111.17(19) yes C28 C29 C43 114.9(2) no N27 C31 C32 109.0(2) yes N27 C31 C33 108.7(2) yes N27 C31 C34 111.2(2) yes C32 C31 C33 108.9(2) no C32 C31 C34 108.0(2) no C33 C31 C34 110.8(2) no P26 C35 C36 110.86(19) yes C28 C37 C38 122.7(2) no C28 C37 C42 118.2(2) no C38 C37 C42 118.9(2) no C37 C38 C39 120.3(3) no C38 C39 C40 120.4(3) no C39 C40 C41 119.5(3) no C40 C41 C42 120.3(3) no C37 C42 C41 120.5(3) no C29 C43 C44 122.2(2) no C29 C43 C48 118.3(2) no C44 C43 C48 119.5(2) no C43 C44 C45 119.9(2) no C44 C45 C46 120.4(2) no C45 C46 C47 119.6(2) no C46 C47 C48 120.3(3) no C43 C48 C47 120.3(2) no N27 C28 H75 109.00 no C29 C28 H75 106.00 no C37 C28 H75 111.00 no O25 C29 H76 109.00 no C28 C29 H76 108.00 no C43 C29 H76 109.00 no C31 C32 H82 113.00 no C31 C32 H83 110.00 no C31 C32 H84 109.00 no H82 C32 H83 109.00 no H82 C32 H84 108.00 no H83 C32 H84 107.00 no C31 C33 H85 111.00 no C31 C33 H86 108.00 no C31 C33 H87 111.00 no H85 C33 H86 110.00 no H85 C33 H87 108.00 no H86 C33 H87 108.00 no C31 C34 H88 109.00 no C31 C34 H89 109.00 no C31 C34 H90 111.00 no H88 C34 H89 111.00 no H88 C34 H90 108.00 no H89 C34 H90 108.00 no P26 C35 H77 109.00 no P26 C35 H78 108.00 no C36 C35 H77 111.00 no C36 C35 H78 110.00 no H77 C35 H78 109.00 no C35 C36 H79 109.00 no C35 C36 H80 108.00 no C35 C36 H81 111.00 no H79 C36 H80 110.00 no H79 C36 H81 110.00 no H80 C36 H81 109.00 no C37 C38 H95 120.00 no C39 C38 H95 120.00 no C38 C39 H94 120.00 no C40 C39 H94 120.00 no C39 C40 H93 119.00 no C41 C40 H93 121.00 no C40 C41 H92 119.00 no C42 C41 H92 121.00 no C37 C42 H91 119.00 no C41 C42 H91 120.00 no C43 C44 H100 120.00 no C45 C44 H100 120.00 no C44 C45 H99 119.00 no C46 C45 H99 121.00 no C45 C46 H98 121.00 no C47 C46 H98 120.00 no C46 C47 H97 121.00 no C48 C47 H97 119.00 no C43 C48 H96 119.00 no C47 C48 H96 120.00 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C4 H50 O6 1_455 0.9400 2.2800 3.196(3) 165.00 yes C28 H75 O30 1_655 0.9300 2.2700 3.179(3) 165.00 yes