data_12507 _audit_creation_date "12-09-05" _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title 'p21m in P2(1)/m' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.0250(4) _cell_length_b 9.9052(5) _cell_length_c 8.9614(4) _cell_angle_alpha 90 _cell_angle_beta 92.4100(10) _cell_angle_gamma 90 _cell_volume 711.70(6) _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 1 21/m 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-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' 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' 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' _cell_formula_units_Z 2 # Given Formula = C15 H15 N1 O3 # Dc = 1.20 Fooo = 288.00 Mu = 0.84 M = 128.64 # Found Formula = C15 H23 N1 O3 # Dc = 1.24 FOOO = 288.00 Mu = 0.85 M = 132.68 _chemical_formula_sum 'C15 H23 N1 O3' _chemical_formula_moiety 'C15 H23 N1 O3' _chemical_compound_source ? _chemical_formula_weight 265.35 _cell_measurement_reflns_used 9988 _cell_measurement_theta_min 3 _cell_measurement_theta_max 24 _cell_measurement_temperature 150 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_min 0.045 _exptl_crystal_size_mid 0.107 _exptl_crystal_size_max 0.171 _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 288 _exptl_absorpt_coefficient_mu 0.085 # Sheldrick geometric approximatio 1.00 1.00 # No experimental values of Tmin/max available _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 1.00 _exptl_absorpt_correction_T_max 1.00 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device 'Area' _diffrn_radiation_monochromator 'diamond 111' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.41238 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _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 17465 _reflns_number_total 4827 _diffrn_reflns_av_R_equivalents 0.045 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 4827 # Theoretical number of reflections is about 11308 _diffrn_reflns_theta_min 1.320 _diffrn_reflns_theta_max 23.900 _diffrn_measured_fraction_theta_max 0.824 _diffrn_reflns_theta_full 17.925 _diffrn_measured_fraction_theta_full 0.945 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.47 _refine_diff_density_max 0.55 # 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 4820 _refine_ls_number_restraints 1 _refine_ls_number_parameters 155 _oxford_refine_ls_R_factor_ref 0.1017 _refine_ls_wR_factor_ref 0.2618 _refine_ls_goodness_of_fit_ref 1.0709 _refine_ls_shift/su_max 0.0066575 _refine_ls_shift/su_mean 0.0000958 # The values computed with all filters except I/sigma _oxford_reflns_number_all 4823 _refine_ls_R_factor_all 0.1060 _refine_ls_wR_factor_all 0.2912 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4392 _refine_ls_R_factor_gt 0.0963 _refine_ls_wR_factor_gt 0.2519 # 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 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= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 0.79P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. Sheldrick, G. M. (2008). Acta Cryst A64, 112-122. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 0.48655(14) 0.7500 -0.12927(15) 0.0330 1.0000 Uani S T . . . . O2 O -0.20301(19) 0.66928(19) -0.0742(2) 0.0219 0.5000 Uani . . . . . . O3 O -0.1435(2) 0.8656(2) 0.0411(3) 0.0256 0.5000 Uani . . . . . . N1 N 0.35505(14) 0.7500 -0.05400(14) 0.0184 1.0000 Uani S T . . . . C1 C 0.18810(14) 0.7500 -0.13225(15) 0.0128 1.0000 Uani S T . . . . C2 C 0.0797(2) 0.7094(2) -0.0006(2) 0.0139 0.5000 Uani . . . . . . H21 H 0.0793 0.6084 0.0001 0.0500 0.5000 Uiso R . . . . . C3 C 0.17262(19) 0.750000(10) 0.13932(19) 0.0270 1.0000 Uani S T . . . . H3411 H 0.1490 0.6859 0.2205 0.0500 0.5000 Uiso R . . . . . H341 H 0.1371 0.8412 0.1700 0.0500 0.5000 Uiso R . . . . . C4 C 0.35809(16) 0.7500 0.11078(16) 0.0153 1.0000 Uani S T . . . . C5 C 0.1929(3) 0.6527(3) -0.2612(3) 0.0241 0.5000 Uani . . . . . . H52 H 0.2942 0.6704 -0.3174 0.0500 0.5000 Uiso R . . . . . H92 H 0.2002 0.5593 -0.2224 0.0500 0.5000 Uiso R . . . . . C6 C 0.0385(4) 0.6661(5) -0.3696(5) 0.0395 0.5000 Uani . . . . . . H81 H -0.0623 0.6409 -0.3161 0.0500 0.5000 Uiso R . . . . . H73 H 0.0493 0.6025 -0.4539 0.0500 0.5000 Uiso R . . . . . C7 C 0.0190(4) 0.8058(5) -0.4295(4) 0.0427 0.5000 Uani . . . . . . H72 H 0.1162 0.8293 -0.4889 0.0500 0.5000 Uiso R . . . . . H71 H -0.0826 0.8113 -0.4959 0.0500 0.5000 Uiso R . . . . . C8 C 0.0048(3) 0.9082(4) -0.3005(4) 0.0339 0.5000 Uani . . . . . . H83 H -0.0989 0.8902 -0.2478 0.0500 0.5000 Uiso R . . . . . H82 H -0.0015 1.0013 -0.3404 0.0500 0.5000 Uiso R . . . . . C9 C 0.1535(3) 0.8972(2) -0.1909(3) 0.0210 0.5000 Uani . . . . . . H91 H 0.2538 0.9306 -0.2398 0.0500 0.5000 Uiso R . . . . . H93 H 0.1347 0.9564 -0.1041 0.0500 0.5000 Uiso R . . . . . C10 C -0.09907(16) 0.7500 -0.00925(18) 0.0184 1.0000 Uani S T . . . . C11 C 0.4678(4) 0.6403(3) 0.1790(3) 0.0226 0.5000 Uani . . . . . . H1541 H 0.4187 0.5511 0.1538 0.0500 0.5000 Uiso R . . . . . H153 H 0.5793 0.6448 0.1358 0.0500 0.5000 Uiso R . . . . . C12 C 0.4859(4) 0.6532(4) 0.3489(3) 0.0314 0.5000 Uani . . . . . . H142 H 0.5617 0.5820 0.3894 0.0500 0.5000 Uiso R . . . . . H144 H 0.3758 0.6405 0.3927 0.0500 0.5000 Uiso R . . . . . C13 C 0.5542(4) 0.7935(4) 0.3942(3) 0.0375 0.5000 Uani . . . . . . H132 H 0.5594 0.8014 0.5045 0.0500 0.5000 Uiso R . . . . . H131 H 0.6689 0.8030 0.3590 0.0500 0.5000 Uiso R . . . . . C14 C 0.4452(4) 0.9059(4) 0.3267(3) 0.0267 0.5000 Uani . . . . . . H143 H 0.4955 0.9945 0.3525 0.0500 0.5000 Uiso R . . . . . H141 H 0.3339 0.9019 0.3701 0.0500 0.5000 Uiso R . . . . . C15 C 0.4254(3) 0.8931(3) 0.1572(3) 0.0189 0.5000 Uani . . . . . . H154 H 0.3470 0.9628 0.1177 0.0500 0.5000 Uiso R . . . . . H157 H 0.5347 0.9083 0.1125 0.0500 0.5000 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 0.0079(4) 0.0740(12) 0.0173(5) 0.0000 0.0035(3) 0.0000 O2 0.0092(5) 0.0232(7) 0.0332(9) 0.0000(6) -0.0005(5) -0.0022(5) O3 0.0149(6) 0.0234(8) 0.0388(10) -0.0051(7) 0.0039(6) 0.0064(5) N1 0.0071(3) 0.0340(7) 0.0140(5) 0.0000 0.0016(3) 0.0000 C1 0.0077(4) 0.0155(5) 0.0153(5) 0.0000 0.0002(3) 0.0000 C2 0.0078(5) 0.0150(6) 0.0190(7) 0.0023(5) 0.0019(5) 0.0006(4) C3 0.0106(5) 0.0546(12) 0.0159(6) 0.0000 0.0034(4) 0.0000 C4 0.0098(4) 0.0229(6) 0.0134(5) 0.0000 0.0017(3) 0.0000 C5 0.0213(8) 0.0255(10) 0.0261(10) -0.0122(8) 0.0068(7) -0.0048(7) C6 0.0268(12) 0.064(2) 0.0277(15) -0.0214(16) 0.0019(12) -0.0154(14) C7 0.0217(10) 0.090(3) 0.0156(11) 0.0061(14) -0.0042(9) -0.0023(13) C8 0.0204(9) 0.0526(18) 0.0289(12) 0.0205(12) 0.0021(9) 0.0111(11) C9 0.0174(7) 0.0193(8) 0.0266(10) 0.0071(7) 0.0046(7) 0.0033(6) C10 0.0086(4) 0.0255(6) 0.0215(6) 0.0000 0.0029(4) 0.0000 C11 0.0202(11) 0.0264(13) 0.0214(11) 0.0040(9) 0.0027(9) 0.0070(9) C12 0.0285(13) 0.0485(19) 0.0173(11) 0.0095(12) 0.0012(9) 0.0118(13) C13 0.0241(10) 0.072(3) 0.0158(9) -0.0025(10) -0.0039(8) 0.0036(12) C14 0.0203(9) 0.0400(15) 0.0197(10) -0.0079(10) 0.0012(8) -0.0046(10) C15 0.0145(9) 0.0243(11) 0.0180(9) -0.0018(8) 0.0016(7) -0.0021(7) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 1.71(2) 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 . N1 . 1.2761(16) yes O2 . O2 4_565 1.599(4) yes O2 . O3 4_565 1.172(3) yes O2 . C10 . 1.278(2) yes O3 . C10 . 1.287(2) yes N1 . C1 . 1.4858(17) yes N1 . C4 . 1.4758(19) yes C1 . C2 4_565 1.548(2) yes C1 . C9 4_565 1.571(2) yes C1 . C5 4_565 1.506(2) yes C1 . C2 . 1.548(2) yes C1 . C5 . 1.506(2) yes C1 . C9 . 1.571(2) yes C2 . C2 4_565 0.804(4) yes C2 . H21 . 1.000 no C2 . C3 . 1.487(3) yes C2 . C10 . 1.489(2) yes C3 . H341 4_565 0.990 no C3 . H3411 4_565 0.990 no C3 . H3411 . 0.990 no C3 . H341 . 0.990 no C3 . C4 . 1.5208(19) yes H3411 . H341 4_565 0.532 no C4 . C15 4_565 1.567(3) yes C4 . C11 4_565 1.512(3) yes C4 . C11 . 1.512(3) yes C4 . C15 . 1.567(3) yes C5 . C8 4_565 1.650(4) yes C5 . H91 4_565 0.975 no C5 . C9 4_565 0.871(4) yes C5 . H52 . 0.990 no C5 . H92 . 0.990 no C5 . C6 . 1.547(5) yes H92 . H91 4_565 0.474 no H92 . C9 4_565 0.644 no C6 . C6 4_565 1.663(10) yes C6 . H72 4_565 1.261 no C6 . C8 4_565 1.006(6) yes C6 . H81 . 0.990 no C6 . H73 . 0.990 no C6 . C7 . 1.490(6) yes H81 . H83 4_565 0.755 no H81 . C8 4_565 0.734 no H73 . C7 4_565 0.968 no C7 . C7 4_565 1.105(10) yes C7 . H72 . 0.990 no C7 . H71 . 0.990 no C7 . C8 . 1.546(6) yes C8 . H83 . 0.990 no C8 . H82 . 0.990 no C8 . C9 . 1.517(4) yes C9 . H91 . 0.990 no C9 . H93 . 0.990 no C11 . C14 4_565 1.419(4) yes C11 . H157 4_565 0.949 no C11 . H1541 . 0.990 no C11 . H153 . 0.990 no C11 . C12 . 1.529(4) yes H1541 . H154 4_565 0.663 no H1541 . C15 4_565 0.557 no H153 . H157 4_565 0.665 no H153 . C15 4_565 1.312 no C12 . C15 4_565 1.824(5) yes C12 . C13 4_565 0.852(6) yes C12 . H142 . 0.990 no C12 . H144 . 0.990 no C12 . C13 . 1.542(6) yes H142 . C14 4_565 1.078 no H142 . C13 4_565 1.235 no H144 . H141 4_565 0.570 no H144 . C14 4_565 0.948 no C13 . C13 4_565 0.862(8) yes C13 . H132 . 0.990 no C13 . H131 . 0.990 no C13 . C14 . 1.526(5) yes C14 . H143 . 0.990 no C14 . H141 . 0.990 no C14 . C15 . 1.526(4) yes C15 . H154 . 0.990 no C15 . H157 . 0.990 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 O2 4_565 O2 . O3 4_565 107.16(14) yes O2 4_565 O2 . C10 . 51.27(9) yes O3 4_565 O2 . C10 . 63.21(14) yes O2 4_565 O3 . C10 . 62.40(15) yes O1 . N1 . C1 . 119.99(12) yes O1 . N1 . C4 . 123.34(12) yes C1 . N1 . C4 . 116.67(10) yes C2 4_565 C1 . C9 4_565 113.51(12) yes C2 4_565 C1 . C5 4_565 116.87(13) yes C9 4_565 C1 . C5 4_565 110.31(17) yes C2 4_565 C1 . N1 . 99.48(11) yes C9 4_565 C1 . N1 . 107.53(10) yes C5 4_565 C1 . N1 . 108.09(12) yes C2 4_565 C1 . C2 . 30.11(15) yes C9 4_565 C1 . C2 . 85.21(12) yes C5 4_565 C1 . C2 . 141.65(13) yes N1 . C1 . C2 . 99.47(11) yes C2 4_565 C1 . C5 . 141.65(13) yes C9 4_565 C1 . C5 . 32.81(14) yes C5 4_565 C1 . C5 . 79.5(2) yes N1 . C1 . C5 . 108.09(12) yes C2 . C1 . C5 . 116.87(13) yes C2 4_565 C1 . C9 . 85.21(12) yes C9 4_565 C1 . C9 . 136.4(2) yes C5 4_565 C1 . C9 . 32.81(14) yes N1 . C1 . C9 . 107.53(10) yes C2 . C1 . C9 . 113.51(12) yes C5 . C1 . C9 . 110.31(17) yes C1 . C2 . C2 4_565 74.94(7) yes C1 . C2 . H21 . 105.5 no C2 4_565 C2 . H21 . 179.6 no C1 . C2 . C3 . 107.14(12) yes C2 4_565 C2 . C3 . 74.31(8) yes H21 . C2 . C3 . 105.5 no C1 . C2 . C10 . 117.46(14) yes C2 4_565 C2 . C10 . 74.33(8) yes H21 . C2 . C10 . 105.5 no C3 . C2 . C10 . 114.75(14) yes C2 . C3 . C2 4_565 31.38(15) yes C2 . C3 . H341 4_565 81.2 no C2 4_565 C3 . H341 4_565 109.9 no C2 . C3 . H3411 4_565 133.5 no C2 4_565 C3 . H3411 4_565 110.0 no H341 4_565 C3 . H3411 4_565 108.3 no C2 . C3 . H3411 . 110.0 no C2 4_565 C3 . H3411 . 133.5 no H341 4_565 C3 . H3411 . 31.2 no H3411 4_565 C3 . H3411 . 79.7 no C2 . C3 . H341 . 109.9 no C2 4_565 C3 . H341 . 81.2 no H341 4_565 C3 . H341 . 131.8 no H3411 4_565 C3 . H341 . 31.2 no H3411 . C3 . H341 . 108.3 no C2 . C3 . C4 . 108.52(13) yes C2 4_565 C3 . C4 . 108.52(13) yes H341 4_565 C3 . C4 . 110.0 no H3411 4_565 C3 . C4 . 110.1 no H3411 . C3 . C4 . 110.1 no H341 . C3 . C4 . 110.0 no C3 . H3411 . H341 4_565 74.4 no C3 . H341 . H3411 4_565 74.4 no C3 . C4 . C15 4_565 106.53(11) yes C3 . C4 . C11 4_565 119.32(14) yes C15 4_565 C4 . C11 4_565 110.8(2) yes C3 . C4 . N1 . 101.14(11) yes C15 4_565 C4 . N1 . 104.86(12) yes C11 4_565 C4 . N1 . 112.91(13) yes C3 . C4 . C11 . 119.32(14) yes C15 4_565 C4 . C11 . 18.87(12) yes C11 4_565 C4 . C11 . 91.9(3) yes N1 . C4 . C11 . 112.91(13) yes C3 . C4 . C15 . 106.53(11) yes C15 4_565 C4 . C15 . 129.5(2) yes C11 4_565 C4 . C15 . 18.87(12) yes N1 . C4 . C15 . 104.86(12) yes C11 . C4 . C15 . 110.8(2) yes C1 . C5 . C8 4_565 110.18(17) yes C1 . C5 . H91 4_565 114.8 no C8 4_565 C5 . H91 4_565 100.3 no C1 . C5 . C9 4_565 77.7(2) yes C8 4_565 C5 . C9 4_565 65.8(3) yes H91 4_565 C5 . C9 4_565 64.6 no C1 . C5 . H52 . 109.0 no C8 4_565 C5 . H52 . 136.0 no H91 4_565 C5 . H52 . 80.4 no C9 4_565 C5 . H52 . 143.1 no C1 . C5 . H92 . 109.4 no C8 4_565 C5 . H92 . 76.9 no H91 4_565 C5 . H92 . 27.9 no C9 4_565 C5 . H92 . 39.9 no H52 . C5 . H92 . 107.8 no C1 . C5 . C6 . 112.4(2) yes C8 4_565 C5 . C6 . 36.5(2) yes H91 4_565 C5 . C6 . 125.3 no C9 4_565 C5 . C6 . 101.4(3) yes H52 . C5 . C6 . 108.6 no H92 . C5 . C6 . 109.5 no C5 . H92 . H91 4_565 74.3 no C5 . H92 . C9 4_565 60.1 no H91 4_565 H92 . C9 4_565 123.8 no C5 . C6 . C6 4_565 94.9(2) yes C5 . C6 . H72 4_565 97.1 no C6 4_565 C6 . H72 4_565 87.9 no C5 . C6 . C8 4_565 77.3(4) yes C6 4_565 C6 . C8 4_565 137.0(3) yes H72 4_565 C6 . C8 4_565 134.8 no C5 . C6 . H81 . 108.9 no C6 4_565 C6 . H81 . 104.6 no H72 4_565 C6 . H81 . 149.7 no C8 4_565 C6 . H81 . 43.2 no C5 . C6 . H73 . 109.4 no C6 4_565 C6 . H73 . 129.5 no H72 4_565 C6 . H73 . 46.7 no C8 4_565 C6 . H73 . 92.3 no H81 . C6 . H73 . 108.0 no C5 . C6 . C7 . 112.0(3) yes C6 4_565 C6 . C7 . 21.80(15) yes H72 4_565 C6 . C7 . 73.0 no C8 4_565 C6 . C7 . 150.9(4) yes H81 . C6 . C7 . 109.5 no H73 . C6 . C7 . 109.1 no C6 . H81 . H83 4_565 148.1 no C6 . H81 . C8 4_565 69.6 no H83 4_565 H81 . C8 4_565 83.3 no C6 . H73 . C7 4_565 36.9 no C6 . C7 . H73 4_565 158.3 no C6 . C7 . C7 4_565 21.80(15) yes H73 4_565 C7 . C7 4_565 159.8 no C6 . C7 . H72 . 109.8 no H73 4_565 C7 . H72 . 56.4 no C7 4_565 C7 . H72 . 103.6 no C6 . C7 . H71 . 109.9 no H73 4_565 C7 . H71 . 91.2 no C7 4_565 C7 . H71 . 93.2 no H72 . C7 . H71 . 108.2 no C6 . C7 . C8 . 110.4(2) yes H73 4_565 C7 . C8 . 65.2 no C7 4_565 C7 . C8 . 131.0(2) yes H72 . C7 . C8 . 109.4 no H71 . C7 . C8 . 109.1 no C7 . H72 . C6 4_565 28.9 no C7 . C8 . C5 4_565 79.9(2) yes C7 . C8 . H81 4_565 60.0 no C5 4_565 C8 . H81 4_565 117.1 no C7 . C8 . C6 4_565 14.0(2) yes C5 4_565 C8 . C6 4_565 66.2(3) yes H81 4_565 C8 . C6 4_565 67.3 no C7 . C8 . H83 . 109.2 no C5 4_565 C8 . H83 . 127.7 no H81 4_565 C8 . H83 . 49.2 no C6 4_565 C8 . H83 . 114.5 no C7 . C8 . H82 . 110.2 no C5 4_565 C8 . H82 . 116.8 no H81 4_565 C8 . H82 . 121.4 no C6 4_565 C8 . H82 . 118.0 no H83 . C8 . H82 . 108.0 no C7 . C8 . C9 . 110.9(2) yes C5 4_565 C8 . C9 . 31.59(15) yes H81 4_565 C8 . C9 . 128.8 no C6 4_565 C8 . C9 . 97.0(3) yes H83 . C8 . C9 . 109.4 no H82 . C8 . C9 . 109.1 no C8 . H83 . H81 4_565 47.4 no C8 . C9 . C1 . 113.9(2) yes C8 . C9 . H92 4_565 97.2 no C1 . C9 . H92 4_565 132.0 no C8 . C9 . C5 4_565 82.6(3) yes C1 . C9 . C5 4_565 69.5(2) yes H92 4_565 C9 . C5 4_565 80.0 no C8 . C9 . H91 . 108.8 no C1 . C9 . H91 . 108.8 no H92 4_565 C9 . H91 . 23.5 no C5 4_565 C9 . H91 . 62.8 no C8 . C9 . H93 . 109.0 no C1 . C9 . H93 . 108.5 no H92 4_565 C9 . H93 . 93.4 no C5 4_565 C9 . H93 . 167.4 no H91 . C9 . H93 . 107.6 no C9 . H91 . C5 4_565 52.6 no C9 . H91 . H92 4_565 32.8 no C5 4_565 H91 . H92 4_565 77.8 no C2 . C10 . C2 4_565 31.33(15) yes C2 . C10 . O3 4_565 91.27(12) yes C2 4_565 C10 . O3 4_565 120.18(14) yes C2 . C10 . O3 . 120.18(14) yes C2 4_565 C10 . O3 . 91.27(12) yes O3 4_565 C10 . O3 . 125.7(2) yes C2 . C10 . O2 4_565 143.30(14) yes C2 4_565 C10 . O2 4_565 117.63(12) yes O3 4_565 C10 . O2 4_565 122.10(15) yes O3 . C10 . O2 4_565 54.39(13) yes C2 . C10 . O2 . 117.63(12) yes C2 4_565 C10 . O2 . 143.30(14) yes O3 4_565 C10 . O2 . 54.39(13) yes O3 . C10 . O2 . 122.10(15) yes O2 4_565 C10 . O2 . 77.46(19) yes C4 . C11 . C14 4_565 120.9(2) yes C4 . C11 . H157 4_565 116.5 no C14 4_565 C11 . H157 4_565 121.3 no C4 . C11 . H1541 . 109.3 no C14 4_565 C11 . H1541 . 81.9 no H157 4_565 C11 . H1541 . 68.5 no C4 . C11 . H153 . 109.3 no C14 4_565 C11 . H153 . 122.2 no H157 4_565 C11 . H153 . 40.1 no H1541 . C11 . H153 . 108.0 no C4 . C11 . C12 . 111.8(2) yes C14 4_565 C11 . C12 . 26.97(19) yes H157 4_565 C11 . C12 . 129.4 no H1541 . C11 . C12 . 108.8 no H153 . C11 . C12 . 109.6 no H154 4_565 H1541 . C11 . 128.8 no H154 4_565 H1541 . C15 4_565 108.3 no C11 . H1541 . C15 4_565 20.5 no H157 4_565 H153 . C11 . 66.6 no H157 4_565 H153 . C15 4_565 47.3 no C11 . H153 . C15 4_565 19.8 no C11 . C12 . C15 4_565 14.20(14) yes C11 . C12 . C13 4_565 124.0(4) yes C15 4_565 C12 . C13 4_565 138.2(4) yes C11 . C12 . H142 . 109.7 no C15 4_565 C12 . H142 . 107.5 no C13 4_565 C12 . H142 . 83.9 no C11 . C12 . H144 . 109.6 no C15 4_565 C12 . H144 . 97.8 no C13 4_565 C12 . H144 . 117.2 no H142 . C12 . H144 . 108.0 no C11 . C12 . C13 . 110.8(3) yes C15 4_565 C12 . C13 . 123.5(2) yes C13 4_565 C12 . C13 . 26.0(3) yes H142 . C12 . C13 . 109.8 no H144 . C12 . C13 . 108.9 no C14 4_565 H142 . C12 . 39.0 no C14 4_565 H142 . C13 4_565 82.2 no C12 . H142 . C13 4_565 43.3 no H141 4_565 H144 . C12 . 118.5 no H141 4_565 H144 . C14 4_565 77.0 no C12 . H144 . C14 4_565 42.0 no C12 . C13 . H142 4_565 155.2 no C12 . C13 . C13 4_565 25.69(16) yes H142 4_565 C13 . C13 4_565 176.5 no C12 . C13 . C12 4_565 102.6(4) yes H142 4_565 C13 . C12 4_565 52.8 no C13 4_565 C13 . C12 4_565 128.3(3) yes C12 . C13 . H132 . 109.5 no H142 4_565 C13 . H132 . 87.5 no C13 4_565 C13 . H132 . 94.5 no C12 4_565 C13 . H132 . 115.2 no C12 . C13 . H131 . 109.0 no H142 4_565 C13 . H131 . 81.2 no C13 4_565 C13 . H131 . 95.5 no C12 4_565 C13 . H131 . 112.1 no H132 . C13 . H131 . 108.1 no C12 . C13 . C14 . 111.2(2) yes H142 4_565 C13 . C14 . 44.4 no C13 4_565 C13 . C14 . 136.86(17) yes C12 4_565 C13 . C14 . 8.7(3) yes H132 . C13 . C14 . 109.7 no H131 . C13 . C14 . 109.2 no H142 4_565 C14 . C13 . 53.3 no H142 4_565 C14 . C11 4_565 112.3 no C13 . C14 . C11 4_565 92.4(3) yes H142 4_565 C14 . H144 4_565 104.3 no C13 . C14 . H144 4_565 75.0 no C11 4_565 C14 . H144 4_565 121.9 no H142 4_565 C14 . H143 . 56.1 no C13 . C14 . H143 . 109.4 no C11 4_565 C14 . H143 . 115.9 no H144 4_565 C14 . H143 . 121.9 no H142 4_565 C14 . H141 . 125.2 no C13 . C14 . H141 . 109.1 no C11 4_565 C14 . H141 . 120.5 no H144 4_565 C14 . H141 . 34.1 no H143 . C14 . H141 . 108.0 no H142 4_565 C14 . C15 . 125.4 no C13 . C14 . C15 . 111.6(3) yes C11 4_565 C14 . C15 . 19.42(14) yes H144 4_565 C14 . C15 . 122.9 no H143 . C14 . C15 . 109.3 no H141 . C14 . C15 . 109.3 no H144 4_565 H141 . C14 . 68.9 no C14 . C15 . C4 . 111.1(2) yes C14 . C15 . H153 4_565 96.3 no C4 . C15 . H153 4_565 91.1 no C14 . C15 . C12 4_565 21.71(16) yes C4 . C15 . C12 4_565 95.6(2) yes H153 4_565 C15 . C12 4_565 81.4 no C14 . C15 . H1541 4_565 88.7 no C4 . C15 . H1541 4_565 148.6 no H153 4_565 C15 . H1541 4_565 111.5 no C12 4_565 C15 . H1541 4_565 108.8 no C14 . C15 . H154 . 109.6 no C4 . C15 . H154 . 109.2 no H153 4_565 C15 . H154 . 137.4 no C12 4_565 C15 . H154 . 130.7 no H1541 4_565 C15 . H154 . 39.5 no C14 . C15 . H157 . 109.4 no C4 . C15 . H157 . 109.4 no H153 4_565 C15 . H157 . 29.6 no C12 4_565 C15 . H157 . 102.3 no H1541 4_565 C15 . H157 . 85.0 no H154 . C15 . H157 . 108.0 no H1541 4_565 H154 . C15 . 32.3 no H153 4_565 H157 . C15 . 103.1 no H153 4_565 H157 . C11 4_565 73.3 no C15 . H157 . C11 4_565 30.3 no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 N1 C1 C2 164.73(8) . . . . no O1 N1 C1 C5 42.30(12) . . . . no O1 N1 C1 C9 -76.78(12) . . . . no C4 N1 C1 C2 -15.27(8) . . . . no C4 N1 C1 C5 -137.70(12) . . . . no C4 N1 C1 C9 103.22(12) . . . . no O1 N1 C4 C3 180.00(1) . . . . no O1 N1 C4 C11 -51.32(14) . . . . no O1 N1 C4 C15 69.39(11) . . . . no C1 N1 C4 C3 0.00(1) . . . . no C1 N1 C4 C11 128.68(14) . . . . no C1 N1 C4 C15 -110.61(11) . . . . no N1 C1 C2 C3 24.66(12) . . . . no N1 C1 C2 C10 155.50(12) . . . . no C5 C1 C2 C3 140.59(15) . . . . no C5 C1 C2 C10 -88.57(18) . . . . no C9 C1 C2 C3 -89.28(16) . . . . no C9 C1 C2 C10 41.57(19) . . . . no N1 C1 C5 C6 -168.2(2) . . . . no C2 C1 C5 C6 80.8(3) . . . . no C9 C1 C5 C6 -50.9(3) . . . . no N1 C1 C9 C8 167.98(19) . . . . no C2 C1 C9 C8 -83.0(2) . . . . no C5 C1 C9 C8 50.3(2) . . . . no C1 C2 C3 C4 -27.05(13) . . . . no C10 C2 C3 C4 -159.39(10) . . . . no C1 C2 C10 O2 88.43(18) . . . . no C1 C2 C10 O3 -88.3(2) . . . . no C3 C2 C10 O2 -144.33(16) . . . . no C3 C2 C10 O3 39.0(2) . . . . no C2 C3 C4 N1 16.57(8) . . . . no C2 C3 C4 C11 -107.89(18) . . . . no C2 C3 C4 C15 125.91(14) . . . . no N1 C4 C11 C12 173.0(2) . . . . no C3 C4 C11 C12 -68.5(3) . . . . no C15 C4 C11 C12 55.7(3) . . . . no N1 C4 C15 C14 -176.76(18) . . . . no C3 C4 C15 C14 76.6(2) . . . . no C11 C4 C15 C14 -54.6(3) . . . . no C1 C5 C6 C7 57.0(4) . . . . no C5 C6 C7 C8 -57.9(4) . . . . no C6 C7 C8 C9 55.8(3) . . . . no C7 C8 C9 C1 -52.4(3) . . . . no C4 C11 C12 C13 -56.5(3) . . . . no C11 C12 C13 C14 55.7(3) . . . . no C12 C13 C14 C15 -55.5(3) . . . . no C13 C14 C15 C4 54.7(3) . . . . no _iucr_refine_instruction_details_constraints ; # # Punched on 05/09/12 at 11:33:24 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 341,X'S) H (3411,X'S) RIDE C ( 5,X'S) H ( 52,X'S) H ( 92,X'S) RIDE C ( 6,X'S) H ( 81,X'S) H ( 73,X'S) RIDE C ( 7,X'S) H ( 72,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 83,X'S) H ( 82,X'S) RIDE C ( 9,X'S) H ( 91,X'S) H ( 93,X'S) RIDE C ( 11,X'S) H ( 153,X'S) H (1541,X'S) RIDE C ( 12,X'S) H ( 142,X'S) H ( 144,X'S) RIDE C ( 13,X'S) H ( 132,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 143,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 154,X'S) H ( 157,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 05/09/12 at 11:33:24 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # start Validation Reply Form _vrf_PLAT770_12507 ; PROBLEM: Suspect C-H bond in CIF RESPONSE: Problematics pair belong to different "parts" of a disorder. These are not bonds. ; _vrf_PLAT022_12507 ; PROBLEM: Ratio Unique / Expected Reflections (too) Low RESPONSE: Crystal did not diffract well into high angle regions despite using synchrotron radiation. ;