#------------------------------------------------------------------------------ #$Date: 2021-10-14 04:56:50 +0300 (Thu, 14 Oct 2021) $ #$Revision: 269932 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/49/1564913.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_1564913 loop_ _publ_author_name 'Bara, Dominic' 'Meekel, Emily' 'Pakamore, Ignas' 'Wilson, Claire' 'Ling, Sanliang' 'Forgan, Ross S.' _publ_section_title ; Exploring and Expanding the Fe-Terephthalate Metal-Organic Framework Phase Space by Coordination and Oxidation Modulation ; _journal_name_full 'Materials Horizons' _journal_paper_doi 10.1039/D1MH01663F _journal_year 2021 _chemical_formula_moiety 'C11 H11 Fe N O5' _chemical_formula_sum 'C11 H11 Fe N O5' _chemical_formula_weight 293.06 _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' _space_group_name_H-M_alt 'P n m a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_block_doi 10.5517/ccdc.csd.cc28391r _audit_creation_date 2019-09-05 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-06-07 deposited with the CCDC. 2021-10-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.4334(19) _cell_length_b 7.2431(7) _cell_length_c 8.7675(9) _cell_measurement_reflns_used 9927 _cell_measurement_temperature 150 _cell_measurement_theta_max 28.30 _cell_measurement_theta_min 2.55 _cell_volume 1234.1(2) _computing_cell_refinement 'SAINT V8.37A (Bruker-AXS, 2016)' _computing_data_collection 'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)' _computing_data_reduction 'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 150 _diffrn_detector 'charge integrating pixel array detector' _diffrn_detector_area_resol_mean 7.4074 _diffrn_detector_type 'Bruker PHOTON II' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_collimation 'focusing mirrors' _diffrn_radiation_monochromator 'multilayer mirror optics' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_unetI/netI 0.0149 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 24397 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.303 _diffrn_reflns_theta_min 2.549 _diffrn_source 'microfocus sealed tube' _diffrn_source_type 'INCOATEC I\ms 3.0' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.233 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.7001 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0685 before and 0.0509 after correction. The Ratio of minimum to maximum transmission is 0.9388. The \l/2 correction factor is Not present.' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.577 _exptl_crystal_description block _exptl_crystal_F_000 600 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.700 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.072 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 99 _refine_ls_number_reflns 1654 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.120 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0323 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+1.0827P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0939 _refine_ls_wR_factor_ref 0.0967 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1477 _reflns_number_total 1654 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1mh01663f2.cif _cod_data_source_block FeDMFBDC _cod_database_code 1564913 _shelx_shelxl_version_number 2018/3 _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_max 0.964 _shelx_estimated_absorpt_t_min 0.908 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances N3S-C4S 1.454 with sigma of 0.02 N3S-C2S 1.346 with sigma of 0.02 O1S-C2S 1.254 with sigma of 0.02 3. Others Fixed Sof: H4SA(0.5) H4SB(0.5) H4SC(0.5) H5SA(0.5) H5SB(0.5) H5SC(0.5) 4.a Aromatic/amide H refined with riding coordinates: C2S(H2S), C3(H3), C4(H4) 4.b Idealised Me refined as rotating group: C4S(H4SA,H4SB,H4SC), C5S(H5SA,H5SB,H5SC) ; _shelx_res_file ; TITL mo_djb_07_10g_150k_0m_a.res in Pnma mo_djb_07_10g_150k_0m.res created by SHELXL-2018/3 at 09:37:34 on 05-Sep-2019 REM Old TITL mo_DJB_07_10g_150K_0m in P2(1)2(1)2(1) REM SHELXT solution in Pnma REM R1 0.076, Rweak 0.001, Alpha 0.016, Orientation a'=c, b'=a, c'=b REM Formula found by SHELXT: C12 O5 Fe CELL 0.71073 19.4334 7.2431 8.7675 90 90 90 ZERR 4 0.0019 0.0007 0.0009 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,-Z SYMM 0.5+X,0.5-Y,0.5-Z SFAC C H Fe N O UNIT 44 44 4 4 20 DFIX 1.454 N3S C4S DFIX 1.346 N3S C2S DFIX 1.254 O1S C2S L.S. 4 0 0 PLAN 20 SIZE 0.03 0.07 0.08 TEMP -123.15 BOND $H list 4 fmap 2 53 ACTA REM REM REM WGHT 0.048200 1.082700 FVAR 0.55329 FE1 3 0.500000 0.500000 0.500000 10.50000 0.00626 0.01130 = 0.01157 -0.00116 0.00033 -0.00053 O1S 5 0.495513 0.750000 0.361139 10.50000 0.02088 0.01294 = 0.01287 0.00000 0.00106 0.00000 O1 5 0.583483 0.595525 0.621102 11.00000 0.01293 0.01856 = 0.02738 0.00025 -0.00824 -0.00248 O2 5 0.926120 0.904455 0.844028 11.00000 0.01485 0.01922 = 0.02669 -0.00040 -0.01015 -0.00250 N3S 4 0.492836 0.750000 0.102367 10.50000 0.04019 0.02545 = 0.01436 0.00000 -0.00177 0.00000 C1 1 0.611354 0.750000 0.638671 10.50000 0.01009 0.01899 = 0.01461 0.00000 -0.00348 0.00000 C6 1 0.897809 0.750000 0.826368 10.50000 0.01110 0.01828 = 0.01358 0.00000 -0.00450 0.00000 C5 1 0.823501 0.750000 0.777274 10.50000 0.01104 0.01714 = 0.01935 0.00000 -0.00591 0.00000 C2 1 0.685777 0.750000 0.687946 10.50000 0.01113 0.01687 = 0.01890 0.00000 -0.00464 0.00000 C2S 1 0.524445 0.750000 0.232483 10.50000 0.03250 0.01665 = 0.02144 0.00000 0.00034 0.00000 AFIX 43 H2S 2 0.573324 0.750000 0.230774 10.50000 -1.20000 AFIX 0 C3 1 0.720360 0.914767 0.709330 11.00000 0.01640 0.01531 = 0.05670 0.00008 -0.01398 0.00289 AFIX 43 H3 2 0.697142 1.028491 0.693038 11.00000 -1.20000 AFIX 0 C4 1 0.789026 0.914964 0.754607 11.00000 0.01588 0.01453 = 0.05764 -0.00297 -0.01379 -0.00216 AFIX 43 H4 2 0.812314 1.028768 0.770008 11.00000 -1.20000 AFIX 0 C4S 1 0.417355 0.750000 0.096268 10.50000 0.04150 0.06205 = 0.03258 0.00000 -0.01285 0.00000 PART -1 AFIX 137 H4SA 2 0.398934 0.794699 0.193548 10.50000 -1.50000 H4SB 2 0.400842 0.624182 0.077551 10.50000 -1.50000 H4SC 2 0.401893 0.831119 0.013634 10.50000 -1.50000 AFIX 0 PART 0 C5S 1 0.528327 0.750000 -0.043288 10.50000 0.07002 0.04117 = 0.01838 0.00000 0.00574 0.00000 PART -1 AFIX 137 H5SA 2 0.522908 0.870835 -0.092120 10.50000 -1.50000 H5SB 2 0.508700 0.654179 -0.109129 10.50000 -1.50000 H5SC 2 0.577336 0.724986 -0.026963 10.50000 -1.50000 AFIX 0 HKLF 4 REM mo_djb_07_10g_150k_0m_a.res in Pnma REM wR2 = 0.096712, GooF = S = 1.11899, Restrained GooF = 1.12025 for all data REM R1 = 0.032263 for 1477 Fo > 4sig(Fo) and 0.035712 for all 1654 data REM 99 parameters refined using 3 restraints END WGHT 0.0461 1.0891 REM Highest difference peak 0.700, deepest hole -0.374, 1-sigma level 0.072 Q1 1 0.4743 0.7500 0.2342 10.50000 0.05 0.70 Q2 1 0.5853 0.7500 0.1129 10.50000 0.05 0.69 Q3 1 0.8575 0.7500 0.7981 10.50000 0.05 0.50 Q4 1 0.4744 0.7500 -0.0402 10.50000 0.05 0.48 Q5 1 0.6492 0.7500 0.6621 10.50000 0.05 0.43 Q6 1 0.6987 0.8272 0.7111 11.00000 0.05 0.39 Q7 1 0.7985 0.8313 0.7938 11.00000 0.05 0.38 Q8 1 0.7580 0.9039 0.7292 11.00000 0.05 0.32 Q9 1 0.5123 0.3987 0.4967 11.00000 0.05 0.32 Q10 1 0.5796 0.6619 0.6545 11.00000 0.05 0.32 Q11 1 0.9169 0.8414 0.8620 11.00000 0.05 0.31 Q12 1 0.5087 0.7500 0.3326 10.50000 0.05 0.28 Q13 1 0.5051 0.5338 0.4077 11.00000 0.05 0.25 Q14 1 0.5803 0.5613 0.6741 11.00000 0.05 0.22 Q15 1 0.5938 0.5433 0.6553 11.00000 0.05 0.22 Q16 1 0.9050 0.9393 0.8854 11.00000 0.05 0.22 Q17 1 0.4608 0.7500 0.3691 10.50000 0.05 0.22 Q18 1 0.7002 1.0072 0.6211 11.00000 0.05 0.19 Q19 1 0.5178 0.7500 0.1302 10.50000 0.05 0.18 Q20 1 0.5027 0.8282 0.1520 11.00000 0.05 0.18 ; _shelx_res_checksum 14241 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -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 0.500000 0.500000 0.500000 0.00971(13) Uani 1 2 d S T P . . O1S O 0.49551(7) 0.750000 0.3611(2) 0.0156(3) Uani 1 2 d DS T P . . O1 O 0.58348(6) 0.59553(16) 0.62110(14) 0.0196(3) Uani 1 1 d . . . . . O2 O 0.92612(6) 0.90446(16) 0.84403(14) 0.0203(3) Uani 1 1 d . . . . . N3S N 0.49284(12) 0.750000 0.1024(3) 0.0267(5) Uani 1 2 d DS T P . . C1 C 0.61135(11) 0.750000 0.6387(2) 0.0146(4) Uani 1 2 d S T P . . C6 C 0.89781(11) 0.750000 0.8264(2) 0.0143(4) Uani 1 2 d S T P . . C5 C 0.82350(11) 0.750000 0.7773(3) 0.0158(4) Uani 1 2 d S T P . . C2 C 0.68578(11) 0.750000 0.6879(3) 0.0156(4) Uani 1 2 d S T P . . C2S C 0.52445(15) 0.750000 0.2325(3) 0.0235(5) Uani 1 2 d DS T P . . H2S H 0.573324 0.750000 0.230774 0.028 Uiso 1 2 calc RS T P . . C3 C 0.72036(9) 0.9148(2) 0.7093(3) 0.0295(4) Uani 1 1 d . . . . . H3 H 0.697142 1.028491 0.693038 0.035 Uiso 1 1 calc R . . . . C4 C 0.78903(9) 0.9150(2) 0.7546(3) 0.0294(4) Uani 1 1 d . . . . . H4 H 0.812314 1.028768 0.770008 0.035 Uiso 1 1 calc R . . . . C4S C 0.41735(17) 0.750000 0.0963(4) 0.0454(8) Uani 1 2 d DS T P . . H4SA H 0.398934 0.794699 0.193548 0.068 Uiso 0.5 1 calc GR . . A -1 H4SB H 0.400842 0.624182 0.077551 0.068 Uiso 0.5 1 calc GR . . A -1 H4SC H 0.401893 0.831119 0.013634 0.068 Uiso 0.5 1 calc GR . . A -1 C5S C 0.5283(2) 0.750000 -0.0433(4) 0.0432(8) Uani 1 2 d S T P . . H5SA H 0.522908 0.870835 -0.092120 0.065 Uiso 0.5 1 calc GR . . B -1 H5SB H 0.508700 0.654179 -0.109129 0.065 Uiso 0.5 1 calc GR . . B -1 H5SC H 0.577336 0.724986 -0.026963 0.065 Uiso 0.5 1 calc GR . . B -1 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 0.00626(19) 0.0113(2) 0.0116(2) -0.00116(10) 0.00033(9) -0.00053(9) O1S 0.0209(8) 0.0129(8) 0.0129(8) 0.000 0.0011(6) 0.000 O1 0.0129(5) 0.0186(6) 0.0274(6) 0.0002(5) -0.0082(4) -0.0025(4) O2 0.0148(5) 0.0192(6) 0.0267(6) -0.0004(5) -0.0101(4) -0.0025(4) N3S 0.0402(13) 0.0255(12) 0.0144(10) 0.000 -0.0018(8) 0.000 C1 0.0101(9) 0.0190(11) 0.0146(9) 0.000 -0.0035(8) 0.000 C6 0.0111(9) 0.0183(11) 0.0136(9) 0.000 -0.0045(7) 0.000 C5 0.0110(9) 0.0171(10) 0.0194(10) 0.000 -0.0059(8) 0.000 C2 0.0111(9) 0.0169(11) 0.0189(10) 0.000 -0.0046(8) 0.000 C2S 0.0325(13) 0.0167(11) 0.0214(12) 0.000 0.0003(10) 0.000 C3 0.0164(8) 0.0153(8) 0.0567(12) 0.0001(8) -0.0140(8) 0.0029(6) C4 0.0159(8) 0.0145(8) 0.0576(12) -0.0030(8) -0.0138(8) -0.0022(6) C4S 0.0415(18) 0.062(2) 0.0326(16) 0.000 -0.0129(14) 0.000 C5S 0.070(2) 0.0412(18) 0.0184(13) 0.000 0.0057(15) 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 10.33774/chemrxiv-2021-lkt60 2021 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 O1S Fe1 O1S 180.0 . 5_666 ? O1 Fe1 O1S 87.69(5) 5_666 . ? O1 Fe1 O1S 92.31(5) 5_666 5_666 ? O1 Fe1 O1S 87.69(5) . 5_666 ? O1 Fe1 O1S 92.31(5) . . ? O1 Fe1 O1 180.0 5_666 . ? O1 Fe1 O2 95.29(5) 5_666 8_755 ? O1 Fe1 O2 95.29(5) . 4_466 ? O1 Fe1 O2 84.71(5) 5_666 4_466 ? O1 Fe1 O2 84.71(5) . 8_755 ? O2 Fe1 O1S 93.58(5) 8_755 5_666 ? O2 Fe1 O1S 93.58(5) 4_466 . ? O2 Fe1 O1S 86.42(5) 8_755 . ? O2 Fe1 O1S 86.42(5) 4_466 5_666 ? O2 Fe1 O2 180.00(4) 8_755 4_466 ? Fe1 O1S Fe1 112.03(8) 3_656 . ? C2S O1S Fe1 118.76(6) . 3_656 ? C2S O1S Fe1 118.76(6) . . ? C1 O1 Fe1 134.78(12) . . ? C6 O2 Fe1 132.31(12) . 4_566 ? C2S N3S C4S 120.4(3) . . ? C2S N3S C5S 123.3(3) . . ? C5S N3S C4S 116.3(3) . . ? O1 C1 O1 126.57(19) . 7_575 ? O1 C1 C2 116.71(10) . . ? O1 C1 C2 116.71(10) 7_575 . ? O2 C6 O2 125.88(19) 7_575 . ? O2 C6 C5 117.06(10) 7_575 . ? O2 C6 C5 117.06(10) . . ? C4 C5 C6 120.32(10) . . ? C4 C5 C6 120.32(10) 7_575 . ? C4 C5 C4 119.4(2) . 7_575 ? C3 C2 C1 120.31(10) 7_575 . ? C3 C2 C1 120.31(10) . . ? C3 C2 C3 119.4(2) 7_575 . ? O1S C2S N3S 125.2(3) . . ? O1S C2S H2S 117.4 . . ? N3S C2S H2S 117.4 . . ? C2 C3 H3 119.8 . . ? C2 C3 C4 120.37(16) . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 120.26(15) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? N3S C4S H4SA 109.5 . . ? N3S C4S H4SB 109.5 . . ? N3S C4S H4SC 109.5 . . ? H4SA C4S H4SB 109.5 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 109.5 . . ? N3S C5S H5SA 109.5 . . ? N3S C5S H5SB 109.5 . . ? N3S C5S H5SC 109.5 . . ? H5SA C5S H5SB 109.5 . . ? H5SA C5S H5SC 109.5 . . ? H5SB C5S H5SC 109.5 . . ? 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 O1S 2.1837(10) 5_666 ? Fe1 O1S 2.1837(10) . ? Fe1 O1 2.0587(11) . ? Fe1 O1 2.0587(11) 5_666 ? Fe1 O2 2.1001(11) 4_466 ? Fe1 O2 2.1001(11) 8_755 ? O1S C2S 1.260(3) . ? O1 C1 1.2526(15) . ? O2 C6 1.2563(15) . ? N3S C2S 1.296(3) . ? N3S C4S 1.468(4) . ? N3S C5S 1.451(4) . ? C1 C2 1.509(3) . ? C6 C5 1.507(3) . ? C5 C4 1.384(2) . ? C5 C4 1.384(2) 7_575 ? C2 C3 1.382(2) 7_575 ? C2 C3 1.382(2) . ? C2S H2S 0.9500 . ? C3 H3 0.9500 . ? C3 C4 1.392(2) . ? C4 H4 0.9500 . ? C4S H4SA 0.9800 . ? C4S H4SB 0.9800 . ? C4S H4SC 0.9800 . ? C5S H5SA 0.9800 . ? C5S H5SB 0.9800 . ? C5S H5SC 0.9800 . ?