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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/7/21/49/7214970.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.
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data_7214970
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 Mn N12 O4 S'
_chemical_formula_weight         553.44
_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                   12.8656(6)
_cell_length_b                   12.8656(6)
_cell_length_c                   14.5185(13)
_cell_measurement_temperature    273(2)
_cell_volume                     2403.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4678
_diffrn_reflns_theta_full        25.95
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  0.9344
_exptl_absorpt_correction_T_min  0.8746
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         1547
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0486P)²+1.0126P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0899
_reflns_number_gt                1415
_reflns_number_total             1547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26334c.txt
_cod_data_source_block           L-4
_cod_original_sg_symbol_H-M      I4(1)
_cod_database_code               7214970
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
C1 C 0.3105(3) 0.8109(3) 0.2094(3) 0.0603(12) Uani 1 1 d .
H1 H 0.2626 0.8408 0.1672 0.072 Uiso 1 1 calc R
C2 C 0.3011(3) 0.7151(4) 0.2478(3) 0.0536(10) Uani 1 1 d .
H2 H 0.2472 0.6661 0.2371 0.064 Uiso 1 1 calc R
C3 C 0.4402(3) 0.7895(3) 0.2995(3) 0.0403(8) Uani 1 1 d .
C4 C 0.5371(3) 0.8154(3) 0.3465(3) 0.0379(8) Uani 1 1 d .
C5 C 0.6731(3) 0.8228(3) 0.4355(3) 0.0488(10) Uani 1 1 d .
H5 H 0.7231 0.8069 0.4815 0.059 Uiso 1 1 calc R
C6 C 0.6739(3) 0.9055(3) 0.3781(3) 0.0452(9) Uani 1 1 d .
H6 H 0.7262 0.9577 0.3766 0.054 Uiso 1 1 calc R
C7 C 0.3017(3) 1.0676(3) 0.0726(3) 0.0546(11) Uani 1 1 d .
H7 H 0.2490 1.0873 0.1150 0.066 Uiso 1 1 calc R
C8 C 0.2889(3) 1.0637(3) -0.0202(3) 0.0559(11) Uani 1 1 d .
H8 H 0.2280 1.0799 -0.0543 0.067 Uiso 1 1 calc R
C9 C 0.4478(3) 1.0186(3) 0.0171(3) 0.0443(9) Uani 1 1 d .
Mn1 Mn 0.5000 1.0000 0.21981(5) 0.0444(2) Uani 1 2 d S
N1 N 0.3998(2) 0.8581(3) 0.2406(2) 0.0500(8) Uani 1 1 d .
N2 N 0.3838(2) 0.7034(3) 0.3047(2) 0.0449(8) Uani 1 1 d .
H2A H 0.3901 0.6625 0.3328 0.054 Uiso 1 1 d R
N3 N 0.5872(2) 0.9026(2) 0.3217(2) 0.0430(7) Uani 1 1 d .
H3 H 0.4007 1.0439 -0.1026 0.052 Uiso 1 1 d R
N4 N 0.5858(2) 0.7665(2) 0.4144(2) 0.0408(7) Uani 1 1 d .
H4 H 0.5644 0.7282 0.4388 0.049 Uiso 1 1 d R
N5 N 0.4001(3) 1.0394(3) 0.0968(3) 0.0512(8) Uani 1 1 d .
N6 N 0.3829(2) 1.0313(2) -0.0541(2) 0.0495(8) Uani 1 1 d .
O1 O 0.5229(2) 0.5902(2) 0.5080(2) 0.0582(8) Uani 1 1 d .
O2 O 0.5885(3) 0.4797(3) 0.3908(3) 0.0950(15) Uani 1 1 d .
S1 S 0.5000 0.5000 0.44923(10) 0.0506(4) 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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
C2 C1 N1 109.8(4) . .
N2 C2 C1 106.3(4) . .
N2 C3 N1 112.1(3) . .
N2 C3 C4 129.1(3) . .
N1 C3 C4 118.7(3) . .
N4 C4 N3 111.7(3) . .
N4 C4 C3 129.9(3) . .
N3 C4 C3 118.3(3) . .
C6 C5 N4 106.6(4) . .
C5 C6 N3 109.7(3) . .
C8 C7 N5 111.0(4) . .
C7 C8 N6 105.1(4) . .
N5 C9 N6 111.0(3) . .
N5 C9 C9 120.0(2) . 6_564
N6 C9 C9 128.9(2) . 6_564
N3 Mn1 N3 97.35(17) 6_564 .
N3 Mn1 N1 75.23(12) 6_564 6_564
N3 Mn1 N1 94.49(12) . 6_564
N3 Mn1 N1 94.49(12) 6_564 .
N3 Mn1 N1 75.23(12) . .
N1 Mn1 N1 164.63(18) 6_564 .
N3 Mn1 N5 96.38(12) 6_564 .
N3 Mn1 N5 158.92(12) . .
N1 Mn1 N5 104.44(13) 6_564 .
N1 Mn1 N5 87.83(12) . .
N3 Mn1 N5 158.92(12) 6_564 6_564
N3 Mn1 N5 96.38(12) . 6_564
N1 Mn1 N5 87.83(12) 6_564 6_564
N1 Mn1 N5 104.44(13) . 6_564
N5 Mn1 N5 75.50(17) . 6_564
C3 N1 C1 104.1(3) . .
C3 N1 Mn1 113.5(2) . .
C1 N1 Mn1 142.2(3) . .
C3 N2 C2 107.6(4) . .
C4 N3 C6 104.5(3) . .
C4 N3 Mn1 113.9(2) . .
C6 N3 Mn1 141.2(3) . .
C4 N4 C5 107.6(3) . .
C9 N5 C7 104.8(4) . .
C9 N5 Mn1 112.2(2) . .
C7 N5 Mn1 142.5(3) . .
C9 N6 C8 108.1(4) . .
O2 S1 O2 108.1(4) . 6_554
O2 S1 O1 108.99(17) . .
O2 S1 O1 110.8(2) 6_554 .
O2 S1 O1 110.8(2) . 6_554
O2 S1 O1 108.99(17) 6_554 6_554
O1 S1 O1 109.1(2) . 6_554
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.358(7) .
C1 N1 1.377(5) .
C2 N2 1.355(5) .
C3 N2 1.326(5) .
C3 N1 1.335(5) .
C3 C4 1.461(5) .
C4 N4 1.326(5) .
C4 N3 1.343(5) .
C5 C6 1.352(5) .
C5 N4 1.371(5) .
C6 N3 1.384(5) .
C7 C8 1.358(7) .
C7 N5 1.363(6) .
C8 N6 1.370(5) .
C9 N5 1.338(5) .
C9 N6 1.339(5) .
C9 C9 1.426(8) 6_564
Mn1 N3 2.240(3) 6_564
Mn1 N3 2.240(3) .
Mn1 N1 2.254(3) 6_564
Mn1 N1 2.254(3) .
Mn1 N5 2.258(4) .
Mn1 N5 2.258(4) 6_564
O1 S1 1.471(3) .
O2 S1 1.443(4) .
S1 O2 1.443(4) 6_554
S1 O1 1.471(3) 6_554
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139198332
