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#$Date: 2022-05-05 23:48:44 +0300 (Thu, 05 May 2022) $
#$Revision: 275041 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/12/7061276.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_7061276
loop_
_publ_author_name
'Gurbanov, Atash V.'
'Andrade, Marta A.'
'Martins, Luísa M. D. R. S.'
'Mahmudov, Kamran T.'
'Pombeiro, Armando J. L.'
_publ_section_title
;
 Water-soluble Al(iii), Fe(iii) and Cu(ii) formazanates: synthesis,
 structure, and applications in alkane and alcohol oxidations
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5002
_journal_page_last               5011
_journal_paper_doi               10.1039/D1NJ06211E
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C28 H26 Fe N10 O16 S4, 2(H2 O)'
_chemical_formula_sum            'C28 H30 Fe N10 O18 S4'
_chemical_formula_weight         978.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-12-02 deposited with the CCDC.	2022-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.212(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.4924(12)
_cell_length_b                   6.7910(4)
_cell_length_c                   14.9191(7)
_cell_measurement_reflns_used    4802
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.65
_cell_measurement_theta_min      2.78
_cell_volume                     2466.8(2)
_computing_cell_refinement       'APEX3 Software (Bruker, 2019)'
_computing_data_collection       'APEX3 Software (Bruker, 2019)'
_computing_data_reduction        'APEX3 Software (Bruker, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       'omega and phi'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12389
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.716
_diffrn_reflns_theta_min         2.639
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       plate
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2546
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0404
_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)+(0.0452P)²+3.8350P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1913
_reflns_number_total             2546
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1nj06211e2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7061275--7061277.cif.'
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7061276
_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_min   0.875
_shelx_estimated_absorpt_t_max   0.952
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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 0.0381(2) Uani 1 4 d S T P . .
S1 S 0.10940(3) 0.500000 0.37423(7) 0.0468(3) Uani 1 2 d S T P . .
S2 S 0.37739(4) 0.500000 0.15452(7) 0.0544(3) Uani 1 2 d S T P . .
N1 N 0.23581(10) 0.500000 0.4550(2) 0.0348(6) Uani 1 2 d S T P A .
H1N H 0.2157(15) 0.500000 0.396(3) 0.042 Uiso 1 2 d S U P . .
N2 N 0.28972(10) 0.500000 0.48315(19) 0.0338(6) Uani 1 2 d S T P . .
N3 N 0.27750(10) 0.500000 0.31680(19) 0.0362(6) Uani 1 2 d S T P . .
N4 N 0.30618(11) 0.500000 0.26619(19) 0.0386(7) Uani 1 2 d S T P . .
N5 N 0.41485(11) 0.500000 0.4755(2) 0.0449(7) Uani 1 2 d S T P . .
O1 O 0.1364(3) 0.500000 0.3067(5) 0.059(3) Uani 0.428(7) 2 d S T P A 1
O2 O 0.0740(2) 0.3257(9) 0.3574(3) 0.068(2) Uani 0.428(7) 1 d . . P A 1
O1' O 0.05697(17) 0.500000 0.3775(4) 0.0630(19) Uani 0.572(7) 2 d S T P A 2
O2' O 0.12415(17) 0.3269(9) 0.3358(3) 0.094(3) Uani 0.572(7) 1 d . . P A 2
O3 O 0.39494(8) 0.6775(4) 0.21245(14) 0.0646(6) Uani 1 1 d D . . . .
O4 O 0.39211(13) 0.500000 0.0706(2) 0.0920(13) Uani 1 2 d S T P . .
O5 O 0.48152(7) 0.7233(3) 0.39387(13) 0.0574(5) Uani 1 1 d D . . . .
H5A H 0.5054(10) 0.780(5) 0.381(2) 0.086 Uiso 1 1 d D U . . .
H5B H 0.4538(9) 0.704(6) 0.3407(17) 0.086 Uiso 1 1 d D U . . .
O6 O 0.4453(2) 1.000000 0.1601(4) 0.1246(17) Uani 1 2 d DS T P . .
H6A H 0.4372(18) 0.9000(15) 0.189(3) 0.187 Uiso 1 1 d D U . . .
C1 C 0.21339(13) 0.500000 0.5255(2) 0.0331(7) Uani 1 2 d S T P . .
C2 C 0.15620(13) 0.500000 0.4978(2) 0.0357(7) Uani 1 2 d S T P A .
C3 C 0.13509(15) 0.500000 0.5694(3) 0.0484(9) Uani 1 2 d S T P . .
H3 H 0.097232 0.500000 0.551087 0.058 Uiso 1 2 calc R U P A .
C4 C 0.16891(18) 0.500000 0.6665(3) 0.0571(11) Uani 1 2 d S T P A .
H4 H 0.154053 0.500000 0.713540 0.069 Uiso 1 2 calc R U P . .
C5 C 0.22539(17) 0.500000 0.6942(3) 0.0515(10) Uani 1 2 d S T P . .
H5 H 0.248514 0.500000 0.760006 0.062 Uiso 1 2 calc R U P A .
C6 C 0.24738(15) 0.500000 0.6243(2) 0.0440(9) Uani 1 2 d S T P A .
H6 H 0.285302 0.500000 0.643452 0.053 Uiso 1 2 calc R U P . .
C7 C 0.30971(12) 0.500000 0.4164(2) 0.0325(7) Uani 1 2 d S T P . .
C8 C 0.36863(13) 0.500000 0.4508(2) 0.0361(8) Uani 1 2 d S T P . .
C9 C 0.27525(13) 0.500000 0.1639(2) 0.0422(8) Uani 1 2 d S T P . .
C10 C 0.30446(14) 0.500000 0.1044(2) 0.0435(9) Uani 1 2 d S T P . .
C11 C 0.27684(17) 0.500000 0.0039(3) 0.0575(11) Uani 1 2 d S T P . .
H11 H 0.296430 0.500000 -0.035946 0.069 Uiso 1 2 calc R U P . .
C12 C 0.22022(18) 0.500000 -0.0370(3) 0.0687(13) Uani 1 2 d S T P . .
H12 H 0.201689 0.500000 -0.104483 0.082 Uiso 1 2 calc R U P . .
C13 C 0.19122(18) 0.500000 0.0209(3) 0.0725(14) Uani 1 2 d S T P . .
H13 H 0.153039 0.500000 -0.007529 0.087 Uiso 1 2 calc R U P . .
C14 C 0.21810(15) 0.500000 0.1219(3) 0.0613(12) Uani 1 2 d S T P . .
H14 H 0.198093 0.500000 0.160975 0.074 Uiso 1 2 calc R U P . .
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'
S S 0.1246 0.1234 '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
_geom_angle_publ_flag
O5 Fe1 O5 180.0 6_565 2_656 ?
O5 Fe1 O5 87.89(12) 6_565 5_666 ?
O5 Fe1 O5 92.11(12) 2_656 5_666 ?
O5 Fe1 O5 92.11(12) 6_565 . ?
O5 Fe1 O5 87.89(12) 2_656 . ?
O5 Fe1 O5 180.0 5_666 . ?
O5 Fe1 N5 92.62(7) 6_565 5_666 ?
O5 Fe1 N5 87.38(7) 2_656 5_666 ?
O5 Fe1 N5 87.38(7) 5_666 5_666 ?
O5 Fe1 N5 92.62(7) . 5_666 ?
O5 Fe1 N5 87.38(7) 6_565 . ?
O5 Fe1 N5 92.62(7) 2_656 . ?
O5 Fe1 N5 92.62(7) 5_666 . ?
O5 Fe1 N5 87.38(7) . . ?
N5 Fe1 N5 180.0 5_666 . ?
O1' S1 O2' 116.3(2) . . ?
O2' S1 O2' 110.8(5) 6_565 . ?
O1 S1 O2 109.8(3) . 6_565 ?
O1 S1 O2 109.8(3) . . ?
O2 S1 O2 107.4(5) 6_565 . ?
O1' S1 C2 105.0(3) . . ?
O2' S1 C2 103.16(17) 6_565 . ?
O2' S1 C2 103.16(17) . . ?
O1 S1 C2 112.9(3) . . ?
O2 S1 C2 108.4(2) 6_565 . ?
O2 S1 C2 108.4(2) . . ?
O3 S2 O3 112.58(17) 6_565 . ?
O3 S2 O4 112.50(10) 6_565 . ?
O3 S2 O4 112.49(10) . . ?
O3 S2 C10 106.95(10) 6_565 . ?
O3 S2 C10 106.95(10) . . ?
O4 S2 C10 104.72(17) . . ?
N2 N1 C1 119.2(3) . . ?
N2 N1 H1N 120(2) . . ?
C1 N1 H1N 121(2) . . ?
C7 N2 N1 118.2(3) . . ?
N4 N3 C7 112.2(2) . . ?
N3 N4 C9 114.4(3) . . ?
C8 N5 Fe1 171.7(3) . . ?
Fe1 O5 H5A 123(2) . . ?
Fe1 O5 H5B 117(2) . . ?
H5A O5 H5B 109(2) . . ?
H6A O6 H6A 102(3) . 6_575 ?
C6 C1 N1 120.5(3) . . ?
C6 C1 C2 119.0(3) . . ?
N1 C1 C2 120.5(3) . . ?
C3 C2 C1 119.3(3) . . ?
C3 C2 S1 118.2(3) . . ?
C1 C2 S1 122.6(2) . . ?
C4 C3 C2 121.3(3) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 119.6(3) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C6 C5 C4 120.1(4) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C1 120.7(3) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
N2 C7 N3 123.7(3) . . ?
N2 C7 C8 116.1(3) . . ?
N3 C7 C8 120.2(3) . . ?
N5 C8 C7 178.3(4) . . ?
C10 C9 C14 119.5(3) . . ?
C10 C9 N4 117.2(3) . . ?
C14 C9 N4 123.3(3) . . ?
C11 C10 C9 120.2(3) . . ?
C11 C10 S2 118.6(3) . . ?
C9 C10 S2 121.2(3) . . ?
C12 C11 C10 119.8(4) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C13 C12 C11 120.4(4) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C14 120.7(4) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C13 C14 C9 119.3(4) . . ?
C13 C14 H14 120.3 . . ?
C9 C14 H14 120.3 . . ?
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 O5 2.106(2) 6_565 ?
Fe1 O5 2.106(2) 2_656 ?
Fe1 O5 2.106(2) 5_666 ?
Fe1 O5 2.106(2) . ?
Fe1 N5 2.138(3) 5_666 ?
Fe1 N5 2.138(3) . ?
S1 O1' 1.409(5) . ?
S1 O2' 1.428(4) 6_565 ?
S1 O2' 1.428(4) . ?
S1 O1 1.448(6) . ?
S1 O2 1.469(5) 6_565 ?
S1 O2 1.469(5) . ?
S1 C2 1.770(3) . ?
S2 O3 1.449(2) 6_565 ?
S2 O3 1.449(2) . ?
S2 O4 1.451(3) . ?
S2 C10 1.776(4) . ?
N1 N2 1.320(3) . ?
N1 C1 1.398(4) . ?
N1 H1N 0.83(4) . ?
N2 C7 1.298(4) . ?
N3 N4 1.265(4) . ?
N3 C7 1.392(4) . ?
N4 C9 1.419(4) . ?
N5 C8 1.131(4) . ?
O5 H5A 0.823(17) . ?
O5 H5B 0.852(17) . ?
O6 H6A 0.874(16) . ?
O6 H6A 0.874(16) 6_575 ?
C1 C6 1.392(5) . ?
C1 C2 1.404(4) . ?
C2 C3 1.387(5) . ?
C3 C4 1.371(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.380(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.438(4) . ?
C9 C10 1.389(5) . ?
C9 C14 1.392(5) . ?
C10 C11 1.385(5) . ?
C11 C12 1.379(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.363(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.390(6) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
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
C1 N1 N2 C7 180.000(1) . . . . ?
C7 N3 N4 C9 180.000(0) . . . . ?
N2 N1 C1 C6 0.000(1) . . . . ?
N2 N1 C1 C2 180.000(1) . . . . ?
C6 C1 C2 C3 0.000(1) . . . . ?
N1 C1 C2 C3 180.000(1) . . . . ?
C6 C1 C2 S1 180.000(1) . . . . ?
N1 C1 C2 S1 0.000(1) . . . . ?
O1' S1 C2 C3 0.000(1) . . . . ?
O2' S1 C2 C3 122.3(3) 6_565 . . . ?
O2' S1 C2 C3 -122.3(3) . . . . ?
O1 S1 C2 C3 180.000(1) . . . . ?
O2 S1 C2 C3 58.1(3) 6_565 . . . ?
O2 S1 C2 C3 -58.1(3) . . . . ?
O1' S1 C2 C1 180.000(1) . . . . ?
O2' S1 C2 C1 -57.7(3) 6_565 . . . ?
O2' S1 C2 C1 57.7(3) . . . . ?
O1 S1 C2 C1 0.000(1) . . . . ?
O2 S1 C2 C1 -121.9(3) 6_565 . . . ?
O2 S1 C2 C1 121.9(3) . . . . ?
C1 C2 C3 C4 0.000(1) . . . . ?
S1 C2 C3 C4 180.000(1) . . . . ?
C2 C3 C4 C5 0.000(1) . . . . ?
C3 C4 C5 C6 0.000(1) . . . . ?
C4 C5 C6 C1 0.000(1) . . . . ?
N1 C1 C6 C5 180.000(1) . . . . ?
C2 C1 C6 C5 0.000(1) . . . . ?
N1 N2 C7 N3 0.000(1) . . . . ?
N1 N2 C7 C8 180.000(1) . . . . ?
N4 N3 C7 N2 180.000(0) . . . . ?
N4 N3 C7 C8 0.000(1) . . . . ?
N3 N4 C9 C10 180.000(0) . . . . ?
N3 N4 C9 C14 0.000(0) . . . . ?
C14 C9 C10 C11 0.000(0) . . . . ?
N4 C9 C10 C11 180.000(0) . . . . ?
C14 C9 C10 S2 180.000(0) . . . . ?
N4 C9 C10 S2 0.000(0) . . . . ?
O3 S2 C10 C11 -119.58(9) 6_565 . . . ?
O3 S2 C10 C11 119.58(9) . . . . ?
O4 S2 C10 C11 0.000(0) . . . . ?
O3 S2 C10 C9 60.42(9) 6_565 . . . ?
O3 S2 C10 C9 -60.42(9) . . . . ?
O4 S2 C10 C9 180.000(0) . . . . ?
C9 C10 C11 C12 0.000(0) . . . . ?
S2 C10 C11 C12 180.000(0) . . . . ?
C10 C11 C12 C13 0.000(0) . . . . ?
C11 C12 C13 C14 0.000(0) . . . . ?
C12 C13 C14 C9 0.000(0) . . . . ?
C10 C9 C14 C13 0.000(0) . . . . ?
N4 C9 C14 C13 180.000(0) . . . . ?
