#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003060.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003060 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 55 _journal_year 1999 _journal_page_first 231 _journal_page_last 245 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c ' loop_ _publ_author_name ; Fujiko Iwasaki ; _chemical_name_systematic ; 4-(4-pyridyl)methyleneamino-2,2,6,6-tetramethylpiperidin-1-oxyl ; _chemical_name_common 4-Py-TEMPO _chemical_formula_sum 'C15 H22 N3 O ' _chemical_formula_weight 260.36 _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 7.977(6) _cell_length_b 20.158(7) _cell_length_c 11.383(9) _cell_angle_alpha 90 _cell_angle_beta 125.95(6) _cell_angle_gamma 90 _cell_volume 1481.0(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.3 _cell_measurement_theta_max 17.3 _cell_measurement_temperature 295 _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 1.167 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 564.00 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 295 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 3631 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measured_fraction_theta_full 0.973 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.08 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -2 -2 1 -1 -2 -1 -4 -1 _reflns_number_total 3400 _reflns_number_gt 2464 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1204 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_number_reflns 3400 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment refall _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+0.2298P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.148 _refine_diff_density_min -0.190 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol O1 0.66692(17) 0.20588(5) 0.68638(10) 0.0614(3) Uani d . 1 . . O N1 0.57579(17) 0.18079(5) 0.55966(10) 0.0426(2) Uani d . 1 . . N N2 0.32248(19) 0.08646(6) 0.15827(12) 0.0556(3) Uani d . 1 . . N N14 0.1225(2) -0.02359(7) -0.30557(13) 0.0618(3) Uani d . 1 . . N C2 0.5925(2) 0.21876(6) 0.45395(13) 0.0449(3) Uani d . 1 . . C C3 0.5402(2) 0.17283(7) 0.32952(14) 0.0486(3) Uani d . 1 . . C C4 0.3435(2) 0.13250(7) 0.26638(14) 0.0494(3) Uani d . 1 . . C C5 0.3671(3) 0.09152(7) 0.38637(17) 0.0533(3) Uani d . 1 . . C C6 0.4072(2) 0.13205(6) 0.51462(14) 0.0476(3) Uani d . 1 . . C C7 0.1824(2) 0.09644(8) 0.02753(16) 0.0546(3) Uani d . 1 . . C C11 0.1579(2) 0.05324(7) -0.08720(14) 0.0500(3) Uani d . 1 . . C C12 0.0459(2) 0.07502(8) -0.22893(16) 0.0596(4) Uani d . 1 . . C C13 0.0340(3) 0.03546(9) -0.33276(16) 0.0623(4) Uani d . 1 . . C C15 0.2279(3) -0.04471(9) -0.16901(17) 0.0645(4) Uani d . 1 . . C C16 0.2495(2) -0.00854(8) -0.05737(16) 0.0594(4) Uani d . 1 . . C C21 0.8150(3) 0.24249(10) 0.5323(2) 0.0655(4) Uani d . 1 . . C C22 0.4489(3) 0.27924(8) 0.40051(19) 0.0627(4) Uani d . 1 . . C C61 0.2127(3) 0.16838(9) 0.4769(2) 0.0613(4) Uani d . 1 . . C C62 0.4821(4) 0.08522(8) 0.6422(2) 0.0661(4) Uani d . 1 . . C H4 0.220(2) 0.1627(7) 0.2193(15) 0.051(4) Uiso d . 1 . . H H7 0.082(3) 0.1336(9) -0.0051(18) 0.076(5) Uiso d . 1 . . H H12 -0.022(3) 0.1174(9) -0.2521(19) 0.078(5) Uiso d . 1 . . H H13 -0.049(3) 0.0500(8) -0.436(2) 0.077(5) Uiso d . 1 . . H H15 0.294(3) -0.0890(10) -0.1486(19) 0.084(6) Uiso d . 1 . . H H16 0.330(3) -0.0255(8) 0.036(2) 0.073(5) Uiso d . 1 . . H H21 0.907(3) 0.2050(10) 0.574(2) 0.082(6) Uiso d . 1 . . H H22 0.831(3) 0.2648(10) 0.463(2) 0.094(6) Uiso d . 1 . . H H23 0.846(3) 0.2743(9) 0.608(2) 0.078(5) Uiso d . 1 . . H H24 0.297(3) 0.2678(10) 0.335(2) 0.085(6) Uiso d . 1 . . H H25 0.475(3) 0.3036(9) 0.482(2) 0.082(5) Uiso d . 1 . . H H26 0.478(3) 0.3088(10) 0.348(2) 0.099(7) Uiso d . 1 . . H H31 0.660(2) 0.1408(8) 0.3669(16) 0.059(4) Uiso d . 1 . . H H32 0.530(2) 0.2005(8) 0.2524(17) 0.063(4) Uiso d . 1 . . H H51 0.244(3) 0.0638(8) 0.3487(17) 0.066(5) Uiso d . 1 . . H H52 0.490(2) 0.0604(7) 0.4235(16) 0.055(4) Uiso d . 1 . . H H61 0.112(3) 0.1383(10) 0.4606(19) 0.082(6) Uiso d . 1 . . H H62 0.248(3) 0.1981(9) 0.5561(19) 0.075(5) Uiso d . 1 . . H H63 0.145(3) 0.1973(9) 0.386(2) 0.076(5) Uiso d . 1 . . H H64 0.615(3) 0.0634(10) 0.675(2) 0.089(6) Uiso d . 1 . . H H65 0.375(3) 0.0500(10) 0.611(2) 0.090(6) Uiso d . 1 . . H H66 0.511(3) 0.1101(10) 0.726(2) 0.085(6) Uiso d . 1 . . H 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 0.0810(7) 0.0637(6) 0.0419(5) -0.0090(5) 0.0375(5) -0.0116(4) N1 0.0540(6) 0.0399(5) 0.0381(5) 0.0006(4) 0.0294(5) -0.0023(4) N2 0.0587(7) 0.0626(7) 0.0485(6) -0.0005(6) 0.0332(6) -0.0140(5) N14 0.0656(8) 0.0754(9) 0.0488(7) -0.0134(7) 0.0361(6) -0.0173(6) C2 0.0550(7) 0.0429(6) 0.0400(6) -0.0044(5) 0.0297(6) -0.0001(5) C3 0.0601(8) 0.0519(7) 0.0423(7) -0.0035(6) 0.0348(6) -0.0024(6) C4 0.0516(7) 0.0529(7) 0.0450(7) 0.0010(6) 0.0290(6) -0.0111(6) C5 0.0662(9) 0.0463(7) 0.0653(9) -0.0117(7) 0.0486(8) -0.0157(6) C6 0.0621(8) 0.0416(6) 0.0556(7) -0.0041(6) 0.0438(7) -0.0066(5) C7 0.0555(8) 0.0576(8) 0.0510(8) 0.0013(7) 0.0314(7) -0.0074(6) C11 0.0479(7) 0.0574(8) 0.0447(7) -0.0061(6) 0.0272(6) -0.0097(6) C12 0.0639(9) 0.0591(9) 0.0498(8) -0.0024(7) 0.0301(7) -0.0019(7) C13 0.0665(9) 0.0752(11) 0.0428(7) -0.0142(8) 0.0308(7) -0.0050(7) C15 0.0693(10) 0.0658(10) 0.0545(8) 0.0035(8) 0.0342(8) -0.0109(7) C16 0.0629(9) 0.0661(9) 0.0417(7) 0.0036(7) 0.0266(7) -0.0041(6) C21 0.0656(10) 0.0730(11) 0.0593(9) -0.0208(9) 0.0374(8) -0.0073(8) C22 0.0844(12) 0.0420(7) 0.0576(9) 0.0055(7) 0.0395(9) 0.0052(7) C61 0.0641(9) 0.0651(9) 0.0730(10) -0.0033(8) 0.0505(9) -0.0136(8) C62 0.1050(14) 0.0474(8) 0.0774(11) 0.0006(9) 0.0711(11) 0.0036(8)