#------------------------------------------------------------------------------ #$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/16/2101647.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_2101647 loop_ _publ_author_name 'Suzuki, E.' 'Kabasawa, H.' 'Honma, T.' 'Nozaki, R.' 'Shiozaki, Y.' _publ_section_title ; Temperature dependence of crystal structure of NaK~0.72~(NH~4~)~0.28~(+)-C~4~H~4~O~6~.4H~2~O in the paraelectric phase ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 976 _journal_page_last 981 _journal_paper_doi 10.1107/S0108768196005502 _journal_volume 52 _journal_year 1996 _chemical_formula_moiety 'Na K0.72 (N H4 )0.28 (C4 H4 O6 ), 4H2 O' _chemical_formula_sum 'C4 H13.12 K0.72 N0.28 Na O10' _chemical_formula_weight 276.32 _space_group_IT_number 18 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2 2ab' _symmetry_space_group_name_H-M 'P 21 21 2' _atom_type_scat_source 'IntTabIV and Stewart, Davidson & Simpson (1965)' _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_formula_units_Z 4 _cell_length_a 11.9290(10) _cell_length_b 14.2970(10) _cell_length_c 6.2210(10) _cell_measurement_reflns_used 30 _cell_measurement_temperature 253 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 20 _cell_volume 1061.0(2) _diffrn_measurement_device 'Rigaku AFC-5' _diffrn_measurement_method '\w (2\q<30), 2\q-\w (30<2\q)' _diffrn_radiation_type MoK\a~1~ _diffrn_radiation_wavelength 0.70926 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 4160 _diffrn_reflns_theta_max 37.5 _diffrn_standards_decay_% 1 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.4606 _exptl_absorpt_correction_T_max 0.8436 _exptl_absorpt_correction_T_min 0.8423 _exptl_absorpt_correction_type 'numerical integration (DABEX; Dwiggins, 1975)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.730 _exptl_crystal_description sphere _exptl_crystal_F_000 575.04 _exptl_crystal_size_rad 0.25 _refine_diff_density_max 0.57 _refine_diff_density_min -0.47 _refine_ls_extinction_coef 'g = 3.973E-4' _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_goodness_of_fit_obs 1.1732 _refine_ls_hydrogen_treatment 'H atoms: see text' _refine_ls_number_parameters 197 _refine_ls_number_reflns 1989 _refine_ls_R_factor_obs 0.0498 _refine_ls_shift/esd_max <0.03 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s(F~o~)^2^ + (0.015F~o~)^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.0442 _reflns_number_observed 3284 _reflns_number_total 1989 _reflns_observed_criterion F~o~>3\s(F~o~) _cod_data_source_file oh0056.cif _cod_data_source_block oh0056b _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'w = 1/[\s(F~o~)^2^ + (0.015F~o~)^2^]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s(F~o~)^2^ + (0.015F~o~)^2^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_formula_sum 'C4 H13.12 K0.72 N0.28 Na1 O10' _cod_database_code 2101647 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z 1/2-x,1/2+y,-z 1/2+x,1/2-y,-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Na .26889(8) .49286(7) .47729(15) .0228(5) N(1) .0 .0 .0462(3) .0507(11) N(2) .0 .5 .1608(2) .0255(5) C(1) .1544(2) .1881(2) .2849(4) .0167(11) C(2) .1255(2) .2735(2) .4235(4) .0163(11) C(3) .1788(2) .2639(2) .6453(4) .0171(10) C(4) .1536(3) .3517(2) .7805(4) .0215(12) O(1) .1203(2) .10910(10) .3521(3) .0216(9) O(2) .2087(2) .20270(10) .1178(3) .0256(9) O(3) .2341(2) .40590(10) .8134(3) .0308(10) O(4) .0546(2) .36260(10) .8435(3) .0308(10) O(5) .1645(2) .35710(10) .3242(3) .0221(9) O(6) .2958(2) .2478(2) .6278(4) .0249(10) O(7) .3949(2) .0824(2) .4800(4) .0289(12) O(8) .2476(3) .0414(2) .8844(3) .0444(13) O(9) .4365(3) .2989(3) .0397(5) .0523(18) O(10) .4250(2) .3977(2) .4181(5) .0562(18) H(2) .037(2) .279(2) .433(4) .018(7) H(3) .146(2) .209(2) .731(4) .019(7) H(5) .191(3) .340(2) .212(6) .019(11) H(6) .327(4) .285(3) .621(7) .041(17) H(7a) .375(4) .119(3) .514(7) .021(14) H(7b) .433(4) .093(3) .346(7) .049(14) H(8a) .262(4) .002(3) .976(5) .015(8) H(8b) .241(3) .091(3) .960(6) .034(11) H(9a) .379(4) .282(3) .003(7) .047(15) H(9b) .464(4) .255(4) .076(7) .044(19) H(10a) .443(4) .376(3) .304(7) .037(15) H(10b) .491(3) .394(2) .474(5) .017(9) H(N1a) .042 .041 .134 .109 H(N1b) .038 -.037 -.003 .124 H(N2a) .025 .449 .038 .077 H(N2b) .053 .520 .211 .051 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 O(1) C(1) O(2) 126.3(2) yes O(1) C(1) C(2) 116.8(2) yes O(2) C(1) C(2) 116.9(2) yes C(1) C(2) O(5) 110.5(2) yes C(1) C(2) C(3) 110.0(2) yes O(5) C(2) C(3) 109.4(2) yes C(2) O(5) H(5) 105(2) yes C(2) C(3) O(6) 110.8(2) yes C(2) C(3) C(4) 109.8(2) yes O(6) C(3) C(4) 111.5(2) yes C(3) O(6) H(6) 116(4) yes C(3) C(4) O(4) 117.1(2) yes C(3) C(4) O(3) 116.3(2) yes O(3) C(4) O(4) 126.6(2) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag C(1) C(2) 1.535(3) yes C(2) C(3) 1.526(3) yes C(3) C(4) 1.541(3) yes C(1) O(1) 1.270(3) yes C(1) O(2) 1.242(3) yes C(2) O(5) 1.424(3) yes C(2) H(2) 1.06(3) yes C(3) O(6) 1.419(3) yes C(3) H(3) 1.03(3) yes C(4) O(3) 1.251(3) yes C(4) O(4) 1.254(4) yes O(5) H(5) 0.80(4) yes O(6) H(6) 0.65(4) yes