#------------------------------------------------------------------------------ #$Date: 2017-06-01 01:00:56 +0300 (Thu, 01 Jun 2017) $ #$Revision: 197080 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/41/4514128.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_4514128 loop_ _publ_author_name 'Malaspina, Lorraine A.' 'Edwards, Alison J.' 'Woi\'nska, Magdalena' 'Jayatilaka, Dylan' 'Turner, Michael J.' 'Price, Jason R.' 'Herbst-Irmer, Regine' 'Sugimoto, Kunihisa' 'Nishibori, Eiji' 'Grabowsky, Simon' _publ_contact_author ; Dr. Simon Grabowsky University of Bremen Institute for Inorganic Chemistry and Crystallography Leobener Str. NW2 28359 Bremen Germany ; _publ_section_title ; Predicting the Position of the Hydrogen Atom in the Short Intramolecular Hydrogen Bond of the Hydrogen Maleate Anion from Geometric Correlations ; _journal_name_full 'Crystal Growth & Design' _journal_paper_doi 10.1021/acs.cgd.7b00390 _journal_year 2017 _chemical_formula_moiety 'C4 H3 O4, K' _chemical_formula_sum 'C4 H3 K O4' _chemical_formula_weight 154.16 _chemical_name_common 'Potassium hydrogen maleate' _space_group_IT_number 57 _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 57 _symmetry_space_group_name_Hall '-P 2c 2b' _symmetry_space_group_name_H-M 'P b c m' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary isomor _audit_creation_date 2017-03-09 _audit_creation_method CRYSTALS_ver_14.61 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 4.5071(9) _cell_length_b 7.7017(15) _cell_length_c 15.921(3) _cell_measurement_radiation Synchrotron _cell_measurement_reflns_used 133388 _cell_measurement_temperature 25 _cell_measurement_theta_max 36.075 _cell_measurement_theta_min 0.635 _cell_measurement_wavelength 0.3531 _cell_volume 552.66(19) _computing_cell_refinement 'LaueG (Piltz, 2011)' _computing_data_collection 'MAATEL/ANSTO control program' _computing_data_reduction 'argonne_boxes (Wilkinson et al., 1988) & LaueG (Piltz, 2011)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _diffrn_ambient_temperature 12 _diffrn_measured_fraction_theta_full 0.884 _diffrn_measured_fraction_theta_max 0.884 _diffrn_measurement_details '20 images, exposure time 100 to 100 minutes' _diffrn_measurement_device 'Laue image-plate diffractometer' _diffrn_measurement_device_type KOALA _diffrn_measurement_method Laue _diffrn_radiation_probe neutron _diffrn_radiation_type neutron _diffrn_radiation_wavelength 0.85 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_unetI/netI 0.0622 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 16079 _diffrn_reflns_reduction_process 'LaueG (Piltz, 2011)' _diffrn_reflns_resolution_max 1.54 _diffrn_reflns_theta_full 70.68 _diffrn_reflns_theta_max 70.78 _diffrn_source 'nuclear reactor' _diffrn_source_details 'thermal neutrons, supermirror guides' _diffrn_source_type 'OPAL reactor, ANSTO, Lucas Heights, Australia' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.0 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 176 _exptl_crystal_size_max 1.6 _exptl_crystal_size_mid 1.5 _exptl_crystal_size_min 0.4 _refine_diff_density_max 0.58 _refine_diff_density_min -0.56 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.0000 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 57 _refine_ls_number_reflns 695 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0264 _refine_ls_shift/su_max 0.0005269 _refine_ls_shift/su_mean 0.0000804 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 80.9 36.7 55.0 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0644 _refine_ls_wR_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.0436 _reflns_number_gt 774 _reflns_number_total 946 _reflns_threshold_expression >2sigma(I) _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _oxford_refine_ls_r_factor_ref 0.0237 _oxford_refine_ls_scale 1.299(6) _oxford_reflns_number_all 811 _oxford_reflns_threshold_expression_ref I>3.0\s(I) _iucr_refine_instructions_details ; # # Punched on 09/03/17 at 15:38: 6 # #LIST 12 BLOCK CONT SCALE CONT K ( 1 ,X'S,U'S) UNTIL LAST END # # Punched on 09/03/17 at 15:38: 6 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _cod_data_source_file KHmal_F2.cif _cod_data_source_block KHmal_neutron_F2 _cod_original_cell_volume 552.66(11) _cod_original_sg_symbol_H-M 'P b c m ' _cod_database_code 4514128 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,z x,-y+1/2,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -x,-y,z+1/2 x,y,-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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp K1 K 0.7613(3) 0.2500 0.5000 0.0048 1.0000 Uani S T O3 O 1.26408(14) 0.08071(8) 0.42891(4) 0.0067 1.0000 Uani . . C1 C 1.21688(13) 0.10372(6) 0.35308(3) 0.0047 1.0000 Uani . . O1 O 1.01024(15) 0.20572(8) 0.32615(3) 0.0066 1.0000 Uani . . C2 C 1.41275(15) 0.01030(6) 0.29216(3) 0.0057 1.0000 Uani . . H2 H 1.5813(3) -0.06738(17) 0.32338(8) 0.0207 1.0000 Uani . . H1 H 1.0012(4) 0.2081(3) 0.2500 0.0186 1.0000 Uani S T 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 K1 0.0051(9) 0.0046(6) 0.0048(6) 0.0007(3) 0.0000 0.0000 O3 0.0080(3) 0.0077(2) 0.0044(2) 0.00015(16) -0.00005(17) 0.00057(17) C1 0.0051(2) 0.00502(19) 0.00396(19) -0.00015(13) -0.00017(15) 0.00009(15) O1 0.0073(3) 0.0076(2) 0.0050(2) -0.00011(18) -0.00044(17) 0.00251(18) C2 0.0064(3) 0.00627(19) 0.00451(17) 0.00011(12) -0.00023(18) 0.00146(15) H2 0.0208(7) 0.0243(6) 0.0170(4) 0.0021(4) -0.0032(5) 0.0110(5) H1 0.0170(10) 0.0176(7) 0.0211(7) 0.0000 0.0000 0.0050(6) 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 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 6.6484 'Neutron Data Booklet 2nd Ed July 2003, ILL Table 1.1' H 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 -3.7409 'Neutron Data Booklet 2nd Ed July 2003, ILL Table 1.1' O 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 5.8050 'Neutron Data Booklet 2nd Ed July 2003, ILL Table 1.1' K 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 3.6700 'Neutron Data Booklet 2nd Ed July 2003, ILL Table 1.1' loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O3 . C1 O1 . 122.30(5) yes O3 . C1 C2 . 117.50(5) yes O1 . C1 C2 . 120.19(5) yes C1 . O1 H1 . 111.40(10) no C1 . C2 C2 8_555 130.42(3) yes C1 . C2 H2 . 112.37(8) no C2 8_555 C2 H2 . 117.21(7) no O1 . H1 O1 8_555 175.80(18) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O3 C1 . 1.2387(8) yes C1 O1 . 1.2916(8) yes C1 C2 . 1.4959(8) yes O1 H1 . 1.2131(6) no C2 C2 8_555 1.3424(11) yes C2 H2 . 1.0871(14) 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 C2 H2 O1 3_845 153.30(10) 1.0872(15) 2.5387(16) 3.5439(11) yes