#------------------------------------------------------------------------------ #$Date: 2019-11-17 10:13:00 +0200 (Sun, 17 Nov 2019) $ #$Revision: 229283 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/78/7047842.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_7047842 loop_ _publ_author_name 'Lin, Wenxin' 'Cui, Yuanjing' 'Yang, Yu' 'Hu, Quan' 'Qian, Guodong' _publ_section_title ; A biocompatible metal-organic framework as a pH and temperature dual-responsive drug carrier. ; _journal_issue 44 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 15882 _journal_page_last 15887 _journal_paper_doi 10.1039/c8dt03202e _journal_volume 47 _journal_year 2018 _chemical_formula_sum 'C5 H11 N O6 Zn' _chemical_formula_weight 246.52 _chemical_name_systematic ZJU-129 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2013 _audit_update_record ; 2016-08-28 deposited with the CCDC. 2018-10-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.2283(4) _cell_length_b 10.4670(4) _cell_length_c 11.1858(7) _cell_measurement_reflns_used 6485 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.054 _cell_measurement_theta_min 2.664 _cell_volume 846.30(8) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_unetI/netI 0.0225 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 8907 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.095 _diffrn_reflns_theta_min 2.665 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 2.902 _exptl_crystal_density_diffrn 1.935 _exptl_crystal_description none _exptl_crystal_F_000 504 _refine_diff_density_max 0.262 _refine_diff_density_min -0.211 _refine_diff_density_rms 0.044 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.020(14) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 127 _refine_ls_number_reflns 1666 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.011 _refine_ls_R_factor_all 0.0169 _refine_ls_R_factor_gt 0.0160 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+0.0426P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.0433 _reflns_Friedel_coverage 0.690 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.997 _reflns_number_gt 1618 _reflns_number_total 1666 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8dt03202e2.cif _cod_data_source_block a _cod_depositor_comments 'Adding full bibliography for 7047842.cif.' _cod_database_code 7047842 _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. ; _shelxl_version_number 2013-2 _shelx_res_file ; TITL a in P2(1)2(1)2(1) New: P212121 CELL 0.71073 7.2283 10.4670 11.1858 90.000 90.000 90.000 ZERR 4 0.0004 0.0004 0.0007 0.000 0.000 0.000 LATT -1 SYMM 0.50000 - X , - Y , 0.50000 + Z SYMM 0.50000 + X , 0.50000 - Y , - Z SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC C H N O Zn UNIT 20 44 4 24 4 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! L.S. 5 FMAP 2 PLAN -20 ACTA BOND $H CONF TWIN WGHT 0.028300 0.042600 BASF 0.02004 FVAR 0.29559 ZN1 5 0.621978 0.571208 -0.459307 11.00000 0.02313 0.02410 = 0.02081 0.00114 0.00204 0.00032 H1 2 -0.413505 0.119745 -0.444569 11.00000 0.01946 O1 4 0.303887 0.459292 -0.446770 11.00000 0.03496 0.05239 = 0.02349 0.00424 0.00230 -0.00852 O1A 4 0.698024 0.381381 -0.479316 11.00000 0.03196 0.02406 = 0.06184 -0.00318 0.01311 -0.00264 AFIX 3 H3 2 0.651893 0.315821 -0.450476 11.00000 -1.50000 AFIX 0 O1M 4 0.141991 0.128407 -0.124355 11.00000 0.02578 0.02640 = 0.03223 -0.00254 -0.00321 0.00589 O2 4 0.022996 0.256144 0.015729 11.00000 0.03226 0.03147 = 0.02296 0.00007 -0.00336 0.00910 O20 4 0.483962 0.533850 -0.304303 11.00000 0.02682 0.03981 = 0.02807 0.00213 0.00537 -0.00887 N8 3 -0.181529 0.391375 -0.138722 11.00000 0.02407 0.03096 = 0.02354 0.00325 -0.00010 0.00613 AFIX 3 H2 2 -0.193599 0.468435 -0.166642 11.00000 -1.20000 H5 2 -0.297799 0.369955 -0.131212 11.00000 -1.20000 AFIX 0 H6 2 0.777917 0.363243 -0.508662 11.00000 0.05776 C2 1 0.213545 0.422901 -0.240784 11.00000 0.03089 0.03953 = 0.02133 0.00225 0.00318 -0.00819 AFIX 23 H2A 2 0.156590 0.494386 -0.199665 11.00000 -1.20000 H2B 2 0.288406 0.376896 -0.183109 11.00000 -1.20000 AFIX 0 C3 1 0.062479 0.334708 -0.286550 11.00000 0.02842 0.03100 = 0.01857 -0.00084 0.00211 -0.00069 AFIX 23 H3A 2 0.119738 0.261581 -0.324870 11.00000 -1.20000 H3B 2 -0.008964 0.379659 -0.346710 11.00000 -1.20000 AFIX 0 C4 1 0.039301 0.218673 -0.090220 11.00000 0.01786 0.01898 = 0.02723 0.00164 0.00063 -0.00356 C14 1 -0.068925 0.286959 -0.189237 11.00000 0.01936 0.02445 = 0.02079 -0.00080 -0.00039 -0.00122 AFIX 13 H14 2 -0.153241 0.224795 -0.225615 11.00000 -1.20000 AFIX 0 C19 1 0.338519 0.473981 -0.338881 11.00000 0.02562 0.02850 = 0.02559 0.00322 0.00416 0.00026 O3 4 -0.466235 0.152486 -0.413441 11.00000 0.03505 0.03431 = 0.03113 0.00255 0.00214 0.00521 AFIX 3 H4 2 -0.472504 0.115596 -0.335102 11.00000 -1.50000 REM ##### AFIX 0 HKLF 4 REM a in P2(1)2(1)2(1) New: P212121 REM R1 = 0.0160 for 1618 Fo > 4sig(Fo) and 0.0169 for all 1666 data REM 127 parameters refined using 0 restraints END WGHT 0.0235 0.0771 REM Highest difference peak 0.262, deepest hole -0.211, 1-sigma level 0.044 Q1 1 0.4946 0.5694 -0.4648 11.00000 0.05 0.26 Q2 1 -0.0066 0.2604 -0.1408 11.00000 0.05 0.25 Q3 1 0.6445 0.6015 -0.5367 11.00000 0.05 0.24 Q4 1 0.6282 0.6379 -0.4959 11.00000 0.05 0.23 Q5 1 0.6273 0.6251 -0.3956 11.00000 0.05 0.23 Q6 1 0.6239 0.4838 -0.4714 11.00000 0.05 0.22 Q7 1 0.7587 0.5743 -0.4614 11.00000 0.05 0.21 Q8 1 0.6177 0.5424 -0.5368 11.00000 0.05 0.20 Q9 1 -0.1927 0.4336 -0.2095 11.00000 0.05 0.20 Q10 1 0.4886 0.7548 -0.4326 11.00000 0.05 0.19 Q11 1 0.5835 0.5435 -0.3803 11.00000 0.05 0.18 Q12 1 -0.0252 0.3004 -0.2387 11.00000 0.05 0.17 Q13 1 0.4467 0.7383 -0.5402 11.00000 0.05 0.16 Q14 1 0.3850 0.7427 -0.4969 11.00000 0.05 0.16 Q15 1 -0.1160 0.3387 -0.1759 11.00000 0.05 0.15 Q16 1 0.2799 0.4364 -0.2941 11.00000 0.05 0.15 Q17 1 0.5104 0.7812 -0.5195 11.00000 0.05 0.15 Q18 1 0.1201 0.4068 -0.2688 11.00000 0.05 0.14 Q19 1 0.2136 0.4861 -0.4463 11.00000 0.05 0.13 Q20 1 0.4693 0.4811 -0.3373 11.00000 0.05 0.13 ; _shelx_res_checksum 76202 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, 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 Zn1 Zn 0.62198(4) 0.57121(3) -0.45931(2) 0.02268(10) Uani 1 1 d . . H1 H -0.414(4) 0.120(3) -0.445(3) 0.019(10) Uiso 1 1 d . . O1 O 0.3039(3) 0.4593(2) -0.44677(16) 0.0369(5) Uani 1 1 d . . O1A O 0.6980(3) 0.3814(2) -0.4793(2) 0.0393(5) Uani 1 1 d . . H3 H 0.6519 0.3158 -0.4505 0.059 Uiso 1 1 d R U O1M O 0.1420(3) 0.12841(16) -0.12436(16) 0.0281(4) Uani 1 1 d . . O2 O 0.0230(3) 0.25614(18) 0.01573(15) 0.0289(4) Uani 1 1 d . . O20 O 0.4840(3) 0.53385(17) -0.30430(16) 0.0316(4) Uani 1 1 d . . N8 N -0.1815(3) 0.3914(2) -0.13872(18) 0.0262(5) Uani 1 1 d . . H2 H -0.1936 0.4684 -0.1666 0.031 Uiso 1 1 d R U H5 H -0.2978 0.3700 -0.1312 0.031 Uiso 1 1 d R U H6 H 0.778(5) 0.363(4) -0.509(4) 0.058(14) Uiso 1 1 d . . C2 C 0.2135(4) 0.4229(3) -0.2408(2) 0.0306(6) Uani 1 1 d . . H2A H 0.1566 0.4944 -0.1997 0.037 Uiso 1 1 calc R U H2B H 0.2884 0.3769 -0.1831 0.037 Uiso 1 1 calc R U C3 C 0.0625(4) 0.3347(2) -0.2865(2) 0.0260(6) Uani 1 1 d . . H3A H 0.1197 0.2616 -0.3249 0.031 Uiso 1 1 calc R U H3B H -0.0090 0.3797 -0.3467 0.031 Uiso 1 1 calc R U C4 C 0.0393(4) 0.2187(2) -0.0902(2) 0.0214(5) Uani 1 1 d . . C14 C -0.0689(3) 0.2870(2) -0.1892(2) 0.0215(5) Uani 1 1 d . . H14 H -0.1532 0.2248 -0.2256 0.026 Uiso 1 1 calc R U C19 C 0.3385(4) 0.4740(2) -0.3389(2) 0.0266(6) Uani 1 1 d . . O3 O -0.4662(3) 0.1525(2) -0.4134(2) 0.0335(5) Uani 1 1 d . . H4 H -0.4725 0.1156 -0.3351 0.050 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 0.02313(16) 0.02410(14) 0.02081(15) 0.00114(11) 0.00204(12) 0.00032(12) O1 0.0350(10) 0.0524(13) 0.0235(10) 0.0042(8) 0.0023(8) -0.0085(9) O1A 0.0320(11) 0.0241(9) 0.0618(15) -0.0032(10) 0.0131(12) -0.0026(9) O1M 0.0258(10) 0.0264(8) 0.0322(9) -0.0025(7) -0.0032(9) 0.0059(8) O2 0.0323(10) 0.0315(9) 0.0230(9) 0.0001(7) -0.0034(8) 0.0091(8) O20 0.0268(10) 0.0398(10) 0.0281(10) 0.0021(8) 0.0054(8) -0.0089(8) N8 0.0241(11) 0.0310(11) 0.0235(10) 0.0032(8) -0.0001(9) 0.0061(8) C2 0.0309(14) 0.0395(14) 0.0213(12) 0.0023(12) 0.0032(11) -0.0082(14) C3 0.0284(14) 0.0310(12) 0.0186(11) -0.0008(10) 0.0021(10) -0.0007(11) C4 0.0179(12) 0.0190(10) 0.0272(12) 0.0016(10) 0.0006(10) -0.0036(10) C14 0.0194(12) 0.0244(11) 0.0208(11) -0.0008(10) -0.0004(9) -0.0012(10) C19 0.0256(16) 0.0285(12) 0.0256(13) 0.0032(10) 0.0042(10) 0.0003(10) O3 0.0351(12) 0.0343(11) 0.0311(11) 0.0025(9) 0.0021(10) 0.0052(10) 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' 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 O1M Zn1 O20 94.33(7) 4_654 . O1M Zn1 O1A 96.27(8) 4_654 . O20 Zn1 O1A 92.16(9) . . O1M Zn1 N8 102.34(8) 4_654 2_564 O20 Zn1 N8 162.51(8) . 2_564 O1A Zn1 N8 91.22(9) . 2_564 O1M Zn1 O2 103.03(7) 4_654 2_564 O20 Zn1 O2 91.94(7) . 2_564 O1A Zn1 O2 159.90(9) . 2_564 N8 Zn1 O2 79.31(7) 2_564 2_564 Zn1 O1A H3 130.2 . . Zn1 O1A H6 122(4) . . H3 O1A H6 107.1 . . C4 O1M Zn1 125.07(16) . 4_644 C4 O2 Zn1 116.12(15) . 2_565 C19 O20 Zn1 103.78(15) . . C14 N8 Zn1 113.15(15) . 2_565 C14 N8 H2 127.2 . . Zn1 N8 H2 101.1 2_565 . C14 N8 H5 112.2 . . Zn1 N8 H5 98.9 2_565 . H2 N8 H5 100.1 . . C19 C2 C3 113.5(2) . . C19 C2 H2A 108.9 . . C3 C2 H2A 108.9 . . C19 C2 H2B 108.9 . . C3 C2 H2B 108.9 . . H2A C2 H2B 107.7 . . C2 C3 C14 113.9(2) . . C2 C3 H3A 108.8 . . C14 C3 H3A 108.8 . . C2 C3 H3B 108.8 . . C14 C3 H3B 108.8 . . H3A C3 H3B 107.7 . . O2 C4 O1M 125.2(2) . . O2 C4 C14 119.3(2) . . O1M C4 C14 115.5(2) . . N8 C14 C3 111.92(19) . . N8 C14 C4 110.50(19) . . C3 C14 C4 110.48(19) . . N8 C14 H14 107.9 . . C3 C14 H14 107.9 . . C4 C14 H14 107.9 . . O1 C19 O20 121.2(2) . . O1 C19 C2 122.6(2) . . O20 C19 C2 116.2(2) . . H1 O3 H4 108.7 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Zn1 O1M 2.0359(18) 4_654 Zn1 O20 2.0382(18) . Zn1 O1A 2.074(2) . Zn1 N8 2.090(2) 2_564 Zn1 O2 2.1076(18) 2_564 O1 C19 1.242(3) . O1A H3 0.8283 . O1A H6 0.69(4) . O1M C4 1.261(3) . O1M Zn1 2.0359(18) 4_644 O2 C4 1.254(3) . O2 Zn1 2.1076(18) 2_565 O20 C19 1.284(3) . N8 C14 1.475(3) . N8 Zn1 2.090(2) 2_565 N8 H2 0.8693 . N8 H5 0.8739 . C2 C19 1.519(3) . C2 C3 1.519(4) . C2 H2A 0.9700 . C2 H2B 0.9700 . C3 C14 1.529(3) . C3 H3A 0.9700 . C3 H3B 0.9700 . C4 C14 1.533(3) . C14 H14 0.9800 . O3 H1 0.62(3) . O3 H4 0.9587 . 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 _geom_torsion_site_symmetry_1 C19 C2 C3 C14 -177.7(2) . Zn1 O2 C4 O1M 169.59(19) 2_565 Zn1 O2 C4 C14 -9.2(3) 2_565 Zn1 O1M C4 O2 -27.3(4) 4_644 Zn1 O1M C4 C14 151.54(16) 4_644 Zn1 N8 C14 C3 -114.07(18) 2_565 Zn1 N8 C14 C4 9.5(2) 2_565 C2 C3 C14 N8 66.8(3) . C2 C3 C14 C4 -56.8(3) . O2 C4 C14 N8 -0.3(3) . O1M C4 C14 N8 -179.2(2) . O2 C4 C14 C3 124.1(2) . O1M C4 C14 C3 -54.8(3) . Zn1 O20 C19 O1 -4.9(3) . Zn1 O20 C19 C2 175.07(19) . C3 C2 C19 O1 9.6(4) . C3 C2 C19 O20 -170.3(2) .