#------------------------------------------------------------------------------ #$Date: 2016-03-24 03:08:50 +0200 (Thu, 24 Mar 2016) $ #$Revision: 179615 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/50/79/4507999.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_4507999 loop_ _publ_author_name 'Bhattacharya, Suman' 'Saraswatula, Viswanadha G.' 'Saha, Binoy K.' _publ_section_title ; Thermal Expansion in Alkane Diacids---Another Property Showing Alternation in an Odd--Even Series ; _journal_issue 8 _journal_name_full 'Crystal Growth & Design' _journal_page_first 3651 _journal_paper_doi 10.1021/cg400668w _journal_volume 13 _journal_year 2013 _chemical_formula_moiety 'C4 H6 O4' _chemical_formula_sum 'C4 H6 O4' _chemical_formula_weight 118.09 _chemical_name_common C4-beta-polymorph _chemical_name_systematic '1,4-Butanedioic acid' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _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 iterative _atom_sites_solution_secondary difmap _audit_creation_date 2012-11-19 _audit_creation_method ; Olex2 1.2 (compiled 2012.05.09 svn.r2324, GUI svn.r4230) ; _cell_angle_alpha 90.00 _cell_angle_beta 92.862(7) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 5.4768(5) _cell_length_b 8.7831(7) _cell_length_c 5.0287(4) _cell_measurement_reflns_used 560 _cell_measurement_temperature 140(2) _cell_measurement_theta_max 29.1146 _cell_measurement_theta_min 3.7252 _cell_volume 241.60(4) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _diffrn_ambient_temperature 140(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.875 _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0165 _diffrn_reflns_av_unetI/netI 0.0244 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_number 1143 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 28.99 _diffrn_reflns_theta_min 3.72 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.149 _exptl_absorpt_correction_T_max 0.959 _exptl_absorpt_correction_T_min 0.951 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 124 _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _refine_diff_density_max 0.316 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.065 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 41 _refine_ls_number_reflns 560 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0335 _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^)+(0.0539P)^2^+0.0684P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0932 _refine_ls_wR_factor_ref 0.0952 _reflns_number_gt 514 _reflns_number_total 638 _reflns_threshold_expression >2sigma(I) _cod_data_source_file cg400668w_si_002.cif _cod_data_source_block C4-140 _cod_database_code 4507999 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' 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 O2 O 0.07026(15) 0.64096(10) 0.24913(18) 0.0177(3) Uani 1 1 d D O1 O 0.24905(14) 0.42198(9) 0.38022(16) 0.0156(3) Uani 1 1 d . C2 C 0.4177(2) 0.56741(12) 0.0260(2) 0.0120(3) Uani 1 1 d . H2A H 0.5179 0.6538 0.0820 0.014 Uiso 1 1 calc R H2B H 0.3281 0.5950 -0.1382 0.014 Uiso 1 1 calc R C1 C 0.23908(19) 0.53398(13) 0.2359(2) 0.0106(3) Uani 1 1 d . H2 H -0.026(3) 0.618(2) 0.380(3) 0.040(5) Uiso 1 1 d 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 O2 0.0177(5) 0.0179(5) 0.0187(5) 0.0044(3) 0.0122(4) 0.0061(3) O1 0.0144(5) 0.0164(5) 0.0166(5) 0.0033(3) 0.0083(3) 0.0019(3) C2 0.0117(6) 0.0124(6) 0.0122(5) 0.0011(4) 0.0056(4) 0.0002(4) C1 0.0090(6) 0.0130(6) 0.0101(5) -0.0029(4) 0.0023(4) -0.0009(4) 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' O O 0.0106 0.0060 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 C1 O2 H2 108.5(13) . . C2 C2 H2A 109.1 3_665 . C2 C2 H2B 109.1 3_665 . H2A C2 H2B 107.9 . . C1 C2 C2 112.42(11) . 3_665 C1 C2 H2A 109.1 . . C1 C2 H2B 109.1 . . O2 C1 C2 112.18(9) . . O1 C1 O2 123.56(9) . . O1 C1 C2 124.25(10) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O2 C1 1.3222(13) . O2 H2 0.886(15) . O1 C1 1.2220(14) . C2 C2 1.519(2) 3_665 C2 H2A 0.9700 . C2 H2B 0.9700 . C2 C1 1.5034(14) .