#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/06/2100670.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2100670 loop_ _publ_author_name 'Budzianowski, Armand' 'Olejniczak, Anna' 'Katrusiak, Andrzej' _publ_contact_author_address ;Faculty of Crystal Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznan Poland ; _publ_contact_author_email katran@amu.edu.pl _publ_contact_author_fax +48(61)8658008 _publ_contact_author_name 'Andrzej Katrusiak' _publ_contact_author_phone +48(61)8291443 _publ_section_title ; Competing hydrogen-bonding patterns and phase transitions of 1,2-diaminoethane at varied temperature and pressure ; _journal_coeditor_code AV5066 _journal_date_accepted 2006-07-31 _journal_date_recd_electronic 2006-05-22 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 1078 _journal_page_last 1089 _journal_paper_category FA _journal_volume 62 _journal_year 2006 _chemical_formula_moiety 'C2 H8 N2' _chemical_formula_sum 'C2 H8 N2' _chemical_formula_weight 60.10 _chemical_melting_point 284.29 _chemical_name_common ethylenediamine _chemical_name_systematic ; 1,2-diaminoethane phase I gamma ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 114.0(7) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.69(10) _cell_length_b 7.488(5) _cell_length_c 4.849(14) _cell_measurement_pressure 1.50(5)E6 _cell_measurement_reflns_used 516 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 29.82 _cell_measurement_theta_min 5.03 _cell_volume 321(4) _computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2002)' _computing_data_collection 'CrysAlis (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis (Oxford Diffraction, 2002)' _computing_molecular_graphics ;X-Seed (Barbour, 2001) and POV-Ray (Persistence of Vision, 2004) ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 296(2) _diffrn_detector_area_resol_mean 16.4 _diffrn_measured_fraction_theta_full 0.255 _diffrn_measured_fraction_theta_max 0.255 _diffrn_measurement_device_type 'Kuma KM4CCD \k geometry' _diffrn_measurement_method ;HP omega scans - for more details see: A. Budzianowski, A. Katrusiak in High-Pressure Crystallography (Eds.: A. Katrusiak, P. F. McMillan), Dordrecht: Kluwer Acad. Publ., 2004 pp.157-168 ; _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1082 _diffrn_reflns_av_sigmaI/netI 0.0659 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_number 2437 _diffrn_reflns_theta_full 29.82 _diffrn_reflns_theta_max 29.82 _diffrn_reflns_theta_min 5.03 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_correction_T_min 0.45 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ; Katrusiak, A. (2003). REDSHADE - Program for correcting reflections intensities for DAC absorption, gasket shadowing and sample crystal absorption. Adam Mickiewicz University, Pozna\'n. Katrusiak, A. (2004). Z. Kristallogr. 219, 461-467 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 136 _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.325 _refine_diff_density_min -0.272 _refine_ls_extinction_coef 0.8(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.393 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 26 _refine_ls_number_reflns 235 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.393 _refine_ls_R_factor_all 0.2410 _refine_ls_R_factor_gt 0.2374 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.4312 _refine_ls_wR_factor_ref 0.4331 _reflns_number_gt 225 _reflns_number_total 235 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file av5066.cif _[local]_cod_data_source_block DAE15G _[local]_cod_cif_authors_sg_H-M 'P 2(1)/c' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2100670 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' loop_ _atom_site_type_symbol _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 N N1 0.144(4) 0.3449(13) 0.275(3) 0.012(3) Uiso d G 1 H H1 0.1350 0.2312 0.3093 0.014 Uiso d G 1 H H2 0.2069 0.3559 0.1780 0.014 Uiso d G 1 C C1 -0.004(7) 0.436(2) 0.105(5) 0.037(5) Uiso d . 1 H H3 -0.0352 0.4949 0.2479 0.045 Uiso calc R 1 H H4 -0.0791 0.3469 -0.0018 0.045 Uiso calc R 1 N N2 0.651(5) 0.3723(17) 0.317(4) 0.036(5) Uiso d G 1 H H7 0.6942 0.3060 0.2219 0.043 Uiso d G 1 H H8 0.6699 0.3212 0.4965 0.043 Uiso d G 1 C C2 0.503(6) 0.4301(18) 0.118(5) 0.029(5) Uiso d . 1 H H5 0.4531 0.4790 0.2386 0.035 Uiso calc R 1 H H6 0.4456 0.3264 0.0127 0.035 Uiso calc R 1 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle C1 N1 H1 . . 113.6 C1 N1 H2 . . 111.5 H1 N1 H2 . . 108.9 N1 C1 C1 . 3_565 113(6) N1 C1 H3 . . 109.0 C1 C1 H3 3_565 . 109.0 N1 C1 H4 . . 109.0 C1 C1 H4 3_565 . 109.0 H3 C1 H4 . . 107.8 C2 N2 H7 . . 111.9 C2 N2 H8 . . 122.4 H7 N2 H8 . . 108.1 N2 C2 C2 . 3_665 116(6) N2 C2 H5 . . 108.4 C2 C2 H5 3_665 . 108.4 N2 C2 H6 . . 108.4 C2 C2 H6 3_665 . 108.4 H5 C2 H6 . . 107.4 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance N1 C1 . 1.49(6) N1 H1 . 0.8791 N1 H2 . 0.9119 C1 C1 3_565 1.42(3) C1 H3 . 0.9700 C1 H4 . 0.9700 N2 C2 . 1.43(6) N2 H7 . 0.8906 N2 H8 . 0.8984 C2 C2 3_665 1.53(3) C2 H5 . 0.9700 C2 H6 . 0.9700 _journal_paper_doi 10.1107/S010876810602982X