#------------------------------------------------------------------------------ #$Date: 2020-11-06 14:21:51 +0200 (Fri, 06 Nov 2020) $ #$Revision: 258859 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705322.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_7705322 loop_ _publ_author_name 'Adhikary, Amit' 'Das, Krishna Sundar' 'Saha, Sayan' 'Roy, Manasi' 'Mondal, Raju' _publ_section_title ; A free-standing, self-healing multi-stimuli responsive gel showing cryogenic magnetic cooling. ; _journal_issue 38 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 13487 _journal_page_last 13495 _journal_paper_doi 10.1039/d0dt02356f _journal_volume 49 _journal_year 2020 _chemical_formula_sum 'C14 H6 Fe2 N2 O13' _chemical_formula_weight 521.91 _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' _atom_sites_solution_hydrogens mixed _audit_block_doi 10.5517/ccdc.csd.cc20nlx6 _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2019-03-13 deposited with the CCDC. 2020-08-31 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.2220(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.3826(3) _cell_length_b 21.6960(9) _cell_length_c 7.4517(3) _cell_measurement_reflns_used 4500 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 30.45 _cell_measurement_theta_min 3.34 _cell_volume 1840.23(12) _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0038 _diffrn_reflns_av_unetI/netI 0.0039 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 4190 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.445 _diffrn_reflns_theta_min 1.877 _exptl_absorpt_coefficient_mu 1.653 _exptl_crystal_colour Orange _exptl_crystal_density_diffrn 1.884 _exptl_crystal_description Block _exptl_crystal_F_000 1040 _refine_diff_density_max 0.339 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.056 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 145 _refine_ls_number_reflns 2102 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.015 _refine_ls_R_factor_all 0.0207 _refine_ls_R_factor_gt 0.0203 _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^)+(0.0275P)^2^+3.1525P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.0573 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2060 _reflns_number_total 2102 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02356f2.cif _cod_data_source_block Complex_1 _cod_depositor_comments 'Adding full bibliography for 7705322.cif.' _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 7705322 _shelx_shelxl_version_number 2016/6 _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_res_file ; TITL MONO11_b.res in Cc New: C2/c mono.res created by SHELXL-2016/6 at 22:37:46 on 27-Feb-2019 CELL 0.71073 11.3826 21.696 7.4517 90 90.222 90 ZERR 4 0.0003 0.0009 0.0003 0 0.001 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Fe N O UNIT 56 24 8 8 52 REM REM REM L.S. 50 ACTA BOND $H FMAP 2 PLAN -20 CONF WGHT 0.027469 3.152540 FVAR 7.96286 FE1 3 0.132108 0.130749 0.790719 11.00000 0.01770 0.01192 = 0.02844 -0.00048 0.00842 0.00129 O1 5 0.165255 0.223165 0.811355 11.00000 0.02608 0.01244 = 0.02721 -0.00078 0.00430 0.00309 O2 5 0.286880 0.300444 0.734171 11.00000 0.03909 0.01129 = 0.02904 0.00118 -0.00699 -0.00323 O3 5 0.183558 0.041866 0.717125 11.00000 0.01929 0.01281 = 0.04181 -0.00375 0.01231 -0.00042 O4 5 0.326117 -0.014737 0.591651 11.00000 0.02032 0.01476 = 0.05457 -0.01220 0.00983 -0.00009 O5 5 0.212822 0.114434 1.024861 11.00000 0.03147 0.02095 = 0.02783 0.00025 0.00341 0.00967 AFIX 7 H5A 2 0.172298 0.129624 1.109795 11.00000 -1.50000 H5B 2 0.277315 0.134226 1.028749 11.00000 -1.50000 AFIX 0 O6 5 0.020745 0.132360 0.587041 11.00000 0.01796 0.02326 = 0.02705 -0.00311 0.00775 -0.00183 N1 4 0.289407 0.142819 0.657593 11.00000 0.01408 0.01408 = 0.02108 -0.00160 0.00282 -0.00221 C1 1 0.332798 0.199375 0.642749 11.00000 0.01798 0.01320 = 0.02048 0.00229 -0.00292 -0.00285 C2 1 0.436182 0.210253 0.552307 11.00000 0.01975 0.02089 = 0.02664 0.00585 -0.00431 -0.00536 AFIX 43 H2 2 0.465611 0.249988 0.539406 11.00000 -1.20000 AFIX 0 C3 1 0.494795 0.159798 0.481183 11.00000 0.01556 0.03037 = 0.02448 0.00709 0.00369 -0.00466 AFIX 43 H3 2 0.564365 0.165717 0.418459 11.00000 -1.20000 AFIX 0 C4 1 0.450446 0.100236 0.502774 11.00000 0.01420 0.02231 = 0.02921 -0.00356 0.00347 0.00002 AFIX 43 H4 2 0.490160 0.066134 0.457867 11.00000 -1.20000 AFIX 0 C5 1 0.345817 0.093849 0.592941 11.00000 0.01725 0.01316 = 0.02367 -0.00393 0.00201 -0.00151 C6 1 0.257063 0.245716 0.736105 11.00000 0.02547 0.01348 = 0.01943 0.00082 -0.00506 0.00051 C7 1 0.281125 0.034793 0.635730 11.00000 0.01697 0.01454 = 0.03169 -0.00681 0.00650 -0.00291 AFIX 6 O13 5 1.000000 0.058002 0.250000 10.50000 0.05349 0.04214 = 0.06017 0.00000 0.01691 0.00000 H13 2 0.942341 0.082827 0.243912 10.50000 -1.50000 AFIX 0 HKLF 4 REM MONO11_b.res in Cc New: C2/c REM R1 = 0.0203 for 2060 Fo > 4sig(Fo) and 0.0207 for all 2102 data REM 145 parameters refined using 0 restraints END WGHT 0.0286 2.0118 REM Highest difference peak 0.339, deepest hole -0.773, 1-sigma level 0.056 Q1 1 0.0556 -0.0333 0.7616 11.00000 0.05 0.34 Q2 1 -0.0459 0.1209 0.8484 11.00000 0.05 0.11 Q3 1 -0.0214 0.1139 0.9875 11.00000 0.05 0.11 Q4 1 0.3925 0.2006 0.6114 11.00000 0.05 0.11 Q5 1 0.4997 0.2586 0.4435 11.00000 0.05 0.11 Q6 1 0.1046 0.1350 0.7462 11.00000 0.05 0.10 Q7 1 0.2745 0.2793 0.6762 11.00000 0.05 0.10 Q8 1 0.2747 0.1602 0.7222 11.00000 0.05 0.09 Q9 1 0.3493 0.2928 0.6955 11.00000 0.05 0.09 Q10 1 0.1233 0.1391 0.8315 11.00000 0.05 0.09 Q11 1 0.5499 0.1880 0.3342 11.00000 0.05 0.09 Q12 1 0.5482 0.0784 0.4050 11.00000 0.05 0.09 Q13 1 -0.0348 0.1699 0.8396 11.00000 0.05 0.09 Q14 1 0.1486 0.0218 0.6421 11.00000 0.05 0.09 Q15 1 0.4968 0.2172 0.4746 11.00000 0.05 0.09 Q16 1 0.1821 0.0440 0.7754 11.00000 0.05 0.08 Q17 1 0.0191 0.0208 0.8974 11.00000 0.05 0.08 Q18 1 0.0000 0.2065 0.7500 10.50000 0.05 0.08 Q19 1 0.4491 0.0884 0.4020 11.00000 0.05 0.08 Q20 1 0.4392 0.0397 0.5782 11.00000 0.05 0.08 ; _shelx_res_checksum 54267 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 _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.13211(2) 0.13075(2) 0.79072(3) 0.01933(8) Uani 1 1 d . . . . . O1 O 0.16525(10) 0.22317(5) 0.81136(14) 0.0219(2) Uani 1 1 d . . . . . O2 O 0.28688(11) 0.30044(5) 0.73417(15) 0.0265(2) Uani 1 1 d . . . . . O3 O 0.18356(9) 0.04187(5) 0.71712(16) 0.0246(2) Uani 1 1 d . . . . . O4 O 0.32612(10) -0.01474(5) 0.59165(18) 0.0299(3) Uani 1 1 d . . . . . O5 O 0.21282(11) 0.11443(5) 1.02486(15) 0.0267(2) Uani 1 1 d . . . . . H5A H 0.172298 0.129624 1.109795 0.040 Uiso 1 1 d R U . . . H5B H 0.277315 0.134226 1.028749 0.040 Uiso 1 1 d R U . . . O6 O 0.02074(9) 0.13236(5) 0.58704(15) 0.0227(2) Uani 1 1 d . . . . . N1 N 0.28941(10) 0.14282(5) 0.65759(16) 0.0164(2) Uani 1 1 d . . . . . C1 C 0.33280(12) 0.19938(6) 0.64275(19) 0.0172(3) Uani 1 1 d . . . . . C2 C 0.43618(13) 0.21025(7) 0.5523(2) 0.0224(3) Uani 1 1 d . . . . . H2 H 0.465611 0.249988 0.539406 0.027 Uiso 1 1 calc R U . . . C3 C 0.49479(13) 0.15980(8) 0.4812(2) 0.0235(3) Uani 1 1 d . . . . . H3 H 0.564365 0.165717 0.418459 0.028 Uiso 1 1 calc R U . . . C4 C 0.45045(12) 0.10024(7) 0.5028(2) 0.0219(3) Uani 1 1 d . . . . . H4 H 0.490160 0.066134 0.457867 0.026 Uiso 1 1 calc R U . . . C5 C 0.34582(12) 0.09385(6) 0.59294(19) 0.0180(3) Uani 1 1 d . . . . . C6 C 0.25706(13) 0.24572(6) 0.73611(19) 0.0195(3) Uani 1 1 d . . . . . C7 C 0.28113(12) 0.03479(7) 0.6357(2) 0.0211(3) Uani 1 1 d . . . . . O13 O 1.000000 0.05800(11) 0.250000 0.0519(5) Uani 1 2 d GS T P . . H13 H 0.942341 0.082827 0.243912 0.078 Uiso 0.5 1 d G U P . . 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 Fe1 0.01770(12) 0.01192(11) 0.02844(13) -0.00048(7) 0.00842(8) 0.00129(7) O1 0.0261(5) 0.0124(5) 0.0272(5) -0.0008(4) 0.0043(4) 0.0031(4) O2 0.0391(6) 0.0113(5) 0.0290(6) 0.0012(4) -0.0070(5) -0.0032(4) O3 0.0193(5) 0.0128(5) 0.0418(6) -0.0037(4) 0.0123(4) -0.0004(4) O4 0.0203(5) 0.0148(5) 0.0546(8) -0.0122(5) 0.0098(5) -0.0001(4) O5 0.0315(6) 0.0209(5) 0.0278(6) 0.0003(4) 0.0034(5) 0.0097(5) O6 0.0180(5) 0.0233(5) 0.0271(5) -0.0031(4) 0.0078(4) -0.0018(4) N1 0.0141(5) 0.0141(5) 0.0211(6) -0.0016(4) 0.0028(4) -0.0022(4) C1 0.0180(6) 0.0132(6) 0.0205(6) 0.0023(5) -0.0029(5) -0.0029(5) C2 0.0198(7) 0.0209(7) 0.0266(7) 0.0058(6) -0.0043(6) -0.0054(5) C3 0.0156(6) 0.0304(8) 0.0245(7) 0.0071(6) 0.0037(5) -0.0047(6) C4 0.0142(6) 0.0223(7) 0.0292(7) -0.0036(6) 0.0035(5) 0.0000(5) C5 0.0172(6) 0.0132(6) 0.0237(7) -0.0039(5) 0.0020(5) -0.0015(5) C6 0.0255(7) 0.0135(6) 0.0194(6) 0.0008(5) -0.0051(5) 0.0005(5) C7 0.0170(6) 0.0145(6) 0.0317(8) -0.0068(5) 0.0065(5) -0.0029(5) O13 0.0535(14) 0.0421(12) 0.0602(14) 0.000 0.0169(11) 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' Fe Fe 0.3463 0.8444 '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' loop_ _citation_id _citation_doi _citation_year 1 10.1021/acsomega.8b03400 2019 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 _geom_angle_publ_flag O6 Fe1 O6 77.83(5) 2_556 . ? O6 Fe1 O5 90.19(5) 2_556 . ? O6 Fe1 O5 164.84(5) . . ? O6 Fe1 O1 96.37(4) 2_556 . ? O6 Fe1 O1 99.10(4) . . ? O5 Fe1 O1 91.37(5) . . ? O6 Fe1 N1 171.59(5) 2_556 . ? O6 Fe1 N1 100.58(5) . . ? O5 Fe1 N1 92.59(5) . . ? O1 Fe1 N1 75.64(4) . . ? O6 Fe1 O3 112.78(4) 2_556 . ? O6 Fe1 O3 89.68(5) . . ? O5 Fe1 O3 86.41(5) . . ? O1 Fe1 O3 150.75(4) . . ? N1 Fe1 O3 75.33(4) . . ? C6 O1 Fe1 119.37(9) . . ? C7 O3 Fe1 118.74(9) . . ? Fe1 O5 H5A 109.4 . . ? Fe1 O5 H5B 109.5 . . ? H5A O5 H5B 104.4 . . ? Fe1 O6 Fe1 102.13(5) 2_556 . ? C1 N1 C5 121.80(12) . . ? C1 N1 Fe1 118.71(10) . . ? C5 N1 Fe1 119.47(9) . . ? N1 C1 C2 121.16(13) . . ? N1 C1 C6 111.52(12) . . ? C2 C1 C6 127.31(13) . . ? C1 C2 C3 117.65(13) . . ? C1 C2 H2 121.2 . . ? C3 C2 H2 121.2 . . ? C2 C3 C4 120.74(14) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 117.58(14) . . ? C5 C4 H4 121.2 . . ? C3 C4 H4 121.2 . . ? N1 C5 C4 121.01(13) . . ? N1 C5 C7 111.32(12) . . ? C4 C5 C7 127.66(13) . . ? O2 C6 O1 126.53(14) . . ? O2 C6 C1 118.77(14) . . ? O1 C6 C1 114.69(12) . . ? O4 C7 O3 126.38(14) . . ? O4 C7 C5 118.57(13) . . ? O3 C7 C5 115.05(12) . . ? H13 O13 H13 101.4 . 2_755 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O6 1.9673(11) 2_556 ? Fe1 O6 1.9740(12) . ? Fe1 O5 2.0003(12) . ? Fe1 O1 2.0459(10) . ? Fe1 N1 2.0669(12) . ? Fe1 O3 2.0893(10) . ? O1 C6 1.2847(19) . ? O2 C6 1.2350(18) . ? O3 C7 1.2767(17) . ? O4 C7 1.2354(18) . ? O5 H5A 0.8510 . ? O5 H5B 0.8509 . ? N1 C1 1.3275(17) . ? N1 C5 1.3325(18) . ? C1 C2 1.379(2) . ? C1 C6 1.498(2) . ? C2 C3 1.388(2) . ? C2 H2 0.9300 . ? C3 C4 1.397(2) . ? C3 H3 0.9300 . ? C4 C5 1.3767(19) . ? C4 H4 0.9300 . ? C5 C7 1.5124(19) . ? O13 H13 0.8501 . ? O13 H13 0.85(6) 2_755 ? 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 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C1 C2 2.9(2) . . . . ? Fe1 N1 C1 C2 -178.71(10) . . . . ? C5 N1 C1 C6 -176.32(12) . . . . ? Fe1 N1 C1 C6 2.06(15) . . . . ? N1 C1 C2 C3 -1.6(2) . . . . ? C6 C1 C2 C3 177.53(13) . . . . ? C1 C2 C3 C4 -0.6(2) . . . . ? C2 C3 C4 C5 1.5(2) . . . . ? C1 N1 C5 C4 -2.0(2) . . . . ? Fe1 N1 C5 C4 179.66(11) . . . . ? C1 N1 C5 C7 177.01(13) . . . . ? Fe1 N1 C5 C7 -1.36(16) . . . . ? C3 C4 C5 N1 -0.2(2) . . . . ? C3 C4 C5 C7 -179.03(14) . . . . ? Fe1 O1 C6 O2 178.43(11) . . . . ? Fe1 O1 C6 C1 -1.46(16) . . . . ? N1 C1 C6 O2 179.70(13) . . . . ? C2 C1 C6 O2 0.5(2) . . . . ? N1 C1 C6 O1 -0.40(17) . . . . ? C2 C1 C6 O1 -179.58(13) . . . . ? Fe1 O3 C7 O4 176.19(13) . . . . ? Fe1 O3 C7 C5 -3.22(18) . . . . ? N1 C5 C7 O4 -176.52(14) . . . . ? C4 C5 C7 O4 2.4(2) . . . . ? N1 C5 C7 O3 2.94(19) . . . . ? C4 C5 C7 O3 -178.17(15) . . . . ?