#------------------------------------------------------------------------------ #$Date: 2019-05-23 07:01:00 +0300 (Thu, 23 May 2019) $ #$Revision: 215438 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/28/7232813.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_7232813 loop_ _publ_author_name 'Ma, Yike' 'Huang, Liangliang' 'Xiu, Zhijia' 'Yang, Yuheng' 'Wang, Xiaodong' 'Yin, Yanzhen' 'Bi, Yanfeng' 'Zheng, Zhiping' _publ_section_title ; High proton conductivity behavior in a 2D metal sulfite constructed from a histidine ligand ; _journal_issue 28 _journal_name_full 'RSC Advances' _journal_page_first 16130 _journal_paper_doi 10.1039/C9RA01584A _journal_volume 9 _journal_year 2019 _chemical_formula_sum 'C12 H20 N6 O11 S2 Zn2' _chemical_formula_weight 619.20 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-01-23 deposited with the CCDC. 2019-04-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.397(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.6764(7) _cell_length_b 8.3407(4) _cell_length_c 16.8021(8) _cell_measurement_reflns_used 4092 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 25.0378 _cell_measurement_theta_min 2.4731 _cell_volume 2016.21(17) _computing_cell_refinement 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_data_collection 'Bruker Instrument Service vV6.2.3' _computing_data_reduction 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'XT, VERSION 2014/5' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker D8 QUEST' _diffrn_measurement_method '\f & \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_unetI/netI 0.0269 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 8485 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.086 _diffrn_reflns_theta_max 25.086 _diffrn_reflns_theta_min 2.473 _exptl_absorpt_coefficient_mu 2.660 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.6326 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.040 _exptl_crystal_description block _exptl_crystal_F_000 1256 _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.321 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.066 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 151 _refine_ls_number_reflns 1782 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0258 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+3.5637P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.0608 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1537 _reflns_number_total 1782 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ra01584a2.cif _cod_data_source_block Compound_1 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-Scan' changed to 'multi-scan' according to /home/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 4973 2017-02-22 13:04:09Z antanas ; _cod_database_code 7232813 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.592 _shelx_estimated_absorpt_t_max 0.618 _shelx_res_file ; myk35_0m_a.res created by SHELXL-2014/7 TITL myk35_0m_a.res in C2/c CELL 0.71073 14.6764 8.3407 16.8021 90.000 101.397 90.000 ZERR 4.000 0.0007 0.0004 0.0008 0.000 0.002 0.000 LATT 7 SYMM -X, Y, 1/2-Z SFAC C H N O S Zn UNIT 48 80 24 44 8 8 L.S. 30 ACTA BOND $H FMAP 2 PLAN 5 SIZE 0.20 0.21 0.22 TEMP 23 WGHT 0.026400 3.563700 FVAR 0.19195 ZN1 6 0.618209 0.488383 0.567885 11.00000 0.02515 0.01761 = 0.01752 -0.00039 -0.00159 0.00141 S1 5 0.568268 0.624845 0.388281 11.00000 0.02265 0.02019 = 0.02203 0.00001 0.00435 0.00290 O1 4 0.587634 0.641777 0.481140 11.00000 0.05105 0.02631 = 0.02002 0.00671 -0.00475 0.00329 O2 4 0.480280 0.523100 0.367578 11.00000 0.03682 0.02722 = 0.03271 -0.00684 0.01139 -0.01165 O3 4 0.540834 0.793620 0.359482 11.00000 0.02804 0.02133 = 0.02016 0.00373 -0.00078 -0.00026 O4 4 0.728723 0.552205 0.650225 11.00000 0.02678 0.02548 = 0.02209 -0.00811 -0.00403 0.00144 O5 4 0.657748 0.774577 0.678331 11.00000 0.03090 0.02458 = 0.02972 -0.00049 -0.00167 0.00708 N1 3 0.861132 0.765079 0.966127 11.00000 0.02825 0.02001 = 0.01579 0.00197 0.00345 -0.00253 N2 3 0.874666 0.591204 0.770232 11.00000 0.02167 0.02828 = 0.02003 -0.00122 0.00103 -0.00106 AFIX 137 H2A 2 0.858913 0.490816 0.779365 11.00000 -1.50000 H2B 2 0.921786 0.621761 0.809151 11.00000 -1.50000 H2C 2 0.891708 0.596692 0.722327 11.00000 -1.50000 AFIX 0 N3 3 0.892709 0.541757 1.033318 11.00000 0.03993 0.02794 = 0.01834 0.00963 0.00068 0.00315 AFIX 43 H3 2 0.916764 0.475670 1.070926 11.00000 -1.20000 AFIX 0 C1 1 0.721200 0.675717 0.692691 11.00000 0.02282 0.01888 = 0.01724 -0.00012 0.00402 -0.00651 C2 1 0.794229 0.698112 0.769988 11.00000 0.02023 0.01779 = 0.01944 -0.00183 0.00196 -0.00210 AFIX 13 H2 2 0.815711 0.809598 0.772803 11.00000 -1.20000 AFIX 0 C3 1 0.747434 0.665053 0.842105 11.00000 0.02089 0.02553 = 0.01999 -0.00117 0.00377 -0.00370 AFIX 23 H3A 2 0.706223 0.753878 0.846970 11.00000 -1.20000 H3B 2 0.709267 0.569807 0.830099 11.00000 -1.20000 AFIX 0 C4 1 0.810926 0.641761 0.921942 11.00000 0.02285 0.02071 = 0.01917 -0.00102 0.00730 -0.00068 C5 1 0.830667 0.504470 0.964282 11.00000 0.04406 0.01947 = 0.02326 -0.00033 0.00650 -0.00538 AFIX 43 H5 2 0.806472 0.403446 0.949172 11.00000 -1.20000 AFIX 0 C6 1 0.909489 0.697597 1.032372 11.00000 0.03496 0.02524 = 0.02024 0.00149 0.00070 -0.00410 AFIX 43 H6 2 0.949921 0.752330 1.072920 11.00000 -1.20000 AFIX 0 O1W 4 0.000000 0.309402 0.750000 10.50000 0.05208 0.08198 = 0.09541 0.00000 0.04198 0.00000 AFIX 3 H1W 2 0.035450 0.250342 0.728220 11.00000 -1.20000 AFIX 0 HKLF 4 REM myk35_0m_a.res in C2/c REM R1 = 0.0258 for 1537 Fo > 4sig(Fo) and 0.0350 for all 1782 data REM 151 parameters refined using 0 restraints END WGHT 0.0273 3.3978 REM Highest difference peak 0.321, deepest hole -0.284, 1-sigma level 0.066 Q1 1 0.4458 0.5283 0.3854 11.00000 0.05 0.32 Q2 1 0.8772 0.7475 0.7730 11.00000 0.05 0.31 Q3 1 0.6274 0.6109 0.3585 11.00000 0.05 0.30 Q4 1 0.8239 0.7150 0.9408 11.00000 0.05 0.26 Q5 1 0.4997 0.5887 0.3716 11.00000 0.05 0.25 ; _shelx_res_checksum 67959 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Zn1 Zn 0.61821(2) 0.48838(4) 0.56788(2) 0.02089(11) Uani 1 1 d . . . S1 S 0.56827(5) 0.62485(8) 0.38828(4) 0.02163(17) Uani 1 1 d . . . O1 O 0.58763(15) 0.6418(2) 0.48114(11) 0.0341(5) Uani 1 1 d . . . O2 O 0.48028(15) 0.5231(2) 0.36758(12) 0.0316(5) Uani 1 1 d . . . O3 O 0.54083(13) 0.7936(2) 0.35948(11) 0.0239(4) Uani 1 1 d . . . O4 O 0.72872(13) 0.5522(2) 0.65023(11) 0.0260(5) Uani 1 1 d . . . O5 O 0.65775(14) 0.7746(2) 0.67833(12) 0.0295(5) Uani 1 1 d . . . N1 N 0.86113(16) 0.7651(3) 0.96613(13) 0.0215(5) Uani 1 1 d . . . N2 N 0.87467(15) 0.5912(3) 0.77023(13) 0.0237(5) Uani 1 1 d . . . H2A H 0.8589 0.4908 0.7794 0.036 Uiso 1 1 calc R U . H2B H 0.9218 0.6218 0.8092 0.036 Uiso 1 1 calc R U . H2C H 0.8917 0.5967 0.7223 0.036 Uiso 1 1 calc R U . N3 N 0.89271(18) 0.5418(3) 1.03332(14) 0.0294(6) Uani 1 1 d . . . H3 H 0.9168 0.4757 1.0709 0.035 Uiso 1 1 calc R U . C1 C 0.72120(18) 0.6757(3) 0.69269(15) 0.0196(6) Uani 1 1 d . . . C2 C 0.79423(18) 0.6981(3) 0.76999(15) 0.0194(6) Uani 1 1 d . . . H2 H 0.8157 0.8096 0.7728 0.023 Uiso 1 1 calc R U . C3 C 0.74743(19) 0.6651(3) 0.84211(15) 0.0222(6) Uani 1 1 d . . . H3A H 0.7062 0.7539 0.8470 0.027 Uiso 1 1 calc R U . H3B H 0.7093 0.5698 0.8301 0.027 Uiso 1 1 calc R U . C4 C 0.81093(18) 0.6418(3) 0.92194(15) 0.0205(6) Uani 1 1 d . . . C5 C 0.8307(2) 0.5045(3) 0.96428(17) 0.0290(7) Uani 1 1 d . . . H5 H 0.8065 0.4034 0.9492 0.035 Uiso 1 1 calc R U . C6 C 0.9095(2) 0.6976(3) 1.03237(17) 0.0275(7) Uani 1 1 d . . . H6 H 0.9499 0.7523 1.0729 0.033 Uiso 1 1 calc R U . O1W O 0.0000 0.3094(5) 0.7500 0.0727(12) Uani 1 2 d S T P H1W H 0.0355 0.2503 0.7282 0.087 Uiso 1 1 d R U . 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 Zn1 0.02515(19) 0.01761(18) 0.01752(18) -0.00039(13) -0.00159(13) 0.00141(14) S1 0.0227(4) 0.0202(4) 0.0220(4) 0.0000(3) 0.0043(3) 0.0029(3) O1 0.0511(14) 0.0263(12) 0.0200(10) 0.0067(9) -0.0048(10) 0.0033(10) O2 0.0368(12) 0.0272(12) 0.0327(12) -0.0068(9) 0.0114(10) -0.0116(9) O3 0.0280(10) 0.0213(10) 0.0202(10) 0.0037(8) -0.0008(8) -0.0003(9) O4 0.0268(11) 0.0255(11) 0.0221(10) -0.0081(8) -0.0040(8) 0.0014(9) O5 0.0309(11) 0.0246(11) 0.0297(11) -0.0005(9) -0.0017(9) 0.0071(9) N1 0.0282(13) 0.0200(12) 0.0158(12) 0.0020(9) 0.0034(10) -0.0025(10) N2 0.0217(12) 0.0283(14) 0.0200(12) -0.0012(10) 0.0010(10) -0.0011(11) N3 0.0399(15) 0.0279(14) 0.0183(12) 0.0096(10) 0.0007(11) 0.0031(12) C1 0.0228(14) 0.0189(14) 0.0172(14) -0.0001(11) 0.0040(11) -0.0065(12) C2 0.0202(14) 0.0178(14) 0.0194(14) -0.0018(11) 0.0020(11) -0.0021(11) C3 0.0209(14) 0.0255(15) 0.0200(14) -0.0012(11) 0.0038(12) -0.0037(12) C4 0.0228(14) 0.0207(15) 0.0192(14) -0.0010(11) 0.0073(11) -0.0007(12) C5 0.0441(19) 0.0195(15) 0.0233(15) -0.0003(12) 0.0065(14) -0.0054(14) C6 0.0350(17) 0.0252(16) 0.0202(15) 0.0015(12) 0.0007(13) -0.0041(13) O1W 0.052(2) 0.082(3) 0.095(3) 0.000 0.042(2) 0.000 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 O1 Zn1 O2 111.22(9) . 5_666 O1 Zn1 O4 112.68(9) . . O2 Zn1 O4 102.49(8) 5_666 . O1 Zn1 N1 115.53(9) . 4_646 O2 Zn1 N1 106.39(9) 5_666 4_646 O4 Zn1 N1 107.54(8) . 4_646 O3 S1 O2 106.49(11) . . O3 S1 O1 102.88(11) . . O2 S1 O1 105.12(12) . . S1 O1 Zn1 132.59(13) . . S1 O2 Zn1 125.46(12) . 5_666 C1 O4 Zn1 117.33(17) . . C6 N1 C4 105.9(2) . . C6 N1 Zn1 123.62(19) . 4_656 C4 N1 Zn1 129.32(17) . 4_656 C2 N2 H2A 109.5 . . C2 N2 H2B 109.5 . . H2A N2 H2B 109.5 . . C2 N2 H2C 109.5 . . H2A N2 H2C 109.5 . . H2B N2 H2C 109.5 . . C6 N3 C5 108.0(2) . . C6 N3 H3 126.0 . . C5 N3 H3 126.0 . . O5 C1 O4 125.4(2) . . O5 C1 C2 117.5(2) . . O4 C1 C2 117.0(2) . . N2 C2 C1 110.8(2) . . N2 C2 C3 111.8(2) . . C1 C2 C3 107.6(2) . . N2 C2 H2 108.8 . . C1 C2 H2 108.8 . . C3 C2 H2 108.8 . . C4 C3 C2 116.0(2) . . C4 C3 H3A 108.3 . . C2 C3 H3A 108.3 . . C4 C3 H3B 108.3 . . C2 C3 H3B 108.3 . . H3A C3 H3B 107.4 . . C5 C4 N1 108.1(2) . . C5 C4 C3 128.1(3) . . N1 C4 C3 123.8(2) . . C4 C5 N3 107.0(2) . . C4 C5 H5 126.5 . . N3 C5 H5 126.5 . . N1 C6 N3 111.0(3) . . N1 C6 H6 124.5 . . N3 C6 H6 124.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Zn1 O1 1.9246(19) . Zn1 O2 1.973(2) 5_666 Zn1 O4 1.9853(18) . Zn1 N1 1.989(2) 4_646 S1 O3 1.5169(19) . S1 O2 1.527(2) . S1 O1 1.536(2) . O2 Zn1 1.973(2) 5_666 O4 C1 1.270(3) . O5 C1 1.231(3) . N1 C6 1.322(3) . N1 C4 1.391(3) . N1 Zn1 1.989(2) 4_656 N2 C2 1.479(3) . N2 H2A 0.8900 . N2 H2B 0.8900 . N2 H2C 0.8900 . N3 C6 1.324(4) . N3 C5 1.362(4) . N3 H3 0.8600 . C1 C2 1.523(3) . C2 C3 1.531(4) . C2 H2 0.9800 . C3 C4 1.487(4) . C3 H3A 0.9700 . C3 H3B 0.9700 . C4 C5 1.349(4) . C5 H5 0.9300 . C6 H6 0.9300 . O1W H1W 0.8500 .