# Electronic Supplementary Material (ESI) for Chemical Communications # 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_RS53 _database_code_depnum_ccdc_archive 'CCDC 873486' #TrackingRef '10370_web_deposit_cif_file_0_SamThompson_1332840830.rs53.cif' _chemical_name_systematic ; 4-methyl-3-(3-nitrophenyl)-1-phenylimidazolidin-2-one ; _chemical_melting_point 436 _cell_length_a 7.57570(10) _cell_length_b 11.7655(2) _cell_length_c 30.9842(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2761.68(7) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_space_group_name_Hall '-P 2ac 2ab ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 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' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 # Given Formula = C14 H13.12 N2.62 O2.62 # Dc = 1.25 Fooo = 1248.00 Mu = 0.89 M = 260.15 # Found Formula = C16 H15 N3 O3 # Dc = 1.43 FOOO = 1248.00 Mu = 1.01 M = 297.31 _chemical_formula_sum 'C16 H15 N3 O3' _chemical_formula_moiety 'C16 H15 N3 O3' _chemical_compound_source ? _chemical_formula_weight 297.31 _cell_measurement_reflns_used 3039 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.101 # Sheldrick geometric approximatio 0.98 0.98 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.98 _exptl_absorpt_correction_T_max 0.98 # 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 11854 _reflns_number_total 3074 _diffrn_reflns_av_R_equivalents 0.027 # Number of reflections without Friedels Law is 5098 # Number of reflections with Friedels Law is 3074 # Theoretical number of reflections is about 3164 _diffrn_reflns_theta_min 5.611 _diffrn_reflns_theta_max 27.477 _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.279 _diffrn_measured_fraction_theta_full 0.973 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 40 _reflns_limit_h_min 0 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 40 _oxford_diffrn_Wilson_B_factor 2.21 _oxford_diffrn_Wilson_scale 1.82 _atom_sites_solution_primary Direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.28 _refine_diff_density_max 0.24 # 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>3.0\s(I) _refine_ls_number_reflns 2295 _refine_ls_number_restraints 0 _refine_ls_number_parameters 199 _oxford_refine_ls_R_factor_ref 0.0484 _refine_ls_wR_factor_ref 0.0480 _refine_ls_goodness_of_fit_ref 1.0864 _refine_ls_shift/su_max 0.0005713 _refine_ls_shift/su_mean 0.0000451 # The values computed from all data _oxford_reflns_number_all 3074 _refine_ls_R_factor_all 0.0703 _refine_ls_wR_factor_all 0.0639 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2477 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_gt 0.0504 # 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 . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, 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: 1.58 0.242 1.45 0.490E-01 0.421 ; # 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 O1 O 0.37519(19) 0.60511(10) 0.67669(4) 0.0320 1.0000 Uani . . . . . . O2 O 0.1870(2) 0.55317(11) 0.44913(4) 0.0387 1.0000 Uani . . . . . . O3 O 0.12525(19) 0.40017(11) 0.48479(4) 0.0342 1.0000 Uani . . . . . . N1 N 0.3777(2) 0.41793(12) 0.70081(4) 0.0252 1.0000 Uani . . . . . . N2 N 0.4020(2) 0.45113(11) 0.63029(4) 0.0252 1.0000 Uani . . . . . . N3 N 0.1939(2) 0.49454(12) 0.48195(5) 0.0277 1.0000 Uani . . . . . . C1 C 0.3131(2) 0.53328(15) 0.76488(6) 0.0295 1.0000 Uani . . . . . . C2 C 0.3120(3) 0.54418(16) 0.80942(6) 0.0335 1.0000 Uani . . . . . . C3 C 0.3712(3) 0.45732(17) 0.83587(6) 0.0343 1.0000 Uani . . . . . . C4 C 0.4301(3) 0.35736(16) 0.81709(6) 0.0328 1.0000 Uani . . . . . . C5 C 0.4330(2) 0.34457(15) 0.77262(6) 0.0284 1.0000 Uani . . . . . . C6 C 0.3754(2) 0.43336(14) 0.74606(5) 0.0240 1.0000 Uani . . . . . . C7 C 0.3838(2) 0.50259(14) 0.67058(5) 0.0246 1.0000 Uani . . . . . . C8 C 0.4141(3) 0.30769(14) 0.68115(5) 0.0275 1.0000 Uani . . . . . . C9 C 0.3749(3) 0.32780(14) 0.63321(5) 0.0266 1.0000 Uani . . . . . . C10 C 0.4922(3) 0.25822(15) 0.60402(6) 0.0356 1.0000 Uani . . . . . . C11 C 0.3914(2) 0.51395(14) 0.59182(5) 0.0240 1.0000 Uani . . . . . . C12 C 0.4822(2) 0.61702(14) 0.58799(6) 0.0275 1.0000 Uani . . . . . . C13 C 0.4712(3) 0.68109(14) 0.55062(6) 0.0298 1.0000 Uani . . . . . . C14 C 0.3739(3) 0.64236(14) 0.51556(6) 0.0282 1.0000 Uani . . . . . . C15 C 0.2904(2) 0.53879(14) 0.51943(5) 0.0248 1.0000 Uani . . . . . . C16 C 0.2940(2) 0.47376(14) 0.55679(5) 0.0244 1.0000 Uani . . . . . . H11 H 0.2721 0.5936 0.7471 0.0356 1.0000 Uiso R . . . . . H21 H 0.2690 0.6124 0.8220 0.0396 1.0000 Uiso R . . . . . H31 H 0.3725 0.4664 0.8663 0.0409 1.0000 Uiso R . . . . . H41 H 0.4681 0.2965 0.8349 0.0393 1.0000 Uiso R . . . . . H51 H 0.4747 0.2760 0.7601 0.0346 1.0000 Uiso R . . . . . H81 H 0.5341 0.2867 0.6851 0.0342 1.0000 Uiso R . . . . . H82 H 0.3398 0.2505 0.6929 0.0342 1.0000 Uiso R . . . . . H91 H 0.2549 0.3102 0.6275 0.0325 1.0000 Uiso R . . . . . H101 H 0.4675 0.1796 0.6074 0.0421 1.0000 Uiso R . . . . . H102 H 0.6120 0.2724 0.6113 0.0421 1.0000 Uiso R . . . . . H103 H 0.4720 0.2797 0.5749 0.0421 1.0000 Uiso R . . . . . H121 H 0.5521 0.6431 0.6114 0.0327 1.0000 Uiso R . . . . . H131 H 0.5315 0.7517 0.5488 0.0351 1.0000 Uiso R . . . . . H141 H 0.3642 0.6858 0.4898 0.0344 1.0000 Uiso R . . . . . H161 H 0.2306 0.4043 0.5586 0.0288 1.0000 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 O1 0.0469(8) 0.0207(6) 0.0283(6) -0.0001(5) 0.0026(6) 0.0029(6) O2 0.0548(9) 0.0387(7) 0.0227(7) 0.0069(5) -0.0023(6) 0.0030(6) O3 0.0432(8) 0.0285(7) 0.0309(7) -0.0011(5) -0.0052(6) -0.0012(6) N1 0.0320(8) 0.0222(7) 0.0214(7) 0.0008(5) -0.0009(6) 0.0000(6) N2 0.0347(8) 0.0193(6) 0.0217(7) 0.0015(5) -0.0003(6) -0.0011(6) N3 0.0334(8) 0.0269(7) 0.0229(7) 0.0004(5) 0.0014(6) 0.0057(6) C1 0.0327(9) 0.0296(9) 0.0261(8) 0.0015(7) 0.0019(7) 0.0008(7) C2 0.0378(10) 0.0342(9) 0.0285(9) -0.0051(7) 0.0077(8) -0.0019(8) C3 0.0399(10) 0.0428(10) 0.0202(8) -0.0007(7) 0.0012(7) -0.0089(9) C4 0.0361(10) 0.0364(9) 0.0259(9) 0.0048(7) -0.0036(7) -0.0056(8) C5 0.0306(9) 0.0283(9) 0.0265(9) 0.0022(7) -0.0023(7) -0.0016(7) C6 0.0223(8) 0.0276(8) 0.0221(8) 0.0008(6) -0.0002(6) -0.0040(7) C7 0.0276(9) 0.0231(8) 0.0230(8) 0.0009(6) -0.0013(7) 0.0008(7) C8 0.0387(10) 0.0197(7) 0.0240(8) 0.0014(6) -0.0009(7) -0.0012(7) C9 0.0357(9) 0.0207(8) 0.0235(8) 0.0002(6) -0.0001(7) -0.0030(7) C10 0.0531(12) 0.0262(8) 0.0274(9) 0.0004(7) 0.0046(8) 0.0053(9) C11 0.0272(8) 0.0226(8) 0.0223(8) 0.0020(6) 0.0022(6) 0.0038(7) C12 0.0322(9) 0.0248(8) 0.0255(8) -0.0006(6) 0.0005(7) -0.0030(7) C13 0.0365(10) 0.0228(8) 0.0301(9) 0.0022(6) 0.0066(8) -0.0037(7) C14 0.0358(9) 0.0246(8) 0.0243(8) 0.0038(6) 0.0046(7) 0.0050(7) C15 0.0287(9) 0.0247(8) 0.0209(8) -0.0009(6) 0.0017(6) 0.0048(7) C16 0.0276(9) 0.0218(7) 0.0238(8) 0.0008(6) 0.0022(6) 0.0014(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.7149(16) 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 O1 . C7 . 1.223(2) yes O2 . N3 . 1.2299(19) yes O3 . N3 . 1.2291(19) yes N1 . C6 . 1.414(2) yes N1 . C7 . 1.368(2) yes N1 . C8 . 1.459(2) yes N2 . C7 . 1.394(2) yes N2 . C9 . 1.468(2) yes N2 . C11 . 1.405(2) yes N3 . C15 . 1.468(2) yes C1 . C2 . 1.386(3) yes C1 . C6 . 1.395(2) yes C1 . H11 . 0.950 no C2 . C3 . 1.385(3) yes C2 . H21 . 0.950 no C3 . C4 . 1.386(3) yes C3 . H31 . 0.950 no C4 . C5 . 1.386(2) yes C4 . H41 . 0.950 no C5 . C6 . 1.400(2) yes C5 . H51 . 0.950 no C8 . C9 . 1.533(2) yes C8 . H81 . 0.950 no C8 . H82 . 0.950 no C9 . C10 . 1.509(2) yes C9 . H91 . 0.950 no C10 . H101 . 0.950 no C10 . H102 . 0.950 no C10 . H103 . 0.950 no C11 . C12 . 1.399(2) yes C11 . C16 . 1.395(2) yes C12 . C13 . 1.384(2) yes C12 . H121 . 0.950 no C13 . C14 . 1.390(3) yes C13 . H131 . 0.950 no C14 . C15 . 1.378(2) yes C14 . H141 . 0.950 no C15 . C16 . 1.388(2) yes C16 . H161 . 0.950 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 C6 . N1 . C7 . 125.87(14) yes C6 . N1 . C8 . 122.04(13) yes C7 . N1 . C8 . 110.79(13) yes C7 . N2 . C9 . 111.12(13) yes C7 . N2 . C11 . 121.70(13) yes C9 . N2 . C11 . 124.35(14) yes O2 . N3 . O3 . 123.23(15) yes O2 . N3 . C15 . 118.44(14) yes O3 . N3 . C15 . 118.32(13) yes C2 . C1 . C6 . 119.75(17) yes C2 . C1 . H11 . 120.3 no C6 . C1 . H11 . 119.9 no C1 . C2 . C3 . 121.27(17) yes C1 . C2 . H21 . 119.3 no C3 . C2 . H21 . 119.4 no C2 . C3 . C4 . 118.82(17) yes C2 . C3 . H31 . 120.6 no C4 . C3 . H31 . 120.6 no C3 . C4 . C5 . 120.97(17) yes C3 . C4 . H41 . 119.6 no C5 . C4 . H41 . 119.5 no C4 . C5 . C6 . 119.89(17) yes C4 . C5 . H51 . 120.3 no C6 . C5 . H51 . 119.8 no N1 . C6 . C5 . 118.90(15) yes N1 . C6 . C1 . 121.80(15) yes C5 . C6 . C1 . 119.27(16) yes N2 . C7 . N1 . 107.46(14) yes N2 . C7 . O1 . 124.92(15) yes N1 . C7 . O1 . 127.62(15) yes N1 . C8 . C9 . 103.34(13) yes N1 . C8 . H81 . 111.0 no C9 . C8 . H81 . 110.5 no N1 . C8 . H82 . 110.9 no C9 . C8 . H82 . 111.5 no H81 . C8 . H82 . 109.5 no C8 . C9 . N2 . 100.67(13) yes C8 . C9 . C10 . 112.52(15) yes N2 . C9 . C10 . 114.64(15) yes C8 . C9 . H91 . 109.5 no N2 . C9 . H91 . 109.7 no C10 . C9 . H91 . 109.4 no C9 . C10 . H101 . 110.2 no C9 . C10 . H102 . 108.9 no H101 . C10 . H102 . 109.5 no C9 . C10 . H103 . 109.3 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N2 . C11 . C12 . 119.99(15) yes N2 . C11 . C16 . 120.79(15) yes C12 . C11 . C16 . 119.20(15) yes C11 . C12 . C13 . 120.90(16) yes C11 . C12 . H121 . 119.3 no C13 . C12 . H121 . 119.8 no C12 . C13 . C14 . 120.48(16) yes C12 . C13 . H131 . 119.8 no C14 . C13 . H131 . 119.8 no C13 . C14 . C15 . 117.73(16) yes C13 . C14 . H141 . 121.4 no C15 . C14 . H141 . 120.8 no N3 . C15 . C14 . 118.26(15) yes N3 . C15 . C16 . 118.30(15) yes C14 . C15 . C16 . 123.43(16) yes C11 . C16 . C15 . 118.19(15) yes C11 . C16 . H161 . 121.0 no C15 . C16 . H161 . 120.9 no _iucr_refine_instruction_details_constraints ; # # Punched on 03/04/11 at 12:21:34 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 1,X'S) H ( 11,X'S) RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) H ( 102,X'S) H ( 103,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 16,X'S) H ( 161,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 03/04/11 at 12:21:34 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; data_RS63 _database_code_depnum_ccdc_archive 'CCDC 873487' #TrackingRef '10371_web_deposit_cif_file_1_SamThompson_1332840830.rs63.cif' _chemical_name_systematic ; (S)-4-methyl-1-(3-((S)-5-methyl-2-oxo-3-phenylimidazolidin-1-yl)phenyl)-3 -(3-nitrophenyl)imidazolidin-2-one ; _chemical_melting_point 481 _cell_length_a 11.1653(2) _cell_length_b 5.43080(10) _cell_length_c 19.3601(4) _cell_angle_alpha 90 _cell_angle_beta 106.0293(7) _cell_angle_gamma 90 _cell_volume 1128.29(4) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21 1 ' _symmetry_space_group_name_Hall 'P 2yb ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z 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' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C30 H40 N6 O6 # Dc = 1.71 Fooo = 496.00 Mu = 1.21 M = 580.68 # Found Formula = C26 H25 N5 O4 # Dc = 1.39 FOOO = 496.00 Mu = 0.96 M = 471.52 _chemical_formula_sum 'C26 H25 N5 O4' _chemical_formula_moiety 'C26 H25 N5 O4' _chemical_compound_source ? _chemical_formula_weight 471.52 _cell_measurement_reflns_used 2782 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.100 _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 0.096 # Sheldrick geometric approximatio 0.99 0.99 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.99 _exptl_absorpt_correction_T_max 0.99 # 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 4579 _reflns_number_total 2815 _diffrn_reflns_av_R_equivalents 0.021 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 2815 # Theoretical number of reflections is about 5160 _diffrn_reflns_theta_min 5.236 _diffrn_reflns_theta_max 27.478 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.478 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -14 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 7 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _oxford_diffrn_Wilson_B_factor 2.62 _oxford_diffrn_Wilson_scale 1.69 _atom_sites_solution_primary Direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.18 _refine_diff_density_max 0.18 # 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>3.0\s(I) _refine_ls_number_reflns 2377 _refine_ls_number_restraints 1 _refine_ls_number_parameters 316 _oxford_refine_ls_R_factor_ref 0.0348 _refine_ls_wR_factor_ref 0.0366 _refine_ls_goodness_of_fit_ref 1.1200 _refine_ls_shift/su_max 0.0003750 _refine_ls_shift/su_mean 0.0000302 # The values computed from all data _oxford_reflns_number_all 2815 _refine_ls_R_factor_all 0.0444 _refine_ls_wR_factor_all 0.0441 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2495 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_gt 0.0379 # 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 unk _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, 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: 1.14 1.30 1.07 0.412 0.184 ; # 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 O1 O 0.79668(12) 0.2919(3) 0.34576(8) 0.0338 1.0000 Uani . . . . . . C2 C 0.69693(17) 0.3807(4) 0.31281(10) 0.0266 1.0000 Uani . . . . . . N3 N 0.62144(15) 0.5301(4) 0.33980(9) 0.0280 1.0000 Uani . . . . . . C4 C 0.64404(17) 0.6017(4) 0.41262(11) 0.0251 1.0000 Uani . . . . . . C5 C 0.58962(18) 0.8174(4) 0.42877(11) 0.0275 1.0000 Uani . . . . . . C6 C 0.60685(17) 0.8809(4) 0.50020(11) 0.0272 1.0000 Uani . . . . . . C7 C 0.67582(18) 0.7353(4) 0.55562(11) 0.0259 1.0000 Uani . . . . . . C8 C 0.72977(16) 0.5184(4) 0.53952(10) 0.0241 1.0000 Uani . . . . . . C9 C 0.71428(17) 0.4528(4) 0.46772(10) 0.0249 1.0000 Uani . . . . . . N10 N 0.80010(14) 0.3617(4) 0.59424(9) 0.0271 1.0000 Uani . . . . . . C11 C 0.90183(17) 0.2029(4) 0.58498(11) 0.0259 1.0000 Uani . . . . . . C12 C 0.93793(19) 0.0571(4) 0.65577(11) 0.0316 1.0000 Uani . . . . . . N13 N 0.87094(15) 0.1782(4) 0.70077(9) 0.0284 1.0000 Uani . . . . . . C14 C 0.78478(16) 0.3453(4) 0.66204(10) 0.0255 1.0000 Uani . . . . . . O15 O 0.70801(12) 0.4571(3) 0.68416(8) 0.0332 1.0000 Uani . . . . . . C16 C 0.88899(18) 0.1167(4) 0.77384(11) 0.0280 1.0000 Uani . . . . . . C17 C 0.8475(2) 0.2690(5) 0.82062(11) 0.0345 1.0000 Uani . . . . . . C18 C 0.8723(2) 0.2061(5) 0.89268(12) 0.0394 1.0000 Uani . . . . . . C19 C 0.9373(2) -0.0056(5) 0.91927(12) 0.0441 1.0000 Uani . . . . . . C20 C 0.9787(2) -0.1554(5) 0.87357(13) 0.0418 1.0000 Uani . . . . . . C21 C 0.9545(2) -0.0981(4) 0.80070(12) 0.0336 1.0000 Uani . . . . . . C22 C 1.00890(19) 0.3526(5) 0.57344(13) 0.0386 1.0000 Uani . . . . . . C23 C 0.5245(2) 0.6432(5) 0.28255(11) 0.0382 1.0000 Uani . . . . . . C24 C 0.51730(18) 0.4738(5) 0.21814(11) 0.0311 1.0000 Uani . . . . . . N25 N 0.64124(15) 0.3548(4) 0.23999(9) 0.0315 1.0000 Uani . . . . . . C26 C 0.68206(19) 0.1926(4) 0.19434(11) 0.0287 1.0000 Uani . . . . . . C27 C 0.64254(19) 0.2349(5) 0.12010(11) 0.0326 1.0000 Uani . . . . . . C28 C 0.67874(19) 0.0701(5) 0.07540(11) 0.0339 1.0000 Uani . . . . . . N29 N 0.63374(19) 0.1144(5) -0.00281(11) 0.0444 1.0000 Uani . . . . . . O30 O 0.65388(18) -0.0440(5) -0.04300(10) 0.0600 1.0000 Uani . . . . . . O31 O 0.5774(2) 0.3048(5) -0.02407(10) 0.0702 1.0000 Uani . . . . . . C32 C 0.7525(2) -0.1316(5) 0.09923(12) 0.0377 1.0000 Uani . . . . . . C33 C 0.7921(2) -0.1688(5) 0.17273(13) 0.0405 1.0000 Uani . . . . . . C34 C 0.75760(19) -0.0103(5) 0.22007(12) 0.0342 1.0000 Uani . . . . . . C35 C 0.4130(2) 0.2866(5) 0.20419(13) 0.0380 1.0000 Uani . . . . . . H51 H 0.5422 0.9197 0.3913 0.0338 1.0000 Uiso R . . . . . H61 H 0.5693 1.0268 0.5115 0.0336 1.0000 Uiso R . . . . . H71 H 0.6875 0.7829 0.6042 0.0314 1.0000 Uiso R . . . . . H91 H 0.7520 0.3069 0.4565 0.0295 1.0000 Uiso R . . . . . H111 H 0.8709 0.0946 0.5456 0.0326 1.0000 Uiso R . . . . . H121 H 0.9118 -0.1094 0.6476 0.0384 1.0000 Uiso R . . . . . H122 H 1.0253 0.0625 0.6773 0.0384 1.0000 Uiso R . . . . . H171 H 0.8027 0.4151 0.8029 0.0406 1.0000 Uiso R . . . . . H181 H 0.8448 0.3111 0.9245 0.0482 1.0000 Uiso R . . . . . H191 H 0.9514 -0.0482 0.9685 0.0563 1.0000 Uiso R . . . . . H201 H 1.0250 -0.2992 0.8919 0.0499 1.0000 Uiso R . . . . . H211 H 0.9830 -0.2026 0.7691 0.0409 1.0000 Uiso R . . . . . H221 H 1.0723 0.2448 0.5675 0.0478 1.0000 Uiso R . . . . . H222 H 0.9801 0.4514 0.5316 0.0478 1.0000 Uiso R . . . . . H223 H 1.0416 0.4556 0.6139 0.0478 1.0000 Uiso R . . . . . H231 H 0.5475 0.8058 0.2734 0.0481 1.0000 Uiso R . . . . . H232 H 0.4471 0.6471 0.2941 0.0481 1.0000 Uiso R . . . . . H241 H 0.5106 0.5697 0.1762 0.0380 1.0000 Uiso R . . . . . H271 H 0.5927 0.3740 0.1011 0.0389 1.0000 Uiso R . . . . . H321 H 0.7751 -0.2399 0.0664 0.0463 1.0000 Uiso R . . . . . H331 H 0.8452 -0.3044 0.1910 0.0492 1.0000 Uiso R . . . . . H341 H 0.7844 -0.0410 0.2703 0.0414 1.0000 Uiso R . . . . . H351 H 0.4148 0.1886 0.1638 0.0462 1.0000 Uiso R . . . . . H352 H 0.3354 0.3698 0.1948 0.0462 1.0000 Uiso R . . . . . H353 H 0.4234 0.1840 0.2452 0.0462 1.0000 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 O1 0.0253(6) 0.0437(10) 0.0304(7) -0.0045(7) 0.0044(5) 0.0080(7) C2 0.0269(9) 0.0282(11) 0.0255(9) 0.0012(8) 0.0085(7) 0.0025(9) N3 0.0291(8) 0.0325(10) 0.0231(8) 0.0037(7) 0.0085(6) 0.0095(8) C4 0.0244(9) 0.0257(10) 0.0266(10) 0.0006(8) 0.0094(7) 0.0000(8) C5 0.0278(8) 0.0240(11) 0.0320(10) 0.0031(9) 0.0100(8) 0.0017(9) C6 0.0281(9) 0.0211(10) 0.0342(10) -0.0011(8) 0.0117(8) 0.0011(8) C7 0.0265(9) 0.0252(10) 0.0263(9) -0.0034(8) 0.0080(7) -0.0025(8) C8 0.0203(8) 0.0251(10) 0.0268(9) 0.0018(8) 0.0065(7) -0.0011(8) C9 0.0227(8) 0.0236(9) 0.0294(9) 0.0003(8) 0.0089(7) 0.0004(8) N10 0.0253(7) 0.0295(9) 0.0262(8) -0.0004(8) 0.0069(6) 0.0052(8) C11 0.0233(8) 0.0275(10) 0.0269(9) -0.0044(8) 0.0070(7) 0.0028(8) C12 0.0294(9) 0.0344(12) 0.0305(10) -0.0007(9) 0.0074(8) 0.0068(9) N13 0.0293(8) 0.0297(10) 0.0266(8) 0.0030(7) 0.0083(7) 0.0051(8) C14 0.0235(8) 0.0254(10) 0.0273(9) -0.0003(9) 0.0067(7) -0.0014(9) O15 0.0301(7) 0.0415(9) 0.0309(7) 0.0030(7) 0.0131(6) 0.0087(7) C16 0.0265(9) 0.0267(10) 0.0298(10) 0.0022(9) 0.0060(8) -0.0063(9) C17 0.0361(10) 0.0342(12) 0.0314(10) -0.0002(10) 0.0064(8) -0.0033(10) C18 0.0443(12) 0.0434(14) 0.0290(11) 0.0001(10) 0.0075(9) -0.0056(11) C19 0.0490(13) 0.0494(15) 0.0288(11) 0.0066(12) 0.0023(9) -0.0116(13) C20 0.0409(11) 0.0377(13) 0.0403(12) 0.0110(11) 0.0004(9) -0.0039(11) C21 0.0337(10) 0.0305(12) 0.0342(11) 0.0040(9) 0.0054(8) -0.0029(10) C22 0.0260(9) 0.0398(13) 0.0497(13) 0.0041(12) 0.0101(9) 0.0007(10) C23 0.0417(12) 0.0441(14) 0.0279(10) 0.0060(10) 0.0082(9) 0.0189(11) C24 0.0324(9) 0.0367(12) 0.0250(9) 0.0068(10) 0.0091(7) 0.0148(10) N25 0.0305(8) 0.0394(11) 0.0245(8) 0.0015(8) 0.0072(6) 0.0123(9) C26 0.0261(9) 0.0335(11) 0.0274(10) -0.0023(9) 0.0088(7) 0.0024(9) C27 0.0302(10) 0.0388(12) 0.0295(10) 0.0021(10) 0.0095(8) 0.0056(10) C28 0.0285(9) 0.0495(15) 0.0246(10) -0.0053(10) 0.0091(8) -0.0006(11) N29 0.0386(10) 0.0682(16) 0.0291(10) -0.0049(11) 0.0136(8) 0.0005(12) O30 0.0627(11) 0.0847(16) 0.0350(9) -0.0199(11) 0.0175(8) -0.0011(13) O31 0.0862(14) 0.0930(19) 0.0321(9) 0.0118(11) 0.0175(9) 0.0395(15) C32 0.0322(10) 0.0451(13) 0.0360(11) -0.0121(11) 0.0097(9) 0.0016(11) C33 0.0350(10) 0.0383(13) 0.0447(13) -0.0057(11) 0.0052(9) 0.0119(11) C34 0.0327(10) 0.0375(13) 0.0293(10) -0.0010(10) 0.0033(8) 0.0071(10) C35 0.0355(10) 0.0440(14) 0.0382(11) 0.0101(11) 0.0164(9) 0.0097(11) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.8675(16) 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 O1 . C2 . 1.220(2) yes C2 . N3 . 1.373(3) yes C2 . N25 . 1.382(3) yes N3 . C4 . 1.416(3) yes N3 . C23 . 1.454(3) yes C4 . C5 . 1.394(3) yes C4 . C9 . 1.395(3) yes C5 . C6 . 1.386(3) yes C5 . H51 . 0.950 no C6 . C7 . 1.383(3) yes C6 . H61 . 0.950 no C7 . C8 . 1.397(3) yes C7 . H71 . 0.950 no C8 . C9 . 1.399(3) yes C8 . N10 . 1.416(3) yes C9 . H91 . 0.950 no N10 . C11 . 1.476(2) yes N10 . C14 . 1.373(2) yes C11 . C12 . 1.537(3) yes C11 . C22 . 1.512(3) yes C11 . H111 . 0.950 no C12 . N13 . 1.453(3) yes C12 . H121 . 0.950 no C12 . H122 . 0.950 no N13 . C14 . 1.383(3) yes N13 . C16 . 1.413(3) yes C14 . O15 . 1.221(2) yes C16 . C17 . 1.396(3) yes C16 . C21 . 1.399(3) yes C17 . C18 . 1.388(3) yes C17 . H171 . 0.950 no C18 . C19 . 1.381(4) yes C18 . H181 . 0.950 no C19 . C20 . 1.372(4) yes C19 . H191 . 0.950 no C20 . C21 . 1.396(3) yes C20 . H201 . 0.950 no C21 . H211 . 0.950 no C22 . H221 . 0.950 no C22 . H222 . 0.950 no C22 . H223 . 0.950 no C23 . C24 . 1.534(3) yes C23 . H231 . 0.950 no C23 . H232 . 0.950 no C24 . N25 . 1.479(2) yes C24 . C35 . 1.513(3) yes C24 . H241 . 0.950 no N25 . C26 . 1.410(3) yes C26 . C27 . 1.401(3) yes C26 . C34 . 1.394(3) yes C27 . C28 . 1.381(3) yes C27 . H271 . 0.950 no C28 . N29 . 1.477(3) yes C28 . C32 . 1.372(4) yes N29 . O30 . 1.222(3) yes N29 . O31 . 1.221(3) yes C32 . C33 . 1.383(3) yes C32 . H321 . 0.950 no C33 . C34 . 1.387(3) yes C33 . H331 . 0.950 no C34 . H341 . 0.950 no C35 . H351 . 0.950 no C35 . H352 . 0.950 no C35 . H353 . 0.950 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 O1 . C2 . N3 . 127.06(18) yes O1 . C2 . N25 . 125.58(18) yes N3 . C2 . N25 . 107.33(16) yes C2 . N3 . C4 . 125.57(16) yes C2 . N3 . C23 . 111.43(16) yes C4 . N3 . C23 . 122.23(18) yes N3 . C4 . C5 . 119.01(18) yes N3 . C4 . C9 . 120.68(19) yes C5 . C4 . C9 . 120.23(18) yes C4 . C5 . C6 . 118.94(19) yes C4 . C5 . H51 . 120.4 no C6 . C5 . H51 . 120.6 no C5 . C6 . C7 . 121.72(19) yes C5 . C6 . H61 . 119.3 no C7 . C6 . H61 . 119.0 no C6 . C7 . C8 . 119.41(18) yes C6 . C7 . H71 . 120.5 no C8 . C7 . H71 . 120.1 no C7 . C8 . C9 . 119.59(18) yes C7 . C8 . N10 . 121.63(17) yes C9 . C8 . N10 . 118.78(18) yes C8 . C9 . C4 . 120.11(19) yes C8 . C9 . H91 . 119.9 no C4 . C9 . H91 . 120.0 no C8 . N10 . C11 . 123.15(16) yes C8 . N10 . C14 . 124.39(16) yes C11 . N10 . C14 . 112.43(16) yes N10 . C11 . C12 . 102.34(15) yes N10 . C11 . C22 . 111.73(19) yes C12 . C11 . C22 . 112.67(17) yes N10 . C11 . H111 . 109.8 no C12 . C11 . H111 . 110.2 no C22 . C11 . H111 . 109.9 no C11 . C12 . N13 . 104.47(17) yes C11 . C12 . H121 . 110.4 no N13 . C12 . H121 . 110.2 no C11 . C12 . H122 . 111.1 no N13 . C12 . H122 . 111.1 no H121 . C12 . H122 . 109.5 no C12 . N13 . C14 . 111.59(16) yes C12 . N13 . C16 . 122.60(17) yes C14 . N13 . C16 . 125.70(17) yes N13 . C14 . N10 . 108.02(16) yes N13 . C14 . O15 . 125.94(18) yes N10 . C14 . O15 . 126.04(18) yes N13 . C16 . C17 . 121.88(19) yes N13 . C16 . C21 . 118.99(19) yes C17 . C16 . C21 . 119.1(2) yes C16 . C17 . C18 . 119.8(2) yes C16 . C17 . H171 . 119.8 no C18 . C17 . H171 . 120.4 no C17 . C18 . C19 . 121.2(2) yes C17 . C18 . H181 . 119.6 no C19 . C18 . H181 . 119.3 no C18 . C19 . C20 . 119.3(2) yes C18 . C19 . H191 . 120.1 no C20 . C19 . H191 . 120.6 no C19 . C20 . C21 . 120.9(2) yes C19 . C20 . H201 . 119.5 no C21 . C20 . H201 . 119.6 no C16 . C21 . C20 . 119.8(2) yes C16 . C21 . H211 . 119.5 no C20 . C21 . H211 . 120.8 no C11 . C22 . H221 . 109.4 no C11 . C22 . H222 . 109.5 no H221 . C22 . H222 . 109.5 no C11 . C22 . H223 . 109.5 no H221 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.5 no N3 . C23 . C24 . 103.15(18) yes N3 . C23 . H231 . 110.6 no C24 . C23 . H231 . 111.2 no N3 . C23 . H232 . 111.4 no C24 . C23 . H232 . 110.9 no H231 . C23 . H232 . 109.5 no C23 . C24 . N25 . 101.22(16) yes C23 . C24 . C35 . 114.40(18) yes N25 . C24 . C35 . 111.7(2) yes C23 . C24 . H241 . 109.9 no N25 . C24 . H241 . 109.3 no C35 . C24 . H241 . 109.9 no C24 . N25 . C2 . 111.67(16) yes C24 . N25 . C26 . 122.17(17) yes C2 . N25 . C26 . 124.82(17) yes N25 . C26 . C27 . 118.4(2) yes N25 . C26 . C34 . 122.58(18) yes C27 . C26 . C34 . 119.0(2) yes C26 . C27 . C28 . 118.2(2) yes C26 . C27 . H271 . 120.8 no C28 . C27 . H271 . 121.0 no C27 . C28 . N29 . 117.5(2) yes C27 . C28 . C32 . 124.0(2) yes N29 . C28 . C32 . 118.5(2) yes C28 . N29 . O30 . 117.9(2) yes C28 . N29 . O31 . 118.8(2) yes O30 . N29 . O31 . 123.4(2) yes C28 . C32 . C33 . 117.0(2) yes C28 . C32 . H321 . 121.0 no C33 . C32 . H321 . 122.0 no C32 . C33 . C34 . 121.4(2) yes C32 . C33 . H331 . 119.1 no C34 . C33 . H331 . 119.5 no C26 . C34 . C33 . 120.4(2) yes C26 . C34 . H341 . 119.5 no C33 . C34 . H341 . 120.1 no C24 . C35 . H351 . 109.5 no C24 . C35 . H352 . 109.3 no H351 . C35 . H352 . 109.5 no C24 . C35 . H353 . 109.6 no H351 . C35 . H353 . 109.5 no H352 . C35 . H353 . 109.5 no _iucr_refine_instruction_details_constraints ; # # Punched on 14/06/11 at 13:39:47 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) H ( 122,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 19,X'S) H ( 191,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) H ( 222,X'S) H ( 223,X'S) RIDE C ( 23,X'S) H ( 231,X'S) H ( 232,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) H ( 352,X'S) H ( 353,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 14/06/11 at 13:39:47 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ;