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#$Date: 2023-05-17 11:49:43 +0300 (Wed, 17 May 2023) $
#$Revision: 283820 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/72/8107218.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_8107218
loop_
_publ_author_name
'Cui, Hong-Meng'
_publ_section_title
;
 Crystal structure of
 di-μ2-hydroxido-tetrakis(6-methylpyridine-2-carboxylato-k2 N,O)
 diiron(III) trihydrate C28H32Fe2N4O13
;
_journal_issue                   5
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              793
_journal_page_last               795
_journal_paper_doi               10.1515/ncrs-2022-0240
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C28 H26 Fe2 N4 O10, 3(H2 O)'
_chemical_formula_sum            'C28 H32 Fe2 N4 O13'
_chemical_formula_weight         744.27
_chemical_name_systematic
;
[di-μ-hydroxidotetrakis(6-methylpyridine-2-carboxylato)-di-iron(III)]-
hydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 95.190(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0964(3)
_cell_length_b                   13.4889(5)
_cell_length_c                   14.0543(5)
_cell_measurement_reflns_used    5052
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.7817
_cell_measurement_theta_min      2.7910
_cell_volume                     1528.60(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10287
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.878
_diffrn_reflns_theta_min         2.799
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0405
_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/[σ²(Fo²)+(0.0537P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0972
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2670
_reflns_number_total             3566
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0240_suppl.cif
_cod_data_source_block           p
_cod_database_code               8107218
_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   0.951
_shelx_estimated_absorpt_t_min   0.845
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H1W of O1W
 At 1.5 times of:
  All C(H,H,H) groups, H2WA of O2W
2.a Free rotating group:
 O1W(H1W), O2W(H2WA,H2WB)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5A), C10(H10), C11(H11), C12(H12)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C)
;
_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, -z'
'x-1/2, -y, 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 0.86752(4) 0.72914(3) 0.84619(2) 0.01856(11) Uani 1 1 d . . . . .
O1 O 1.11457(19) 0.71986(12) 0.86174(12) 0.0262(4) Uani 1 1 d . . . . .
O2 O 1.3528(2) 0.80230(16) 0.86847(15) 0.0405(5) Uani 1 1 d . . . . .
O3 O 0.8007(2) 0.72871(13) 0.97914(12) 0.0278(4) Uani 1 1 d . . . . .
O4 O 0.6850(3) 0.63967(18) 1.08788(14) 0.0510(6) Uani 1 1 d . . . . .
O5 O 0.6330(2) 0.73046(13) 0.79354(12) 0.0212(3) Uani 1 1 d . . . . .
H5 H 0.563(4) 0.743(2) 0.818(3) 0.048(11) Uiso 1 1 d . . . . .
N1 N 0.9388(2) 0.88338(15) 0.86761(14) 0.0225(4) Uani 1 1 d . . . . .
N2 N 0.8682(2) 0.57198(16) 0.87877(14) 0.0241(4) Uani 1 1 d . . . . .
C1 C 0.6627(3) 0.9509(2) 0.8846(2) 0.0343(6) Uani 1 1 d . . . . .
H1A H 0.609291 0.928190 0.823111 0.051 Uiso 1 1 calc GR . . . .
H1B H 0.613702 1.014059 0.901874 0.051 Uiso 1 1 calc GR . . . .
H1C H 0.646227 0.901373 0.933914 0.051 Uiso 1 1 calc GR . . . .
C2 C 0.8442(3) 0.96457(19) 0.87692(18) 0.0284(6) Uani 1 1 d . . . . .
C3 C 0.9155(3) 1.0585(2) 0.8802(2) 0.0380(7) Uani 1 1 d . . . . .
H3 H 0.847687 1.115410 0.885441 0.046 Uiso 1 1 calc R . . . .
C4 C 1.0840(4) 1.0696(2) 0.8760(2) 0.0427(7) Uani 1 1 d . . . . .
H4 H 1.133033 1.133645 0.877513 0.051 Uiso 1 1 calc R . . . .
C5 C 1.1808(3) 0.9851(2) 0.8694(2) 0.0372(7) Uani 1 1 d . . . . .
H5A H 1.297379 0.990375 0.867306 0.045 Uiso 1 1 calc R . . . .
C6 C 1.1053(3) 0.89439(19) 0.86614(17) 0.0260(5) Uani 1 1 d . . . . .
C7 C 1.2014(3) 0.7985(2) 0.86437(17) 0.0261(5) Uani 1 1 d . . . . .
C8 C 1.0186(3) 0.5124(2) 0.7468(2) 0.0357(6) Uani 1 1 d . . . . .
H8A H 0.945174 0.533604 0.691300 0.054 Uiso 1 1 calc GR . . . .
H8B H 1.075693 0.451183 0.731283 0.054 Uiso 1 1 calc GR . . . .
H8C H 1.100660 0.564315 0.763743 0.054 Uiso 1 1 calc GR . . . .
C9 C 0.9185(3) 0.49403(19) 0.82930(19) 0.0298(6) Uani 1 1 d . . . . .
C10 C 0.8784(4) 0.3976(2) 0.8568(2) 0.0414(7) Uani 1 1 d . . . . .
H10 H 0.911758 0.342379 0.821183 0.050 Uiso 1 1 calc R . . . .
C11 C 0.7918(4) 0.3827(2) 0.9344(2) 0.0467(8) Uani 1 1 d . . . . .
H11 H 0.761238 0.317477 0.951444 0.056 Uiso 1 1 calc R . . . .
C12 C 0.7490(4) 0.4622(2) 0.9877(2) 0.0401(7) Uani 1 1 d . . . . .
H12 H 0.692877 0.452825 1.043556 0.048 Uiso 1 1 calc R . . . .
C13 C 0.7890(3) 0.5556(2) 0.95853(17) 0.0286(6) Uani 1 1 d . . . . .
C14 C 0.7527(3) 0.6475(2) 1.01402(18) 0.0304(6) Uani 1 1 d . . . . .
O1W O 0.750000 0.7497(5) 1.250000 0.204(5) Uani 1 2 d S T P . .
H1W H 0.759169 0.716755 1.191366 0.244 Uiso 1 1 d G . . . .
O2W O 0.4626(5) 0.8189(3) 1.0859(5) 0.1221(15) Uani 1 1 d . . . . .
H2WA H 0.500380 0.760399 1.081962 0.183 Uiso 1 1 d G . . . .
H2WB H 0.489898 0.798188 1.153989 0.10(2) Uiso 1 1 d G . . . .
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_
_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
O1 Fe1 N1 78.10(7) . .
O1 Fe1 N2 86.12(7) . .
O3 Fe1 O1 104.56(7) . .
O3 Fe1 N1 87.94(7) . .
O3 Fe1 N2 78.16(7) . .
O5 Fe1 O1 91.23(7) 2_656 .
O5 Fe1 O1 164.07(7) . .
O5 Fe1 O3 91.04(7) . .
O5 Fe1 O3 164.19(7) 2_656 .
O5 Fe1 O5 73.15(8) 2_656 .
O5 Fe1 N1 96.11(7) 2_656 .
O5 Fe1 N1 106.13(7) . .
O5 Fe1 N2 94.12(7) . .
O5 Fe1 N2 102.69(8) 2_656 .
N2 Fe1 N1 155.67(8) . .
C7 O1 Fe1 119.80(15) . .
C14 O3 Fe1 118.78(16) . .
Fe1 O5 Fe1 106.84(8) 2_656 .
C2 N1 Fe1 130.12(16) . .
C2 N1 C6 119.1(2) . .
C6 N1 Fe1 110.75(15) . .
C9 N2 Fe1 130.59(18) . .
C9 N2 C13 119.2(2) . .
C13 N2 Fe1 109.90(17) . .
N1 C2 C1 118.5(2) . .
N1 C2 C3 120.3(2) . .
C3 C2 C1 121.2(2) . .
C4 C3 C2 120.4(3) . .
C3 C4 C5 118.7(3) . .
C6 C5 C4 118.9(2) . .
N1 C6 C5 122.6(2) . .
N1 C6 C7 114.8(2) . .
C5 C6 C7 122.6(2) . .
O1 C7 C6 115.5(2) . .
O2 C7 O1 125.8(2) . .
O2 C7 C6 118.6(2) . .
N2 C9 C8 118.9(2) . .
N2 C9 C10 119.6(3) . .
C10 C9 C8 121.5(3) . .
C11 C10 C9 120.4(3) . .
C10 C11 C12 119.7(3) . .
C11 C12 C13 118.5(3) . .
N2 C13 C12 122.5(3) . .
N2 C13 C14 115.0(2) . .
C12 C13 C14 122.6(3) . .
O3 C14 C13 115.3(2) . .
O4 C14 O3 125.3(3) . .
O4 C14 C13 119.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 1.9963(16) .
Fe1 O3 1.9915(17) .
Fe1 O5 1.9636(17) 2_656
Fe1 O5 1.9747(16) .
Fe1 N1 2.173(2) .
Fe1 N2 2.169(2) .
O1 C7 1.271(3) .
O2 C7 1.223(3) .
O3 C14 1.275(3) .
O4 C14 1.221(3) .
N1 C2 1.350(3) .
N1 C6 1.358(3) .
N2 C9 1.344(3) .
N2 C13 1.359(3) .
C1 C2 1.495(3) .
C2 C3 1.392(4) .
C3 C4 1.379(4) .
C4 C5 1.391(4) .
C5 C6 1.367(4) .
C6 C7 1.511(4) .
C8 C9 1.494(4) .
C9 C10 1.404(4) .
C10 C11 1.364(5) .
C11 C12 1.370(4) .
C12 C13 1.374(4) .
C13 C14 1.507(4) .
