#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2002920.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_2002920 _journal_name_full 'Acta Crystallographica, Section B' _journal_year 1998 _journal_volume B54 _journal_page_first 695 _journal_page_last 704 _chemical_name_systematic ; 1,4-diaminobenzene.2 4-phenylphenol ; _chemical_name_common 'p-phenylenediamine.2 p-phenylphenol' _chemical_formula_moiety 'C6 H8 N2 , 2C12 H10 O ' _chemical_formula_sum 'C30 H28 N2 O2' _chemical_formula_weight 448.54 _chemical_melting_point .175E-174 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 26.629(5) _cell_length_b 5.4260(10) _cell_length_c 8.095(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.15(2) _cell_angle_gamma 90.00 _cell_volume 1164.9(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 37 _cell_measurement_theta_min 6.82 _cell_measurement_theta_max 12.48 _cell_measurement_temperature 295(2) _exptl_crystal_description prism _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max .40 _exptl_crystal_size_mid .24 _exptl_crystal_size_min .18 _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_meas 1.25 _exptl_crystal_density_method suspension _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 295(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method \w _diffrn_reflns_number 3081 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 9 _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 3.92 _reflns_number_total 2062 _reflns_number_observed 1401 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_obs 0.0477 _refine_ls_wR_factor_all 0.1382 _refine_ls_wR_factor_obs 0.1197 _refine_ls_goodness_of_fit_all 1.030 _refine_ls_goodness_of_fit_obs 1.102 _refine_ls_restrained_S_all 1.030 _refine_ls_restrained_S_obs 1.102 _refine_ls_number_reflns 1041 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment ;hydrogen-bond H position refined, others calc 0.98A C-H, all H iso 1.2xU~iso~ of atom attached ; _refine_ls_weighting_scheme ;w = 1/[\s^2^(Fo^2^)+(0.0640P)^2^+0.1809P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_shift/esd_max 0.004 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.188 _refine_diff_density_min -0.154 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_extinction_coef 0.016(3) 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' 'N' 'N' 0.0061 0.0033 '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' 'XTAL3.4 (Hall et al., 1995), ORTEPIII (Burnett & Johnson, 1996' 'SHELXL-93 (Sheldrick, 1993), XTAL3.4 (Hall et al., 1995)' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol O1 0.14021(5) 0.4667(3) 0.9857(2) 0.0538(5) Uani d . 1 . O H1 0.1320(8) 0.315(5) 1.028(3) 0.065 Uiso d . 1 . H C2 0.19076(7) 0.4714(4) 0.9638(2) 0.0391(5) Uani d . 1 . C C3 0.20854(7) 0.6640(4) 0.8750(3) 0.0458(5) Uani d . 1 . C H3 0.18547(7) 0.7942(4) 0.8318(3) 0.055 Uiso calc R 1 . H C4 0.25894(7) 0.6738(4) 0.8468(3) 0.0442(5) Uani d . 1 . C H4 0.27095(7) 0.8123(4) 0.7833(3) 0.053 Uiso calc R 1 . H C5 0.29318(7) 0.4936(3) 0.9055(2) 0.0348(5) Uani d . 1 . C C6 0.27409(7) 0.3057(4) 0.9972(2) 0.0446(5) Uani d . 1 . C H6 0.29706(7) 0.1766(4) 1.0428(2) 0.054 Uiso calc R 1 . H C7 0.22381(7) 0.2935(4) 1.0267(3) 0.0462(5) Uani d . 1 . C H7 0.21175(7) 0.1577(4) 1.0925(3) 0.055 Uiso calc R 1 . H C8 0.34732(7) 0.5004(3) 0.8708(2) 0.0361(5) Uani d . 1 . C C9 0.36592(7) 0.6826(4) 0.7732(3) 0.0532(6) Uani d . 1 . C H9 0.34300(7) 0.8107(4) 0.7259(3) 0.064 Uiso calc R 1 . H C10 0.41602(8) 0.6883(5) 0.7407(3) 0.0617(7) Uani d . 1 . C H10 0.42802(8) 0.8191(5) 0.6705(3) 0.074 Uiso calc R 1 . H C11 0.44889(8) 0.5131(4) 0.8057(3) 0.0548(6) Uani d . 1 . C H11 0.48446(8) 0.5180(4) 0.7836(3) 0.066 Uiso calc R 1 . H C12 0.43151(8) 0.3310(5) 0.9018(3) 0.0602(7) Uani d . 1 . C H12 0.45477(8) 0.2041(5) 0.9488(3) 0.072 Uiso calc R 1 . H C13 0.38140(7) 0.3240(4) 0.9337(3) 0.0532(6) Uani d . 1 . C H13 0.36970(7) 0.1908(4) 1.0025(3) 0.064 Uiso calc R 1 . H N14 0.10406(6) 0.4776(4) 0.6041(3) 0.0503(5) Uani d . 1 . N H14 0.1099(8) 0.453(4) 0.724(3) 0.060 Uiso d . 1 . H H15 0.1189(8) 0.623(4) 0.579(3) 0.060 Uiso d . 1 . H C15 0.05112(7) 0.4928(4) 0.5530(2) 0.0380(5) Uani d . 1 . C C16 0.01867(7) 0.3207(4) 0.6084(3) 0.0458(5) Uani d . 1 . C H16 0.03160(7) 0.1917(4) 0.6856(3) 0.055 Uiso calc R 1 . H C17 -0.03220(7) 0.3288(4) 0.5556(3) 0.0452(5) Uani d . 1 . C H17 -0.05501(7) 0.2055(4) 0.5963(3) 0.054 Uiso calc R 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 0.0327(7) 0.0602(11) 0.0696(11) 0.0024(7) 0.0098(7) 0.0125(9) C2 0.0326(10) 0.0432(12) 0.0416(11) 0.0001(9) 0.0040(8) -0.0032(10) C3 0.0383(10) 0.0402(12) 0.0586(13) 0.0072(9) 0.0030(9) 0.0040(11) C4 0.0426(11) 0.0361(11) 0.0548(13) -0.0002(9) 0.0086(9) 0.0070(10) C5 0.0348(10) 0.0358(11) 0.0336(10) -0.0008(8) 0.0013(8) -0.0031(9) C6 0.0371(10) 0.0440(12) 0.0523(12) 0.0022(9) 0.0014(9) 0.0112(10) C7 0.0373(10) 0.0471(12) 0.0541(13) -0.0020(9) 0.0043(9) 0.0132(11) C8 0.0350(10) 0.0374(11) 0.0356(10) -0.0030(8) 0.0021(8) -0.0046(9) C9 0.0398(11) 0.0574(15) 0.0627(14) -0.0031(10) 0.0054(10) 0.0174(12) C10 0.0450(12) 0.067(2) 0.074(2) -0.0085(12) 0.0122(11) 0.0182(14) C11 0.0369(11) 0.068(2) 0.0610(14) -0.0034(11) 0.0101(10) -0.0045(13) C12 0.0439(12) 0.063(2) 0.075(2) 0.0135(11) 0.0110(11) 0.0070(14) C13 0.0446(12) 0.0491(13) 0.0674(15) 0.0066(10) 0.0132(10) 0.0130(12) N14 0.0311(9) 0.0625(13) 0.0568(12) 0.0014(8) 0.0016(8) -0.0024(11) C15 0.0274(9) 0.0465(12) 0.0401(10) 0.0010(9) 0.0039(7) -0.0076(10) C16 0.0408(10) 0.0482(13) 0.0483(12) 0.0020(10) 0.0030(9) 0.0103(11) C17 0.0358(10) 0.0470(12) 0.0533(13) -0.0076(9) 0.0073(9) 0.0064(11)