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#$Date: 2020-01-04 05:07:45 +0200 (Sat, 04 Jan 2020) $
#$Revision: 246540 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/71/4517134.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_4517134
loop_
_publ_author_name
'Adhikary, Amit'
'Akhtar, Sohel'
'Pariyar, Anand'
'Batsanov, Andrei S.'
'Mondal, Raju'
_publ_section_title
;
 Correction to “Temperature-Induced
 Single-Crystal-to-Single-Crystal Transformations with Consequential
 Changes in the Magnetic Properties of Fe(III) Complexes”
;
_journal_issue                   23
_journal_name_full               'ACS Omega'
_journal_page_first              20423
_journal_paper_doi               10.1021/acsomega.9b03593
_journal_volume                  4
_journal_year                    2019
_chemical_formula_sum            'C14 H14 Fe2 N2 O13'
_chemical_formula_weight         529.97
_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_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90.043(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3981(11)
_cell_length_b                   21.713(2)
_cell_length_c                   7.5145(7)
_cell_measurement_reflns_used    2608
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      3.33
_cell_volume                     1859.7(3)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12262
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.259
_diffrn_reflns_theta_min         3.334
_exptl_absorpt_coefficient_mu    1.637
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_description       Block
_exptl_crystal_F_000             1072
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0494
_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/[σ²(Fo²)+(0.0745P)²+3.2963P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1517
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1609
_reflns_number_total             2297
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ao9b03593_si_001.cif
_cod_data_source_block           Complex_1
_cod_depositor_comments
'Adding full bibliography for 4517133--4517134.cif.'
_cod_original_cell_volume        1859.8(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4517134
_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.
;
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
Fe01 Fe 0.36806(5) 0.36890(2) 0.70941(7) 0.0254(2) Uani 1 1 d . . .
O6 O 0.5209(2) 0.36753(13) 0.5883(4) 0.0313(7) Uani 1 1 d . . .
O1 O 0.3168(2) 0.45771(13) 0.7817(4) 0.0316(7) Uani 1 1 d . . .
O3 O 0.3343(2) 0.27672(12) 0.6900(4) 0.0305(6) Uani 1 1 d . . .
O5 O 0.2871(3) 0.38461(14) 0.4776(4) 0.0351(7) Uani 1 1 d . . .
H5A H 0.310305 0.357754 0.399302 0.053 Uiso 1 1 d R U .
H5B H 0.310156 0.419889 0.435298 0.053 Uiso 1 1 d R U .
O4 O 0.2118(3) 0.19986(13) 0.7646(4) 0.0368(7) Uani 1 1 d . . .
O2 O 0.1757(2) 0.51471(13) 0.9077(5) 0.0407(8) Uani 1 1 d . . .
N1 N 0.2107(3) 0.35712(14) 0.8426(4) 0.0225(7) Uani 1 1 d . . .
O7 O 0.500000 0.4413(3) 0.250000 0.0761(18) Uani 1 2 d GS T P
H7 H 0.489929 0.462916 0.153730 0.114 Uiso 0.5 1 d G U P
C1 C 0.1545(3) 0.40607(18) 0.9067(5) 0.0248(8) Uani 1 1 d . . .
C3 C 0.0050(4) 0.3411(2) 1.0191(6) 0.0341(10) Uani 1 1 d . . .
H3 H -0.065709 0.335315 1.083673 0.041 Uiso 1 1 calc R U .
C5 C 0.1667(3) 0.30103(17) 0.8582(5) 0.0231(8) Uani 1 1 d . . .
C4 C 0.0627(3) 0.29073(19) 0.9475(5) 0.0301(9) Uani 1 1 d . . .
H4 H 0.031592 0.250340 0.959427 0.036 Uiso 1 1 calc R U .
C7 C 0.2425(4) 0.25413(18) 0.7639(5) 0.0279(8) Uani 1 1 d . . .
C6 C 0.2191(3) 0.46533(18) 0.8637(5) 0.0281(9) Uani 1 1 d . . .
C2 C 0.0502(3) 0.4002(2) 0.9969(6) 0.0326(9) Uani 1 1 d . . .
H2 H 0.010308 0.435274 1.042522 0.039 Uiso 1 1 calc R U .
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'
Fe Fe 0.3463 0.8444 '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
O6 Fe01 O6 77.80(13) . 2_656
O6 Fe01 O5 90.47(12) . .
O6 Fe01 O5 165.19(12) 2_656 .
O6 Fe01 O3 96.84(11) . .
O6 Fe01 O3 99.24(12) 2_656 .
O5 Fe01 O3 91.05(12) . .
O6 Fe01 N1 171.88(12) . .
O6 Fe01 N1 100.39(12) 2_656 .
O5 Fe01 N1 92.45(13) . .
O3 Fe01 N1 75.55(11) . .
O6 Fe01 O1 112.49(11) . .
O6 Fe01 O1 89.58(12) 2_656 .
O5 Fe01 O1 86.57(12) . .
O3 Fe01 O1 150.57(11) . .
N1 Fe01 O1 75.26(11) . .
Fe01 O6 Fe01 102.17(13) . 2_656
C6 O1 Fe01 119.1(2) . .
C7 O3 Fe01 119.8(2) . .
Fe01 O5 H5A 109.5 . .
Fe01 O5 H5B 109.2 . .
H5A O5 H5B 104.5 . .
C5 N1 C1 121.4(3) . .
C5 N1 Fe01 119.0(2) . .
C1 N1 Fe01 119.6(3) . .
H7 O7 H7 114.7 . 2_655
N1 C1 C2 121.4(4) . .
N1 C1 C6 111.5(3) . .
C2 C1 C6 127.1(4) . .
C4 C3 C2 120.4(4) . .
C4 C3 H3 119.8 . .
C2 C3 H3 119.8 . .
N1 C5 C4 121.2(4) . .
N1 C5 C7 111.2(3) . .
C4 C5 C7 127.6(4) . .
C5 C4 C3 117.9(4) . .
C5 C4 H4 121.0 . .
C3 C4 H4 121.0 . .
O4 C7 O3 126.9(4) . .
O4 C7 C5 118.7(4) . .
O3 C7 C5 114.3(3) . .
O2 C6 O1 126.4(4) . .
O2 C6 C1 119.2(3) . .
O1 C6 C1 114.5(3) . .
C1 C2 C3 117.6(4) . .
C1 C2 H2 121.2 . .
C3 C2 H2 121.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe01 O6 1.966(3) .
Fe01 O6 1.977(3) 2_656
Fe01 O5 2.000(3) .
Fe01 O3 2.043(3) .
Fe01 N1 2.070(3) .
Fe01 O1 2.087(3) .
O1 C6 1.284(4) .
O3 C7 1.283(5) .
O5 H5A 0.8701 .
O5 H5B 0.8702 .
O4 C7 1.229(5) .
O2 C6 1.227(5) .
N1 C5 1.323(5) .
N1 C1 1.331(5) .
O7 H7 0.8701 .
O7 H7 0.87(15) 2_655
C1 C2 1.376(5) .
C1 C6 1.517(5) .
C3 C4 1.385(6) .
C3 C2 1.393(6) .
C3 H3 0.9500 .
C5 C4 1.381(5) .
C5 C7 1.512(5) .
C4 H4 0.9500 .
C2 H2 0.9500 .
