#------------------------------------------------------------------------------ #$Date: 2017-10-13 13:16:50 +0300 (Fri, 13 Oct 2017) $ #$Revision: 201980 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/30/00/2300042.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_2300042 loop_ _publ_author_name 'Dawson, Alice' 'Allan, David R.' 'Parsons, Simon' 'Ruf, Michael' _publ_section_title ; Use of a CCD diffractometer in crystal structure determinations at high pressure ; _journal_issue 3 _journal_name_full 'Journal of Applied Crystallography' _journal_page_first 410 _journal_page_last 416 _journal_paper_doi 10.1107/S0021889804007149 _journal_volume 37 _journal_year 2004 _chemical_formula_moiety ' C2 H4 O2 ' _chemical_formula_sum 'C2 H4 O2' _chemical_formula_weight 60.05 _chemical_name_systematic ; acetic acid ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method CRYSTALS_ver_12.20 _cell_angle_alpha 90 _cell_angle_beta 93.177(12) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 3.9447(6) _cell_length_b 13.028(2) _cell_length_c 5.6407(9) _cell_measurement_reflns_used 193 _cell_measurement_temperature 293 _cell_measurement_theta_max 20 _cell_measurement_theta_min 4 _cell_volume 289.44(8) _computing_cell_refinement ; SAINT (Siemens ,1995) ; _computing_data_collection ; SMART (Siemens, 1993) ; _computing_data_reduction ; SAINT (Siemens ,1995) ; _computing_molecular_graphics ; XP ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_structure_solution ; SHELXS 86 (Sheldrick, 1986) ; _diffrn_ambient_temperature 293 _diffrn_measured_fraction_theta_full 0.707 _diffrn_measured_fraction_theta_max 0.610 _diffrn_measurement_device_type ; Bruker SMART ; _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0596 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2385 _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; _diffrn_reflns_theta_full 17.544 _diffrn_reflns_theta_max 23.084 _diffrn_reflns_theta_min 3.942 _diffrn_standards_decay_% 0.00 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.125 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.597 _exptl_absorpt_correction_type 'empirical, analytical and multi-scan' _exptl_absorpt_process_details ; SHADE (Parsons, 2004) SADABS (Siemens, 1996) Data from Sadabs given below. ; _exptl_crystal_colour ' colourless ' _exptl_crystal_density_diffrn 1.378 _exptl_crystal_description ' block ' _exptl_crystal_F_000 128 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.17 _refine_diff_density_max 0.14 _refine_diff_density_min -0.11 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.0384 _refine_ls_hydrogen_treatment 'restrained refall' _refine_ls_matrix_type full _refine_ls_number_parameters 50 _refine_ls_number_reflns 249 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0379 _refine_ls_shift/su_max 0.000935 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; Method = SHELXL 97 (Sheldrick, 1997) W = 1. / [Sigma^2^(Fo^2^)+(0.0428p)^2^+ 0.0675p] where p=0.333*max(Fo^2^,0) + 0.667*Fc^2^ ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0892 _refine_ls_wR_factor_gt 0.0828 _refine_ls_wR_factor_ref 0.0892 _reflns_number_gt 189 _reflns_number_total 251 _reflns_threshold_expression I>2.00u(I) _cod_data_source_file he5280.cif _cod_data_source_block he5280 _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_original_sg_symbol_H-M 'P 21/n' _cod_original_formula_sum ' C2 H4 O2 ' _cod_database_code 2300042 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol O1 0.4025(6) 0.37335(15) 0.4339(4) 0.0563 Uani 1.0000 . . O C1 0.2243(8) 0.3357(3) 0.6031(6) 0.0421 Uani 1.0000 . . C O2 0.1455(5) 0.24643(18) 0.6091(4) 0.0538 Uani 1.0000 . . O C2 0.1409(8) 0.4134(2) 0.7850(6) 0.0526 Uani 1.0000 . . C H1 0.449(9) 0.3271(10) 0.345(5) 0.088(6) Uiso 1.0000 . . H H21 -0.014(4) 0.4574(11) 0.7219(17) 0.088(6) Uiso 1.0000 . . H H22 0.329(2) 0.4477(13) 0.832(3) 0.088(6) Uiso 1.0000 . . H H23 0.057(6) 0.3816(5) 0.910(2) 0.088(6) Uiso 1.0000 . . 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 0.0780(17) 0.0409(18) 0.053(2) -0.0057(11) 0.0286(16) -0.0025(10) C1 0.046(2) 0.036(3) 0.045(3) 0.0015(15) 0.007(2) 0.0021(14) O2 0.0735(18) 0.043(2) 0.047(3) -0.0065(11) 0.0203(18) -0.0034(10) C2 0.059(3) 0.049(3) 0.052(4) 0.0041(14) 0.014(3) -0.0063(14) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C ' 0.0033 0.0016 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 International_Tables_Vol_IV_Table_2.2B loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C1 O1 H1 108.7(9) no O1 C1 O2 122.1(3) yes O1 C1 C2 113.2(3) yes O2 C1 C2 124.7(3) yes C1 C2 H21 109.45(6) no C1 C2 H22 109.45(6) no H21 C2 H22 109.49(6) no C1 C2 H23 109.45(6) no H21 C2 H23 109.49(6) no H22 C2 H23 109.49(6) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C1 . . 1.312(3) yes O1 H1 . . 0.812(9) no C1 O2 . . 1.205(3) yes C1 C2 . . 1.491(4) yes C2 H21 . . 0.896(7) no C2 H22 . . 0.895(7) no C2 H23 . . 0.898(7) no loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 171