#------------------------------------------------------------------------------ #$Date: 2009-11-16 02:43:51 +0100 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003064.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_2003064 _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-iodophenyl)methyleneamino-2,2,6,6-tetramethylpiperidin-1-oxyl ; _chemical_name_common I-TEMPO(a) _chemical_formula_sum 'C16 H22 I N2 O' _chemical_formula_weight 385.27 _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 5.889(4) _cell_length_b 25.851(3) _cell_length_c 11.322(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.27(3) _cell_angle_gamma 90.00 _cell_volume 1662.7(13) _cell_formula_units_Z 4 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 12.7 _cell_measurement_theta_max 16.1 _cell_measurement_temperature 293 _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.040 _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 772.00 _exptl_absorpt_coefficient_mu 1.925 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.708 _exptl_absorpt_correction_T_max 0.926 _diffrn_ambient_temperature 293 _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 4201 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measured_fraction_theta_full 0.978 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -14 _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_% -0.35 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -3 -3 0 8 0 1 0 -2 _reflns_number_total 3843 _reflns_number_gt 2469 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0945 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_number_reflns 3843 _refine_ls_number_parameters 269 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment refall _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+0.8733P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.410 _refine_diff_density_min -0.805 _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' 'I' 'I' -0.4742 1.8119 '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 I1 0.45126(7) 0.004363(10) -0.32970(2) 0.07079(13) Uani d . 1 . . I O1 -0.2183(5) 0.21731(10) 0.5145(2) 0.0585(7) Uani d . 1 . . O N1 -0.1104(5) 0.19722(10) 0.4410(2) 0.0396(6) Uani d . 1 . . N N2 0.1662(5) 0.12361(12) 0.1779(3) 0.0497(7) Uani d . 1 . . N C2 -0.0545(6) 0.23247(13) 0.3482(3) 0.0430(7) Uani d . 1 . . C C3 -0.0005(7) 0.20025(14) 0.2456(3) 0.0446(8) Uani d . 1 . . C C4 0.1610(7) 0.15434(14) 0.2874(3) 0.0436(8) Uani d . 1 . . C C5 0.0622(7) 0.12052(14) 0.3706(3) 0.0465(8) Uani d . 1 . . C C6 0.0205(6) 0.14798(13) 0.4821(3) 0.0437(8) Uani d . 1 . . C C7 0.3460(7) 0.12450(15) 0.1413(3) 0.0483(8) Uani d . 1 . . C C11 0.3692(6) 0.09610(14) 0.0320(3) 0.0448(8) Uani d . 1 . . C C12 0.2093(8) 0.05855(17) -0.0219(4) 0.0594(10) Uani d . 1 . . C C13 0.2309(8) 0.03243(18) -0.1257(4) 0.0627(11) Uani d . 1 . . C C14 0.4139(7) 0.04436(13) -0.1744(3) 0.0477(8) Uani d . 1 . . C C15 0.5738(8) 0.08174(18) -0.1235(4) 0.0603(10) Uani d . 1 . . C C16 0.5511(8) 0.10713(18) -0.0197(4) 0.0620(11) Uani d . 1 . . C C21 0.1498(10) 0.26798(18) 0.4090(4) 0.0606(11) Uani d . 1 . . C C22 -0.2755(9) 0.26510(18) 0.2949(4) 0.0619(11) Uani d . 1 . . C C61 0.2487(8) 0.1601(2) 0.5784(4) 0.0597(10) Uani d . 1 . . C C62 -0.1361(9) 0.11420(17) 0.5396(4) 0.0593(11) Uani d . 1 . . C H4 0.311(6) 0.1664(14) 0.325(3) 0.050(10) Uiso d . 1 . . H H7 0.480(7) 0.1429(17) 0.184(3) 0.068(13) Uiso d . 1 . . H H12 0.090(7) 0.0478(17) 0.015(3) 0.070(13) Uiso d . 1 . . H H13 0.134(9) 0.0048(16) -0.153(4) 0.075(15) Uiso calc . 1 . . H H15 0.700(8) 0.0923(17) -0.163(4) 0.075(13) Uiso calc . 1 . . H H16 0.653(7) 0.1296(15) 0.018(3) 0.055(11) Uiso d . 1 . . H H21 0.297(10) 0.252(2) 0.444(4) 0.093(18) Uiso calc . 1 . . H H22 0.113(8) 0.2853(17) 0.473(4) 0.073(13) Uiso d . 1 . . H H23 0.159(8) 0.2939(19) 0.348(4) 0.087(15) Uiso calc . 1 . . H H24 -0.290(7) 0.2892(17) 0.358(4) 0.072(13) Uiso calc . 1 . . H H25 -0.414(7) 0.2419(15) 0.257(3) 0.053(11) Uiso d . 1 . . H H26 -0.265(8) 0.2852(18) 0.222(4) 0.079(14) Uiso calc . 1 . . H H31 0.066(7) 0.2249(15) 0.193(3) 0.064(12) Uiso d . 1 . . H H32 -0.150(7) 0.1885(14) 0.197(3) 0.047(10) Uiso d . 1 . . H H51 0.161(6) 0.0910(14) 0.400(3) 0.050(10) Uiso d . 1 . . H H52 -0.098(7) 0.1051(14) 0.317(3) 0.053(10) Uiso d . 1 . . H H61 0.362(6) 0.1766(15) 0.550(3) 0.048(11) Uiso d . 1 . . H H62 0.309(8) 0.1289(18) 0.610(4) 0.076(14) Uiso calc . 1 . . H H63 0.220(8) 0.1847(19) 0.651(4) 0.092(16) Uiso calc . 1 . . H H64 -0.056(7) 0.0827(16) 0.557(3) 0.055(11) Uiso d . 1 . . H H65 -0.163(7) 0.1318(16) 0.608(4) 0.067(13) Uiso calc . 1 . . H H66 -0.287(8) 0.1113(16) 0.486(4) 0.063(13) 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 I1 0.1133(3) 0.05549(17) 0.05413(17) 0.00967(15) 0.04074(17) -0.01044(11) O1 0.0764(19) 0.0600(16) 0.0539(15) 0.0096(14) 0.0431(14) -0.0009(12) N1 0.0464(16) 0.0417(14) 0.0369(14) -0.0001(12) 0.0219(13) -0.0020(11) N2 0.0523(18) 0.0571(18) 0.0444(16) 0.0030(15) 0.0209(14) -0.0101(13) C2 0.053(2) 0.0433(17) 0.0383(16) -0.0003(16) 0.0215(15) 0.0012(13) C3 0.049(2) 0.052(2) 0.0370(16) 0.0005(17) 0.0187(16) -0.0035(14) C4 0.044(2) 0.053(2) 0.0382(17) -0.0012(16) 0.0182(15) -0.0080(14) C5 0.055(2) 0.0417(18) 0.0470(19) 0.0053(17) 0.0219(17) 0.0004(14) C6 0.050(2) 0.0431(18) 0.0430(19) 0.0014(15) 0.0209(16) 0.0016(14) C7 0.054(2) 0.050(2) 0.0455(19) 0.0025(18) 0.0199(17) -0.0053(15) C11 0.0465(19) 0.0495(19) 0.0405(18) 0.0077(16) 0.0151(15) -0.0038(14) C12 0.061(3) 0.068(3) 0.059(2) -0.009(2) 0.034(2) -0.0148(19) C13 0.069(3) 0.063(2) 0.064(3) -0.019(2) 0.032(2) -0.021(2) C14 0.064(2) 0.0438(18) 0.0399(17) 0.0100(17) 0.0226(17) -0.0028(14) C15 0.060(3) 0.077(3) 0.053(2) -0.008(2) 0.031(2) -0.013(2) C16 0.058(3) 0.078(3) 0.057(2) -0.018(2) 0.027(2) -0.026(2) C21 0.082(3) 0.054(2) 0.055(2) -0.020(2) 0.036(2) -0.0109(19) C22 0.083(3) 0.058(2) 0.053(2) 0.020(2) 0.032(2) 0.0064(19) C61 0.062(3) 0.067(3) 0.048(2) 0.001(2) 0.011(2) 0.005(2) C62 0.073(3) 0.051(2) 0.064(3) -0.001(2) 0.036(3) 0.008(2)