#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000019.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_4000019 _journal_name_full 'Chemistry of Materials' _journal_year 2000 _publ_section_title ; Hydrogen Bonding in Nitroanilines: Neutron Diffraction Study of m-nitroaniline at 100K ; loop_ _publ_author_name 'Andres E. Goeta' 'Chick C. Wilson' 'Juan C. Autino' 'Javier Ellena' 'Graciela Punte' _chemical_name_systematic ; m-nitroaniline ; _chemical_name_common 'm-nitroaniline' _chemical_formula_sum 'C6 H6 N2 O2' _chemical_formula_weight 138.00 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Pca2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 18.905(4) _cell_length_b 6.484(1) _cell_length_c 5.016(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 614.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prismatic needle' _exptl_crystal_colour orange _exptl_crystal_size_max 10 _exptl_crystal_size_mid 2 _exptl_crystal_size_min 2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 19.07 _exptl_absorpt_coefficient_mu 1.61 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details ; The linear absorption coefficient is wavelength dependent and it is calculated as: mu = 0.82 + 0.79 * lambda [cm^-1] The value of 1.61 given in _exptl_absorpt_coefficient_mu is the value at 1 \%A ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.5-5.0 _diffrn_radiation_type neutron _diffrn_radiation_source 'ISIS spallation source' _diffrn_radiation_monochromator none _diffrn_measurement_device_type 'SXD' _diffrn_measurement_method 'Time of flight LAUE diffraction' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11625 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_av_sigmaI/netI 0.032 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max ? _reflns_number_total 1664 _reflns_number_gt 1664 _reflns_threshold_expression >3sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+6.3506P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method 'Becker-Coppens Lorentzian model' _refine_ls_extinction_coef 0.127 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(10) _refine_ls_number_reflns 1664 _refine_ls_number_parameters 145 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1377 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.410 _refine_diff_density_min -2.238 _refine_diff_density_rms 0.347 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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.15173(9) 1.0450(3) 0.1792(3) 0.0139(2) Uani 1 1 d . . . C2 C 0.09158(10) 1.0156(3) 0.0205(4) 0.0178(3) Uani 1 1 d . . . H2 H 0.0785(4) 1.1276(10) -0.1304(14) 0.0401(12) Uani 1 1 d . . . C3 C 0.04867(11) 0.8448(4) 0.0531(4) 0.0201(3) Uani 1 1 d . . . H3 H 0.0022(4) 0.8277(12) -0.0675(14) 0.0436(14) Uani 1 1 d . . . C4 C 0.06434(10) 0.6960(3) 0.2440(4) 0.0173(3) Uani 1 1 d . . . H4 H 0.0316(3) 0.5610(9) 0.2740(14) 0.0367(11) Uani 1 1 d . . . C5 C 0.12421(9) 0.7283(3) 0.3985(3) 0.0133(2) Uani 1 1 d . . . C6 C 0.16825(9) 0.8975(3) 0.3714(4) 0.0141(2) Uani 1 1 d . . . H6 H 0.2146(3) 0.9134(9) 0.4962(13) 0.0350(10) Uani 1 1 d . . . N1 N 0.19584(8) 1.2117(2) 0.1389(3) 0.0200(2) Uani 1 1 d . . . H11 H 0.2281(3) 1.2447(9) 0.2917(13) 0.0355(10) Uani 1 1 d . . . H12 H 0.1748(3) 1.3348(8) 0.0489(14) 0.0356(10) Uani 1 1 d . . . N2 N 0.14159(8) 0.5766(2) 0.6024(3) 0.0177(2) Uani 1 1 d . . . O1 O 0.10120(18) 0.4316(5) 0.6349(8) 0.0330(6) Uani 1 1 d . . . O2 O 0.19518(16) 0.5999(5) 0.7348(7) 0.0286(5) Uani 1 1 d . . . 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 C1 0.0137(6) 0.0152(6) 0.0128(5) 0.0048(5) 0.0026(5) 0.0010(4) C2 0.0171(7) 0.0210(7) 0.0152(6) 0.0060(6) -0.0024(6) 0.0015(6) H2 0.042(3) 0.040(3) 0.039(3) 0.017(2) -0.011(2) 0.001(2) C3 0.0166(7) 0.0258(8) 0.0180(7) 0.0061(6) -0.0036(6) -0.0017(6) H3 0.035(2) 0.055(3) 0.040(3) 0.013(3) -0.015(2) -0.008(2) C4 0.0162(6) 0.0184(6) 0.0174(6) 0.0036(6) -0.0011(6) -0.0021(5) H4 0.036(2) 0.033(2) 0.042(3) 0.008(2) -0.006(2) -0.0109(18) C5 0.0130(5) 0.0141(5) 0.0127(5) 0.0048(5) 0.0016(5) 0.0011(4) C6 0.0136(6) 0.0153(6) 0.0133(5) 0.0052(5) -0.0009(5) -0.0007(4) H6 0.032(2) 0.036(2) 0.037(2) 0.007(2) -0.012(2) -0.0047(17) N1 0.0207(5) 0.0181(5) 0.0212(5) 0.0075(4) 0.0022(5) -0.0016(4) H11 0.036(2) 0.035(2) 0.035(2) 0.0027(19) -0.006(2) -0.0105(18) H12 0.036(2) 0.0281(19) 0.043(3) 0.0128(19) 0.000(2) 0.0010(16) N2 0.0200(5) 0.0156(4) 0.0176(5) 0.0070(4) 0.0011(4) 0.0002(4) O1 0.0367(14) 0.0244(10) 0.0380(15) 0.0177(11) -0.0021(13) -0.0084(9) O2 0.0284(11) 0.0292(11) 0.0280(11) 0.0151(10) -0.0076(10) -0.0014(9)