# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_[PBB-OH][HP(t-Bu)3] _database_code_depnum_ccdc_archive 'CCDC 905438' #TrackingRef '008TAQA12.cif' #============================================================================== _audit_creation_date 12-09-25 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title 008TAQA12 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 16.0095(3) _cell_length_b 16.0095(3) _cell_length_c 15.8189(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3511.26(13) _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 ' _symmetry_space_group_name_Hall 'R 3 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/3,y+2/3,z+2/3 x+2/3,y+1/3,z+1/3 -y,x-y,z -y+1/3,x-y+2/3,z+2/3 -y+2/3,x-y+1/3,z+1/3 -x+y,-x,z -x+y+1/3,-x+2/3,z+2/3 -x+y+2/3,-x+1/3,z+1/3 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 3 # Given Formula = C48 H29 B1.00 F27 O1.00 P1.00 # Dc = 1.67 Fooo = 1764.00 Mu = 2.06 M = 392.16 # Found Formula = C48 H29.00 B1 F27 O1 P1 # Dc = 1.67 FOOO = 1764.00 Mu = 2.06 M = 392.16 _chemical_formula_sum 'C48 H29.00 B1 F27 O1 P1' _chemical_formula_moiety 'C48 H29.00 B1 F27 O1 P1' _chemical_compound_source syn _chemical_formula_weight 1176.49 _cell_measurement_reflns_used 1778 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_min 0.160 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.350 _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1764 _exptl_absorpt_coefficient_mu 0.206 # Sheldrick geometric approximatio 0.96 0.97 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.97 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 19434 _reflns_number_total 3541 _diffrn_reflns_av_R_equivalents 0.065 # Number of reflections without Friedels Law is 3541 # Number of reflections with Friedels Law is 1779 # Theoretical number of reflections is about 1788 _diffrn_reflns_theta_min 5.362 _diffrn_reflns_theta_max 27.475 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.925 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -20 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min -20 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 4.40 _oxford_diffrn_Wilson_scale 38.38 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.55 _refine_diff_density_max 0.58 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>0.0\s(I) _refine_ls_number_reflns 3541 _refine_ls_number_restraints 7 _refine_ls_number_parameters 241 _oxford_refine_ls_R_factor_ref 0.0719 _refine_ls_wR_factor_ref 0.1056 _refine_ls_goodness_of_fit_ref 0.9714 _refine_ls_shift/su_max 0.0032642 _refine_ls_shift/su_mean 0.0000668 # The values computed with all filters except I/sigma _oxford_reflns_number_all 3541 _refine_ls_R_factor_all 0.0719 _refine_ls_wR_factor_all 0.1056 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2478 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_gt 0.0817 _refine_ls_abs_structure_Flack 0.68(18) _refine_ls_abs_structure_details 'Flack (1983), 1762 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _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: 22.8 37.8 23.7 10.4 2.49 ; # Insert your own references if required - in alphabetical order 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens F1 F 0.24895(13) 0.54734(13) 0.04013(13) 0.0601 1.0000 Uani . . . . . . F2 F 0.24053(15) 0.38181(13) 0.00392(14) 0.0687 1.0000 Uani . . . . . . F3 F 0.32323(15) 0.30784(13) 0.10701(16) 0.0707 1.0000 Uani . . . . . . F4 F 0.42204(16) 0.40864(14) 0.24538(15) 0.0694 1.0000 Uani . . . . . . F5 F 0.30573(14) 0.47383(16) 0.37781(14) 0.0715 1.0000 Uani . . . . . . F6 F 0.4006(2) 0.5527(2) 0.52280(15) 0.0908 1.0000 Uani . . . . . . F7 F 0.58613(18) 0.69938(18) 0.51853(16) 0.0877 1.0000 Uani . . . . . . F8 F 0.67538(15) 0.76581(17) 0.36686(17) 0.0850 1.0000 Uani . . . . . . F9 F 0.57952(14) 0.69071(14) 0.22192(14) 0.0679 1.0000 Uani . . . . . . C1 C 0.3387(2) 0.5706(2) 0.1672(2) 0.0472 1.0000 Uani . . . . . . C2 C 0.2926(2) 0.5161(2) 0.0959(2) 0.0504 1.0000 Uani . . . . . . C3 C 0.2879(2) 0.4303(2) 0.0742(2) 0.0536 1.0000 Uani . . . . . . C4 C 0.3310(2) 0.3938(2) 0.1252(2) 0.0556 1.0000 Uani . . . . . . C5 C 0.3788(2) 0.4447(2) 0.1957(2) 0.0545 1.0000 Uani . . . . . . C6 C 0.3852(2) 0.5322(2) 0.2172(2) 0.0491 1.0000 Uani . . . . . . C7 C 0.4398(2) 0.5790(2) 0.2959(2) 0.0489 1.0000 Uani . . . . . . C8 C 0.3979(2) 0.5461(2) 0.3742(2) 0.0565 1.0000 Uani . . . . . . C9 C 0.4450(3) 0.5849(3) 0.4480(2) 0.0629 1.0000 Uani . . . . . . C10 C 0.5389(3) 0.6591(3) 0.4456(3) 0.0653 1.0000 Uani . . . . . . C11 C 0.5845(2) 0.6927(2) 0.3696(3) 0.0624 1.0000 Uani . . . . . . C12 C 0.5339(2) 0.6531(2) 0.2959(2) 0.0540 1.0000 Uani . . . . . . C13 C 0.2073(3) 0.5718(3) -0.1944(3) 0.0659 1.0000 Uani . . . . . . C14 C 0.1837(3) 0.5823(3) -0.2873(3) 0.0809 1.0000 Uani . . . . . . C15 C 0.1389(2) 0.5836(3) -0.1331(3) 0.0724 1.0000 Uani . . . . . . C16 C 0.1925(3) 0.4703(3) -0.1814(3) 0.0818 1.0000 Uani . . . . . . B1 B 0.3333 0.6667 0.1950(4) 0.0470 1.0000 Uani S T . . . . P1 P 0.333333(7) 0.666667(7) -0.16637(11) 0.0548 1.0000 Uani S T . . . . O2 O 0.333333(10) 0.666667(10) 0.28750(19) 0.0360 1.0000 Uani S T . . . . H141 H 0.2302 0.5771 -0.3254 0.1262 1.0000 Uiso R . . . . . H142 H 0.1910 0.6479 -0.2939 0.1259 1.0000 Uiso R . . . . . H143 H 0.1169 0.5324 -0.2989 0.1263 1.0000 Uiso R . . . . . H151 H 0.1515 0.5721 -0.0743 0.1100 1.0000 Uiso R . . . . . H152 H 0.1443 0.6466 -0.1382 0.1100 1.0000 Uiso R . . . . . H153 H 0.0723 0.5365 -0.1485 0.1102 1.0000 Uiso R . . . . . H161 H 0.2022 0.4602 -0.1219 0.1340 1.0000 Uiso R . . . . . H162 H 0.2350 0.4598 -0.2190 0.1338 1.0000 Uiso R . . . . . H163 H 0.1251 0.4227 -0.1961 0.1339 1.0000 Uiso R . . . . . H15 H 0.3333 0.6667 -0.0781 0.0298 1.0000 Uiso RS . . . . . H23 H 0.3893 0.6804 0.2841 0.0561 0.3333 Uiso 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 F1 0.0626(11) 0.0539(11) 0.0685(11) -0.0079(9) -0.0110(9) 0.0326(9) F2 0.0749(13) 0.0469(10) 0.0782(14) -0.0130(10) -0.0068(10) 0.0260(9) F3 0.0795(14) 0.0434(10) 0.0944(14) -0.0024(9) 0.0139(11) 0.0346(10) F4 0.0833(13) 0.0624(12) 0.0842(14) 0.0115(10) 0.0063(10) 0.0526(11) F5 0.0453(10) 0.0795(14) 0.0749(13) 0.0194(10) 0.0057(9) 0.0202(10) F6 0.0886(16) 0.1043(18) 0.0654(14) 0.0114(13) -0.0003(13) 0.0376(14) F7 0.0840(16) 0.0856(16) 0.0848(16) -0.0129(12) -0.0316(13) 0.0358(13) F8 0.0571(12) 0.0685(14) 0.1067(19) 0.0012(12) -0.0149(11) 0.0145(11) F9 0.0512(10) 0.0614(12) 0.0837(14) 0.0092(10) 0.0135(10) 0.0226(9) C1 0.0413(15) 0.0402(15) 0.0579(18) 0.0023(13) 0.0044(13) 0.0186(13) C2 0.0450(16) 0.0412(15) 0.0660(18) -0.0007(14) 0.0009(14) 0.0222(13) C3 0.0486(17) 0.0384(15) 0.064(2) -0.0025(14) 0.0045(15) 0.0147(13) C4 0.0565(18) 0.0373(15) 0.073(2) 0.0039(15) 0.0139(16) 0.0234(14) C5 0.0516(17) 0.0477(16) 0.071(2) 0.0106(15) 0.0095(16) 0.0299(14) C6 0.0423(16) 0.0438(16) 0.063(2) 0.0040(14) 0.0055(13) 0.0229(13) C7 0.0430(15) 0.0464(16) 0.0619(19) 0.0020(13) 0.0018(14) 0.0257(14) C8 0.0427(17) 0.0552(18) 0.071(2) 0.0101(16) 0.0012(16) 0.0238(15) C9 0.062(2) 0.068(2) 0.064(2) 0.0115(18) 0.0026(19) 0.0361(18) C10 0.062(2) 0.0621(19) 0.076(2) -0.0054(18) -0.0163(19) 0.0348(18) C11 0.0451(17) 0.0471(18) 0.090(3) 0.0007(17) -0.0042(18) 0.0192(15) C12 0.0489(17) 0.0496(17) 0.066(2) 0.0085(15) 0.0076(16) 0.0264(15) C13 0.057(2) 0.0538(19) 0.082(2) 0.0086(17) -0.0086(18) 0.0238(16) C14 0.072(3) 0.084(3) 0.086(3) -0.004(2) -0.022(2) 0.038(2) C15 0.0451(18) 0.071(2) 0.093(3) 0.018(2) 0.0044(18) 0.0228(17) C16 0.068(2) 0.054(2) 0.110(3) -0.001(2) -0.026(2) 0.0210(19) B1 0.0405(18) 0.0405(18) 0.060(4) 0.0000 0.0000 0.0202(9) P1 0.0478(5) 0.0478(5) 0.0688(9) 0.0000 0.0000 0.0239(2) O2 0.0314(9) 0.0314(9) 0.0453(18) 0.0000 0.0000 0.0157(5) _refine_ls_extinction_coef 340(60) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.17706(19) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag F1 . C2 . 1.366(4) yes F2 . C3 . 1.351(4) yes F3 . C4 . 1.349(4) yes F4 . C5 . 1.353(4) yes F5 . C8 . 1.346(4) yes F6 . C9 . 1.343(4) yes F7 . C10 . 1.354(4) yes F8 . C11 . 1.336(4) yes F9 . C12 . 1.350(4) yes C1 . C2 . 1.391(5) yes C1 . C6 . 1.420(4) yes C1 . B1 . 1.642(3) yes C2 . C3 . 1.381(4) yes C3 . C4 . 1.369(5) yes C4 . C5 . 1.367(5) yes C5 . C6 . 1.394(4) yes C6 . C7 . 1.490(5) yes C7 . C8 . 1.382(5) yes C7 . C12 . 1.376(4) yes C8 . C9 . 1.359(5) yes C9 . C10 . 1.374(5) yes C10 . C11 . 1.368(6) yes C11 . C12 . 1.380(5) yes C13 . C14 . 1.548(6) yes C13 . C15 . 1.542(6) yes C13 . C16 . 1.535(5) yes C13 . P1 . 1.874(4) yes C14 . H141 . 0.993 no C14 . H142 . 1.003 no C14 . H143 . 0.980 no C15 . H151 . 0.989 no C15 . H152 . 0.972 no C15 . H153 . 0.980 no C16 . H161 . 0.981 no C16 . H162 . 0.979 no C16 . H163 . 0.988 no B1 . O2 . 1.463(7) yes P1 . H15 . 1.396 no O2 . H23 7_565 0.811 no O2 . H23 4_665 0.811 no O2 . H23 . 0.811 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . C1 . C6 . 114.1(3) yes C2 . C1 . B1 . 123.0(3) yes C6 . C1 . B1 . 122.7(3) yes F1 . C2 . C1 . 120.1(2) yes F1 . C2 . C3 . 114.9(3) yes C1 . C2 . C3 . 125.0(3) yes F2 . C3 . C2 . 120.8(3) yes F2 . C3 . C4 . 119.9(3) yes C2 . C3 . C4 . 119.4(3) yes F3 . C4 . C3 . 120.0(3) yes F3 . C4 . C5 . 121.5(3) yes C3 . C4 . C5 . 118.5(3) yes F4 . C5 . C4 . 118.2(3) yes F4 . C5 . C6 . 119.4(3) yes C4 . C5 . C6 . 122.4(3) yes C1 . C6 . C5 . 120.6(3) yes C1 . C6 . C7 . 123.3(3) yes C5 . C6 . C7 . 116.1(3) yes C6 . C7 . C8 . 120.5(3) yes C6 . C7 . C12 . 123.2(3) yes C8 . C7 . C12 . 116.2(3) yes F5 . C8 . C7 . 118.7(3) yes F5 . C8 . C9 . 118.4(3) yes C7 . C8 . C9 . 122.9(3) yes F6 . C9 . C8 . 121.0(3) yes F6 . C9 . C10 . 119.8(3) yes C8 . C9 . C10 . 119.2(3) yes F7 . C10 . C9 . 119.8(4) yes F7 . C10 . C11 . 120.0(3) yes C9 . C10 . C11 . 120.2(3) yes F8 . C11 . C10 . 120.4(3) yes F8 . C11 . C12 . 120.4(3) yes C10 . C11 . C12 . 119.1(3) yes F9 . C12 . C11 . 117.8(3) yes F9 . C12 . C7 . 120.0(3) yes C11 . C12 . C7 . 122.3(3) yes C14 . C13 . C15 . 111.0(3) yes C14 . C13 . C16 . 109.0(3) yes C15 . C13 . C16 . 107.5(3) yes C14 . C13 . P1 . 111.1(3) yes C15 . C13 . P1 . 107.2(3) yes C16 . C13 . P1 . 111.1(3) yes C13 . C14 . H141 . 109.5 no C13 . C14 . H142 . 107.7 no H141 . C14 . H142 . 109.0 no C13 . C14 . H143 . 108.3 no H141 . C14 . H143 . 112.2 no H142 . C14 . H143 . 110.0 no C13 . C15 . H151 . 110.2 no C13 . C15 . H152 . 112.0 no H151 . C15 . H152 . 110.5 no C13 . C15 . H153 . 108.4 no H151 . C15 . H153 . 109.6 no H152 . C15 . H153 . 106.0 no C13 . C16 . H161 . 110.5 no C13 . C16 . H162 . 110.3 no H161 . C16 . H162 . 111.9 no C13 . C16 . H163 . 108.3 no H161 . C16 . H163 . 107.6 no H162 . C16 . H163 . 108.0 no C1 . B1 . C1 7_565 113.10(19) yes C1 . B1 . C1 4_665 113.10(19) yes C1 7_565 B1 . C1 4_665 113.10(19) yes C1 . B1 . O2 . 105.5(2) yes C1 7_565 B1 . O2 . 105.5(2) yes C1 4_665 B1 . O2 . 105.5(2) yes C13 . P1 . C13 4_665 114.58(10) yes C13 . P1 . C13 7_565 114.58(10) yes C13 4_665 P1 . C13 7_565 114.58(10) yes C13 . P1 . H15 . 103.7 no C13 4_665 P1 . H15 . 103.7 no C13 7_565 P1 . H15 . 103.7 no B1 . O2 . H23 7_565 86.2 no B1 . O2 . H23 4_665 86.2 no H23 7_565 O2 . H23 4_665 119.6 no B1 . O2 . H23 . 86.2 no H23 7_565 O2 . H23 . 119.6 no H23 4_665 O2 . H23 . 119.6 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C15 . H152 . C16 7_565 133.13(14) 0.972 2.483 3.227(5) yes O2 . H23 . C7 . 124.79(8) 0.811 2.152 2.698(5) yes O2 . H23 . C12 . 156.54(7) 0.811 2.569 3.328(5) yes _iucr_refine_instruction_details_constraints ; # # Punched on 25/09/12 at 15:13:58 # #LIST 12 BLOCK SCALE X'S, U'S CONT EXTPARAM CONT ENANTIO RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) H ( 143,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) H ( 153,X'S) RIDE C ( 16,X'S) H ( 161,X'S) H ( 162,X'S) H ( 163,X'S) RIDE P ( 1,X'S) H ( 15,X'S) RIDE O ( 2,X'S) H ( 23,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 25/09/12 at 15:13:58 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ;