#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2002922.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_2002922 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 54 _journal_year 1998 _journal_page_first 695 _journal_page_last 704 _chemical_name_systematic '(1,4-diaminobenzene).(1,6-dihydroxyhexane)' _chemical_name_common 'p-phenylenediamine.1,6-hexanediol' _chemical_formula_moiety 'C6 H8 N2 , C6 H14 O2' _chemical_formula_sum 'C12 H22 N2 O2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_weight 226.3 _chemical_melting_point .8E-80 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 31.2595(11) _cell_length_b 5.1534(2) _cell_length_c 8.2639(5) _cell_angle_alpha 90.00000 _cell_angle_beta 104.189(4) _cell_angle_gamma 90.00000 _cell_volume 1290.64(11) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.25 _cell_measurement_theta_max 18.40 _cell_measurement_temperature 295 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .55 _exptl_crystal_size_mid .34 _exptl_crystal_size_min .30 _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_meas 1.15 _exptl_crystal_density_method suspension _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min 0.879 _exptl_absorpt_correction_T_max 0.933 _diffrn_ambient_temperature 295 _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_radiation_source sealed_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w _diffrn_reflns_number 1418 _diffrn_reflns_av_R_equivalents .018 _diffrn_reflns_av_sigmaI/netI .04 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 26.28 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 2 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 3 _diffrn_reflns_reduction_process 'Lp and empirical absorption correction' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 10.3 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -4 -2 3 -4 2 3 -25 -1 -1 _reflns_number_total 1313 _reflns_number_observed 1020 _reflns_observed_criterion 'F > 3\s(F)' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_R_factor_all .06 _refine_ls_R_factor_obs .041 _refine_ls_wR_factor_all .089 _refine_ls_wR_factor_obs .072 _refine_ls_goodness_of_fit_all .845 _refine_ls_goodness_of_fit_obs .778 _refine_ls_number_reflns 1020 _refine_ls_number_parameters 83 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_hydrogen_treatment ;OH, NH~2~ positions refined, others calc CH = 0.96, U~iso~ = 0.040 ; _refine_ls_weighting_scheme 'w=1/[\s^2^(F~o~)+(0.08F~o~)^2^]' _refine_ls_shift/esd_max .001 _refine_ls_shift/esd_mean . _refine_diff_density_max .258 _refine_diff_density_min -.212 _refine_ls_extinction_method 'Xtal CRYSLSQ (Zachariasen, 1967)' _refine_ls_extinction_coef 53E2(16) _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack 0 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 N ? .004 .003 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? .008 .006 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 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_calc_attached_atom C2 .29513(4) .2305(3) .57643(16) .0317(6) Uani ? ? N3 .34149(4) .2180(3) .64981(17) .0406(7) Uani ? ? C4 .26976(4) .4241(3) .62270(17) .0360(7) Uani ? ? O5 .62435(3) .3231(2) .45928(16) .0487(7) Uani ? ? C6 .58023(4) .3636(3) .46817(19) .0393(7) Uani ? ? C7 .55881(4) .1046(3) .48201(18) .0384(7) Uani ? ? C8 .51137(4) .1301(3) .49686(18) .0379(7) Uani ? ? C1 .27500(4) .0570(3) .45237(16) .0363(7) Uani ? ? H5 .6339(5) .468(4) .431(2) .04000 Uiso ? ? H31 .3489(5) .248(3) .762(2) .04000 Uiso ? ? H32 .3535(5) .058(4) .621(2) .04000 Uiso ? ? H4 .28346 .54499 .70813 .04000 Uiso ? ? H1 .29238 -.07731 .41940 .04000 Uiso ? ? H61 .57987 .46734 .56426 .04000 Uiso ? ? H62 .56430 .45139 .36920 .04000 Uiso ? ? H71 .55895 .00417 .38428 .04000 Uiso ? ? H72 .57568 .01637 .57913 .04000 Uiso ? ? H81 .51143 .22401 .59725 .04000 Uiso ? ? H82 .49488 .22546 .40219 .04000 Uiso ? ? 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 C2 .0289(7) .0325(7) .0356(7) -.0021(5) .0112(5) .0053(5) N3 .0296(7) .0446(8) .0472(8) -.0012(5) .0086(6) .0020(6) C4 .0379(8) .0321(7) .0376(7) -.0029(6) .0087(6) -.0047(6) O5 .0313(6) .0409(7) .0783(9) -.0013(5) .0221(6) .0092(6) C6 .0288(7) .0361(8) .0548(9) -.0017(6) .0136(6) .0031(7) C7 .0299(8) .0363(8) .0499(8) -.0032(6) .0116(6) .0031(6) C8 .0292(7) .0376(8) .0479(8) -.0031(6) .0113(6) .0020(6) C1 .0367(8) .0328(8) .0413(8) .0031(5) .0127(6) -.0036(6) _cod_database_code 2002922