#------------------------------------------------------------------------------ #$Date: 2013-08-27 17:21:32 +0300 (Tue, 27 Aug 2013) $ #$Revision: 87780 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/50/79/4507995.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_4507995 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 'C3 H4 O4' _chemical_formula_sum 'C3 H4 O4' _chemical_formula_weight 104.06 _chemical_name_common C3-220-beta-polymorph _chemical_name_systematic '1,3-Propanoic acid' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _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 108.262(8) _cell_angle_beta 100.971(7) _cell_angle_gamma 95.138(7) _cell_formula_units_Z 2 _cell_length_a 5.1578(4) _cell_length_b 5.3301(5) _cell_length_c 8.2920(7) _cell_measurement_reflns_used 953 _cell_measurement_temperature 220(2) _cell_measurement_theta_max 28.7904 _cell_measurement_theta_min 4.0412 _cell_volume 209.78(3) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) ; _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 ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _diffrn_ambient_temperature 220(2) _diffrn_detector_area_resol_mean 15.9821 _diffrn_measured_fraction_theta_full 0.9942 _diffrn_measured_fraction_theta_max 0.9412 _diffrn_measurement_details ; 1 omega -21.00 14.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -17.4178 -99.0000 0.0000 35 2 omega -72.00 27.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -17.4178 -19.0000 60.0000 99 3 omega -90.00 4.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -17.4178 -37.0000 0.0000 94 4 omega -20.00 19.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -17.4178 -99.0000 150.0000 39 5 omega 57.00 87.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 19.1366 178.0000 90.0000 30 6 omega 13.00 38.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 19.1366 -57.0000 -150.0000 25 7 omega 47.00 95.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 19.1366 178.0000 0.0000 48 8 omega -38.00 51.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -17.4178 57.0000 120.0000 89 9 omega -2.00 31.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 19.1366 57.0000 -90.0000 33 ; _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0226599000 _diffrn_orient_matrix_UB_12 -0.1329996000 _diffrn_orient_matrix_UB_13 -0.0595296000 _diffrn_orient_matrix_UB_21 -0.0988411000 _diffrn_orient_matrix_UB_22 -0.0364579000 _diffrn_orient_matrix_UB_23 0.0411069000 _diffrn_orient_matrix_UB_31 -0.0993950000 _diffrn_orient_matrix_UB_32 0.0340645000 _diffrn_orient_matrix_UB_33 -0.0578723000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0148 _diffrn_reflns_av_unetI/netI 0.0209 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 2015 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 28.83 _diffrn_reflns_theta_min 4.05 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.94234 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 108 _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.316 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.043 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 72 _refine_ls_number_reflns 962 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0348 _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^)+(0.0418P)^2^+0.0715P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0885 _refine_ls_wR_factor_ref 0.0926 _reflns_number_gt 861 _reflns_number_total 962 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file cg400668w_si_002.cif _[local]_cod_data_source_block C3-220 _cod_database_code 4507995 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' 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 O3 O 1.04390(17) 1.19185(18) 0.87378(12) 0.0281(3) Uani 1 1 d . O4 O 0.6691(2) 1.3221(2) 0.94761(14) 0.0332(3) Uani 1 1 d . O1 O 0.9140(3) 0.5633(2) 0.68443(15) 0.0443(3) Uani 1 1 d . O2 O 0.7710(3) 0.7451(2) 0.48399(14) 0.0428(3) Uani 1 1 d . C1 C 0.7845(2) 0.7159(2) 0.63510(16) 0.0242(3) Uani 1 1 d . C3 C 0.8022(2) 1.1523(2) 0.86308(16) 0.0222(3) Uani 1 1 d . C2 C 0.6278(3) 0.8916(3) 0.74670(17) 0.0267(3) Uani 1 1 d . H2A H 0.5588 0.7988 0.8186 0.032 Uiso 1 1 calc R H2B H 0.4749 0.9278 0.6718 0.032 Uiso 1 1 calc R H4 H 0.775(5) 1.473(5) 1.014(3) 0.075(7) Uiso 1 1 d . H2 H 0.878(5) 0.649(5) 0.431(3) 0.069(7) Uiso 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 O3 0.0217(5) 0.0239(5) 0.0368(5) 0.0049(4) 0.0106(4) 0.0061(4) O4 0.0260(5) 0.0246(5) 0.0425(6) -0.0026(4) 0.0153(4) 0.0065(4) O1 0.0647(8) 0.0441(7) 0.0424(6) 0.0222(5) 0.0303(6) 0.0345(6) O2 0.0535(7) 0.0543(7) 0.0310(6) 0.0168(5) 0.0189(5) 0.0328(6) C1 0.0243(6) 0.0195(6) 0.0250(6) 0.0020(5) 0.0066(5) 0.0030(5) C3 0.0231(6) 0.0210(6) 0.0240(6) 0.0068(5) 0.0091(5) 0.0067(5) C2 0.0225(6) 0.0235(6) 0.0309(7) 0.0022(5) 0.0098(5) 0.0051(5) 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 C3 O4 H4 111.1(17) C1 O2 H2 109.1(15) O1 C1 O2 123.62(12) O1 C1 C2 122.29(12) O2 C1 C2 114.08(11) O3 C3 O4 125.22(12) O3 C3 C2 122.00(11) O4 C3 C2 112.79(11) C1 C2 C3 110.55(10) C1 C2 H2A 109.5 C1 C2 H2B 109.5 C3 C2 H2A 109.5 C3 C2 H2B 109.5 H2A C2 H2B 108.1 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O3 C3 1.2272(15) O4 C3 1.2953(15) O4 H4 0.88(3) O1 C1 1.2151(16) O2 C1 1.3003(16) O2 H2 0.87(3) C1 C2 1.5045(17) C3 C2 1.5088(18) C2 H2A 0.9800 C2 H2B 0.9800 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion O3 C3 C2 C1 -7.43(18) O4 C3 C2 C1 172.84(11) O1 C1 C2 C3 87.38(16) O2 C1 C2 C3 -91.78(14)