#------------------------------------------------------------------------------ #$Date: 2016-05-17 08:50:28 +0300 (Tue, 17 May 2016) $ #$Revision: 182987 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/52/7225252.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_7225252 loop_ _publ_author_name 'McFarlane, Andrew R.' 'Geller, Hannah' 'Silverwood, Ian P.' 'Cooper, Richard I.' 'Watkin, David J.' 'Parker, Stewart F.' 'Winfield, John M.' 'Lennon, David' _publ_section_title ; The application of inelastic neutron scattering to investigate the interaction of methyl propanoate with silica ; _journal_name_full 'Phys. Chem. Chem. Phys.' _journal_paper_doi 10.1039/C6CP01276K _journal_year 2016 _chemical_formula_moiety 'C4 H8 O2' _chemical_formula_sum 'C4 H8 O2' _chemical_formula_weight 88.11 _chemical_melting_point 185 _chemical_name_common 'Methyl propionate' _chemical_name_systematic 'Methyl propanoate' _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary other _audit_update_record ; 2016-02-16 deposited with the CCDC. 2016-05-16 downloaded from the CCDC. ; _cell_angle_alpha 87.987(3) _cell_angle_beta 89.585(3) _cell_angle_gamma 84.399(4) _cell_formula_units_Z 4 _cell_length_a 5.9523(5) _cell_length_b 6.7864(5) _cell_length_c 12.7209(11) _cell_measurement_reflns_used 1829 _cell_measurement_temperature 150 _cell_measurement_theta_max 26 _cell_measurement_theta_min 5 _cell_volume 511.08(7) _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_data_reduction 'DENZO/SCALEPACK ' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _computing_publication_material 'CRYSTALS ' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _diffrn_ambient_temperature 150 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measurement_device Area _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 6235 _diffrn_reflns_theta_full 25.090 _diffrn_reflns_theta_max 26.135 _diffrn_reflns_theta_min 5.337 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_description cylinder _exptl_crystal_F_000 192 _exptl_crystal_recrystallization_method 'Zone refinement of a frozen sample' _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad 0.050 _refine_diff_density_max 0.33 _refine_diff_density_min -0.32 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 0.8768 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 157 _refine_ls_number_reflns 1996 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_gt 0.0644 _refine_ls_shift/su_max 0.0001038 _refine_ls_shift/su_mean 0.0000155 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.20P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.2120 _refine_ls_wR_factor_gt 0.1851 _refine_ls_wR_factor_ref 0.2120 _reflns_limit_h_max 7 _reflns_limit_h_min -7 _reflns_limit_k_max 8 _reflns_limit_k_min -8 _reflns_limit_l_max 15 _reflns_limit_l_min 0 _reflns_number_gt 1419 _reflns_number_total 1996 _reflns_threshold_expression I>2.0\s(I) _oxford_diffrn_Wilson_B_factor 3.68 _oxford_diffrn_Wilson_scale 0.37 _oxford_refine_ls_r_factor_ref 0.0893 _oxford_refine_ls_scale 1.75(4) _oxford_reflns_number_all 1996 _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _cod_data_source_file c6cp01276k2.cif _cod_data_source_block 1 _cod_depositor_comments ; The following automatic conversions were performed: '_atom_sites_solution_primary' value 'Other' changed to 'other' according to /usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas ; _cod_original_sg_symbol_H-M 'P -1 ' _cod_database_code 7225252 _iucr_refine_instruction_details_constraints ; BLOCK CONT SCALE CONT O ( 1 ,X'S,U'S) UNTIL C ( 12 ) CONT H ( 43 ,X'S) UNTIL H ( 121 ) END ; _iucr_refine_instruction_details_restraints ; NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; loop_ _symmetry_equiv_pos_as_xyz x,y,z -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_occupancy _atom_site_adp_type O1 O 0.6536(3) 0.2491(2) 0.20934(13) 0.0532 1.0000 Uani C2 C 0.8137(4) 0.2425(3) 0.26701(17) 0.0427 1.0000 Uani O3 O 0.7918(3) 0.2457(2) 0.37237(12) 0.0503 1.0000 Uani C4 C 0.5618(5) 0.2555(4) 0.4114(2) 0.0543 1.0000 Uani C5 C 1.0558(4) 0.2300(4) 0.23429(19) 0.0491 1.0000 Uani C6 C 1.0870(5) 0.2265(5) 0.1160(2) 0.0570 1.0000 Uani O7 O 0.8756(3) 0.7475(3) 0.27727(13) 0.0532 1.0000 Uani C8 C 0.9361(5) 0.7367(5) 0.3871(2) 0.0591 1.0000 Uani C9 C 0.6564(4) 0.7549(3) 0.25497(17) 0.0430 1.0000 Uani O10 O 0.5125(3) 0.7535(3) 0.32170(13) 0.0560 1.0000 Uani C11 C 0.6162(4) 0.7662(4) 0.1388(2) 0.0524 1.0000 Uani C12 C 0.3933(5) 0.7050(5) 0.1068(2) 0.0595 1.0000 Uani H43 H 0.566(6) 0.250(4) 0.490(3) 0.0791 1.0000 Uiso H41 H 0.474(6) 0.374(5) 0.380(3) 0.0786 1.0000 Uiso H42 H 0.500(6) 0.137(5) 0.384(3) 0.0784 1.0000 Uiso H51 H 1.121(5) 0.352(4) 0.264(2) 0.0564 1.0000 Uiso H52 H 1.126(5) 0.109(4) 0.266(2) 0.0562 1.0000 Uiso H62 H 1.250(7) 0.217(4) 0.098(3) 0.0805 1.0000 Uiso H63 H 1.008(6) 0.358(5) 0.082(3) 0.0797 1.0000 Uiso H61 H 1.010(6) 0.115(5) 0.091(3) 0.0806 1.0000 Uiso H83 H 1.106(7) 0.744(5) 0.390(3) 0.0838 1.0000 Uiso H81 H 0.872(6) 0.853(5) 0.422(3) 0.0831 1.0000 Uiso H82 H 0.886(6) 0.623(5) 0.424(3) 0.0835 1.0000 Uiso H111 H 0.616(5) 0.905(4) 0.120(2) 0.0604 1.0000 Uiso H112 H 0.737(5) 0.688(4) 0.108(2) 0.0604 1.0000 Uiso H122 H 0.377(6) 0.723(5) 0.031(3) 0.0879 1.0000 Uiso H123 H 0.272(7) 0.789(5) 0.135(3) 0.0881 1.0000 Uiso H121 H 0.384(6) 0.575(5) 0.130(3) 0.0877 1.0000 Uiso 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 O1 0.0489(10) 0.0719(11) 0.0383(9) -0.0004(7) -0.0037(8) -0.0038(8) C2 0.0514(13) 0.0432(11) 0.0337(11) 0.0008(8) -0.0013(10) -0.0056(9) O3 0.0517(10) 0.0643(10) 0.0353(9) -0.0006(7) 0.0011(7) -0.0086(7) C4 0.0556(15) 0.0664(15) 0.0411(14) -0.0030(11) 0.0111(11) -0.0068(12) C5 0.0459(13) 0.0600(13) 0.0418(13) 0.0008(10) -0.0015(10) -0.0079(11) C6 0.0520(15) 0.0724(16) 0.0467(15) -0.0036(12) 0.0073(11) -0.0069(12) O7 0.0421(9) 0.0754(11) 0.0418(10) 0.0027(7) 0.0029(7) -0.0065(7) C8 0.0592(16) 0.0696(16) 0.0485(15) 0.0046(12) -0.0102(12) -0.0072(13) C9 0.0415(12) 0.0450(11) 0.0425(13) -0.0003(9) 0.0052(9) -0.0055(8) O10 0.0484(10) 0.0813(12) 0.0386(9) -0.0012(8) 0.0100(7) -0.0091(8) C11 0.0549(14) 0.0638(15) 0.0387(13) 0.0004(10) 0.0046(11) -0.0082(12) C12 0.0609(16) 0.0688(16) 0.0486(15) -0.0011(12) -0.0071(12) -0.0055(13) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 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_publ_flag O1 C2 O3 122.4(2) yes O1 C2 C5 126.2(2) yes O3 C2 C5 111.41(19) yes C2 O3 C4 115.23(19) yes O3 C4 H43 108(2) no O3 C4 H41 109.2(19) no H43 C4 H41 115(3) no O3 C4 H42 105.1(19) no H43 C4 H42 111(3) no H41 C4 H42 108(3) no C2 C5 C6 112.9(2) yes C2 C5 H51 106.6(15) no C6 C5 H51 110.5(15) no C2 C5 H52 106.3(16) no C6 C5 H52 109.3(16) no H51 C5 H52 111(2) no C5 C6 H62 110.3(20) no C5 C6 H63 109.0(19) no H62 C6 H63 109(3) no C5 C6 H61 107.2(19) no H62 C6 H61 113(3) no H63 C6 H61 108(3) no C8 O7 C9 116.9(2) yes O7 C8 H83 106(2) no O7 C8 H81 110(2) no H83 C8 H81 105(3) no O7 C8 H82 113(2) no H83 C8 H82 114(3) no H81 C8 H82 108(3) no O7 C9 O10 122.8(2) yes O7 C9 C11 111.64(19) yes O10 C9 C11 125.5(2) yes C9 C11 C12 114.4(2) yes C9 C11 H111 104.6(16) no C12 C11 H111 106.9(16) no C9 C11 H112 106.4(18) no C12 C11 H112 111.8(18) no H111 C11 H112 113(2) no C11 C12 H122 109(2) no C11 C12 H123 111(2) no H122 C12 H123 105(3) no C11 C12 H121 109(2) no H122 C12 H121 112(3) no H123 C12 H121 110(3) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O1 C2 1.203(3) yes C2 O3 1.346(3) yes C2 C5 1.492(3) yes O3 C4 1.449(3) yes C4 H43 1.00(4) no C4 H41 0.99(3) no C4 H42 0.99(3) no C5 C6 1.516(4) yes C5 H51 1.03(3) no C5 H52 0.96(3) no C6 H62 0.99(4) no C6 H63 1.05(3) no C6 H61 0.99(3) no O7 C8 1.443(3) yes O7 C9 1.333(3) yes C8 H83 1.02(4) no C8 H81 0.96(4) no C8 H82 0.96(3) no C9 O10 1.202(3) yes C9 C11 1.496(3) yes C11 C12 1.492(4) yes C11 H111 0.96(3) no C11 H112 0.94(3) no C12 H122 0.98(4) no C12 H123 0.95(4) no C12 H121 0.93(4) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C4 H43 O10 2_666 168(3) 0.999 2.438 3.420(4) yes C8 H83 O10 1_655 159(3) 1.017 2.570 3.536(4) yes