#------------------------------------------------------------------------------
#$Date: 2021-12-07 06:03:46 +0200 (Tue, 07 Dec 2021) $
#$Revision: 271237 $
#$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 G.'
'Pakamorė, 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_issue                   12
_journal_name_full               'Materials horizons'
_journal_page_first              3377
_journal_page_last               3386
_journal_paper_doi               10.1039/d1mh01663f
_journal_volume                  8
_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       'φ and ω 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 λ/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/[σ²(Fo²)+(0.0482P)²+1.0827P] where P=(Fo²+2Fc²)/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 > 2σ(I)'
_cod_data_source_file            d1mh01663f2.cif
_cod_data_source_block           FeDMFBDC
_cod_depositor_comments
'Adding full bibliography for 1564910--1564914.cif.'
_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)
;
_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_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 . ?
