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#$Date: 2025-08-22 16:55:42 +0200 (Fri 22 de Aug de 2025) $
#$Revision: 301864 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/49/7214965.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_7214965
loop_
_publ_author_name
'Tan, Yu-Hui'
'Wu, Jin-Ji'
'Zhou, Hai-Yun'
'Yang, Li-Fei'
'Ye, Bao-Hui'
_publ_section_title
;
 Anion and pH induced spontaneous resolution of Δ- and Λ-[M(H2Biim)3]SO4
 (M = Ru2+, Co2+, Ni2+, Mn2+, Fe2+, and Zn2+) enantiomers
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              8117
_journal_paper_doi               10.1039/c2ce26334c
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C18 H18 Fe N12 O4 S'
_chemical_formula_weight         554.35
_space_group_IT_number           80
_symmetry_space_group_name_Hall  'I 4bw'
_symmetry_space_group_name_H-M   'I 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8660(3)
_cell_length_b                   12.8660(3)
_cell_length_c                   14.3888(5)
_cell_measurement_temperature    153(2)
_cell_volume                     2381.83(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11774
_diffrn_reflns_theta_full        27.38
_diffrn_reflns_theta_max         27.38
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_T_max  0.8607
_exptl_absorpt_correction_T_min  0.8011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.181
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.034(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2614
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0420P)²+1.0088P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0790
_reflns_number_gt                2424
_reflns_number_total             2614
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26334c.txt
_cod_data_source_block           D-5
_cod_original_sg_symbol_H-M      I4(1)
_cod_database_code               7214965
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.5000 0.5000 0.00911(3) 0.04378(13) Uani 1 2 d S
C1 C 0.4300(2) 0.69810(19) -0.1343(2) 0.0576(7) Uani 1 1 d .
H1 H 0.4109 0.7494 -0.0921 0.069 Uiso 1 1 calc R
C2 C 0.4345(2) 0.71071(19) -0.2274(2) 0.0621(7) Uani 1 1 d .
H2 H 0.4184 0.7707 -0.2604 0.075 Uiso 1 1 calc R
C3 C 0.48064(18) 0.55272(18) -0.19121(16) 0.0446(5) Uani 1 1 d .
C4 C 0.41039(19) 0.6718(2) 0.1677(2) 0.0532(6) Uani 1 1 d .
H4 H 0.4623 0.7221 0.1666 0.064 Uiso 1 1 calc R
C5 C 0.3275(2) 0.6724(2) 0.22487(19) 0.0565(6) Uani 1 1 d .
H5 H 0.3122 0.7221 0.2699 0.068 Uiso 1 1 calc R
C6 C 0.31942(16) 0.53643(17) 0.13468(16) 0.0400(4) Uani 1 1 d .
C7 C 0.29244(18) 0.44050(17) 0.08673(16) 0.0418(4) Uani 1 1 d .
C8 C 0.2187(2) 0.3012(2) 0.03267(19) 0.0592(7) Uani 1 1 d .
H6 H 0.1710 0.2483 0.0212 0.071 Uiso 1 1 calc R
C9 C 0.3151(2) 0.3117(2) -0.0062(2) 0.0619(7) Uani 1 1 d .
H9 H 0.3446 0.2660 -0.0488 0.074 Uiso 1 1 calc R
N1 N 0.45797(17) 0.59792(15) -0.11091(16) 0.0509(5) Uani 1 1 d .
N2 N 0.46716(17) 0.61805(15) -0.26360(14) 0.0518(5) Uani 1 1 d .
H2A H 0.4772 0.6041 -0.3214 0.062 Uiso 1 1 calc R
N3 N 0.40672(15) 0.58556(16) 0.11099(14) 0.0456(4) Uani 1 1 d .
N4 N 0.26955(15) 0.58540(16) 0.20388(15) 0.0472(4) Uani 1 1 d .
H4A H 0.2126 0.5662 0.2300 0.057 Uiso 1 1 calc R
N5 N 0.36183(16) 0.40076(16) 0.02751(14) 0.0502(5) Uani 1 1 d .
N6 N 0.20609(16) 0.38322(16) 0.09146(14) 0.0477(4) Uani 1 1 d .
H8 H 0.1525 0.3958 0.1253 0.057 Uiso 1 1 calc R
O1 O 1.0221(2) 0.4111(2) 0.17801(19) 0.0926(9) Uani 1 1 d .
O2 O 0.90983(13) 0.47454(18) 0.29597(13) 0.0636(5) Uani 1 1 d .
S1 S 1.0000 0.5000 0.23698(5) 0.0501(2) Uani 1 2 d S
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'
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
N3 Fe1 N3 96.02(11) 6_554 .
N3 Fe1 N1 160.97(7) 6_554 .
N3 Fe1 N1 95.89(8) . .
N3 Fe1 N1 95.89(8) 6_554 6_554
N3 Fe1 N1 160.97(7) . 6_554
N1 Fe1 N1 76.89(11) . 6_554
N3 Fe1 N5 76.64(7) 6_554 6_554
N3 Fe1 N5 94.03(8) . 6_554
N1 Fe1 N5 87.76(8) . 6_554
N1 Fe1 N5 103.13(8) 6_554 6_554
N3 Fe1 N5 94.03(8) 6_554 .
N3 Fe1 N5 76.64(7) . .
N1 Fe1 N5 103.13(8) . .
N1 Fe1 N5 87.76(8) 6_554 .
N5 Fe1 N5 166.20(11) 6_554 .
C2 C1 N1 110.1(2) . .
C1 C2 N2 106.6(2) . .
N1 C3 N2 111.8(2) . .
N1 C3 C3 119.18(13) . 6_554
N2 C3 C3 128.97(14) . 6_554
C5 C4 N3 109.8(2) . .
C4 C5 N4 106.8(2) . .
N3 C6 N4 111.7(2) . .
N3 C6 C7 118.8(2) . .
N4 C6 C7 129.5(2) . .
N5 C7 N6 112.2(2) . .
N5 C7 C6 117.9(2) . .
N6 C7 C6 130.0(2) . .
N6 C8 C9 106.6(2) . .
C8 C9 N5 109.4(2) . .
C3 N1 C1 104.8(2) . .
C3 N1 Fe1 112.21(15) . .
C1 N1 Fe1 142.05(18) . .
C3 N2 C2 106.8(2) . .
C6 N3 C4 105.03(19) . .
C6 N3 Fe1 113.22(15) . .
C4 N3 Fe1 141.43(16) . .
C6 N4 C5 106.6(2) . .
C7 N5 C9 104.5(2) . .
C7 N5 Fe1 113.20(15) . .
C9 N5 Fe1 142.08(18) . .
C7 N6 C8 107.3(2) . .
O1 S1 O1 108.5(3) . 6_654
O1 S1 O2 110.93(14) . 6_654
O1 S1 O2 108.40(12) 6_654 6_654
O1 S1 O2 108.40(12) . .
O1 S1 O2 110.93(14) 6_654 .
O2 S1 O2 109.70(15) 6_654 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N3 2.191(2) 6_554
Fe1 N3 2.191(2) .
Fe1 N1 2.205(2) .
Fe1 N1 2.205(2) 6_554
Fe1 N5 2.205(2) 6_554
Fe1 N5 2.205(2) .
C1 C2 1.350(4) .
C1 N1 1.380(3) .
C2 N2 1.368(4) .
C3 N1 1.326(3) .
C3 N2 1.350(3) .
C3 C3 1.445(5) 6_554
C4 C5 1.348(4) .
C4 N3 1.378(3) .
C5 N4 1.379(3) .
C6 N3 1.333(3) .
C6 N4 1.342(3) .
C6 C7 1.456(3) .
C7 N5 1.336(3) .
C7 N6 1.335(3) .
C8 N6 1.362(3) .
C8 C9 1.367(4) .
C9 N5 1.383(3) .
O1 S1 1.452(2) .
O2 S1 1.4743(18) .
S1 O1 1.452(2) 6_654
S1 O2 1.4742(18) 6_654
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139198333
