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#$Date: 2025-08-20 23:21:57 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301837 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/68/4316886.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_4316886
loop_
_publ_author_name
'Shi Wang'
'Marilena Ferbinteanu'
'Crina Marinescu'
'Alexandra Dobrinescu'
'Qi-Dan Ling'
'Wei Huang'
_publ_section_title
;
 Case Study on a Rare Effect: The Experimental and Theoretical Analysis of
 a Manganese(III) Spin-Crossover System
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9839
_journal_page_last               9851
_journal_paper_doi               10.1021/ic100364v
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C22 H26 Br2 Mn N4 O2, Cl O4'
_chemical_formula_sum            'C22 H26 Br2 Cl Mn N4 O6'
_chemical_formula_weight         692.66
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_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                 94.918(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.6307(16)
_cell_length_b                   8.0827(7)
_cell_length_c                   18.1802(17)
_cell_measurement_reflns_used    7889
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.8955
_cell_measurement_theta_min      2.1845
_cell_volume                     2581.2(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0658
_diffrn_reflns_av_sigmaI/netI    0.1251
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18212
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.16
_diffrn_standards_number         7752
_exptl_absorpt_coefficient_mu    3.756
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.588
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.797
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.797
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0400P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                3368
_reflns_number_total             5933
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100364v_si_001_1.cif
_cod_data_source_block           mono
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               4316886
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0518(2) 0.1249(5) 0.1130(2) 0.0158(10) Uani 1 1 d . . .
C2 C -0.1160(2) 0.1084(6) 0.0629(2) 0.0193(10) Uani 1 1 d . . .
H1 H -0.1510 0.1976 0.0560 0.023 Uiso 1 1 calc R . .
C3 C -0.1293(2) -0.0362(6) 0.0230(2) 0.0200(11) Uani 1 1 d . . .
H2 H -0.1739 -0.0473 -0.0099 0.024 Uiso 1 1 calc R . .
C4 C -0.0768(3) -0.1657(5) 0.0315(2) 0.0185(10) Uani 1 1 d . . .
C5 C -0.0108(2) -0.1484(5) 0.0759(2) 0.0168(10) Uani 1 1 d . . .
H3 H 0.0264 -0.2338 0.0781 0.020 Uiso 1 1 calc R . .
C6 C 0.0022(2) -0.0047(5) 0.1182(2) 0.0164(10) Uani 1 1 d . . .
Br1 Br -0.09962(3) -0.36759(6) -0.01918(3) 0.02482(13) Uani 1 1 d . . .
C7 C 0.0747(3) 0.0144(5) 0.1606(2) 0.0189(10) Uani 1 1 d . . .
H4 H 0.1155 -0.0539 0.1479 0.023 Uiso 1 1 calc R . .
N1 N 0.08831(19) 0.1170(4) 0.21416(19) 0.0169(8) Uani 1 1 d . . .
C8 C 0.1678(2) 0.1397(6) 0.2456(2) 0.0214(10) Uani 1 1 d . . .
H5 H 0.2005 0.0544 0.2254 0.026 Uiso 1 1 calc R . .
H6 H 0.1705 0.1255 0.2999 0.026 Uiso 1 1 calc R . .
C9 C 0.1971(2) 0.3108(5) 0.2275(2) 0.0222(11) Uani 1 1 d . . .
H7 H 0.2522 0.3157 0.2434 0.027 Uiso 1 1 calc R . .
H8 H 0.1913 0.3253 0.1732 0.027 Uiso 1 1 calc R . .
C10 C 0.1581(3) 0.4541(5) 0.2625(3) 0.0231(11) Uani 1 1 d . . .
H9 H 0.1596 0.4357 0.3164 0.028 Uiso 1 1 calc R . .
H10 H 0.1865 0.5572 0.2542 0.028 Uiso 1 1 calc R . .
N2 N 0.0773(2) 0.4752(5) 0.2322(2) 0.0204(9) Uani 1 1 d . . .
H11 H 0.082(2) 0.490(4) 0.184(2) 0.000(10) Uiso 1 1 d . . .
C11 C 0.0423(3) 0.6230(5) 0.2618(3) 0.0282(12) Uani 1 1 d . . .
H12 H 0.0662 0.7238 0.2431 0.034 Uiso 1 1 calc R . .
H13 H 0.0505 0.6233 0.3164 0.034 Uiso 1 1 calc R . .
Mn1 Mn 0.0000 0.26492(11) 0.2500 0.0162(2) Uani 1 2 d S . .
O1 O -0.04270(16) 0.2636(3) 0.15238(15) 0.0172(7) Uani 1 1 d . . .
C12 C 0.3828(2) 0.1919(5) 0.3289(2) 0.0184(10) Uani 1 1 d . . .
C13 C 0.3519(2) 0.1876(6) 0.3971(3) 0.0254(11) Uani 1 1 d . . .
H14 H 0.3536 0.2845 0.4268 0.030 Uiso 1 1 calc R . .
C14 C 0.3190(3) 0.0463(6) 0.4221(3) 0.0261(12) Uani 1 1 d . . .
H15 H 0.3003 0.0437 0.4696 0.031 Uiso 1 1 calc R . .
C15 C 0.3137(3) -0.0937(6) 0.3766(3) 0.0246(11) Uani 1 1 d . . .
Br2 Br 0.26975(3) -0.29186(6) 0.41145(3) 0.03373(15) Uani 1 1 d . . .
C16 C 0.3378(2) -0.0898(6) 0.3074(3) 0.0225(11) Uani 1 1 d . . .
H16 H 0.3301 -0.1828 0.2757 0.027 Uiso 1 1 calc R . .
C17 C 0.3742(2) 0.0528(6) 0.2831(2) 0.0192(10) Uani 1 1 d . . .
C18 C 0.3938(2) 0.0587(6) 0.2079(3) 0.0225(11) Uani 1 1 d . . .
H17 H 0.3696 -0.0177 0.1738 0.027 Uiso 1 1 calc R . .
N3 N 0.4422(2) 0.1609(5) 0.1837(2) 0.0208(9) Uani 1 1 d . . .
C19 C 0.4437(3) 0.1735(6) 0.1033(2) 0.0262(12) Uani 1 1 d . . .
H18 H 0.4147 0.0806 0.0792 0.031 Uiso 1 1 calc R . .
H19 H 0.4970 0.1659 0.0901 0.031 Uiso 1 1 calc R . .
C20 C 0.4090(3) 0.3375(6) 0.0758(3) 0.0339(13) Uani 1 1 d . . .
H20 H 0.4052 0.3375 0.0212 0.041 Uiso 1 1 calc R . .
H21 H 0.3567 0.3454 0.0914 0.041 Uiso 1 1 calc R . .
C21 C 0.4533(3) 0.4900(6) 0.1033(3) 0.0363(14) Uani 1 1 d . . .
H22 H 0.5062 0.4813 0.0892 0.044 Uiso 1 1 calc R . .
H23 H 0.4299 0.5891 0.0787 0.044 Uiso 1 1 calc R . .
N4 N 0.4549(2) 0.5110(5) 0.1834(3) 0.0304(11) Uani 1 1 d . . .
H24 H 0.414(2) 0.522(5) 0.193(2) 0.000(11) Uiso 1 1 d . . .
C22 C 0.4954(3) 0.6631(6) 0.2087(3) 0.0406(14) Uani 1 1 d . . .
H25 H 0.4661 0.7616 0.1906 0.049 Uiso 1 1 calc R . .
H26 H 0.5460 0.6671 0.1889 0.049 Uiso 1 1 calc R . .
Mn2 Mn 0.5000 0.32294(12) 0.2500 0.0198(2) Uani 1 2 d S . .
O2 O 0.41695(16) 0.3294(4) 0.30834(16) 0.0220(7) Uani 1 1 d . . .
Cl1 Cl 0.25020(6) 0.70432(13) 0.10414(6) 0.0193(2) Uani 1 1 d . . .
O3 O 0.26062(18) 0.8806(4) 0.10170(17) 0.0294(8) Uani 1 1 d . . .
O4 O 0.17186(16) 0.6687(4) 0.11355(17) 0.0233(7) Uani 1 1 d . . .
O5 O 0.27186(18) 0.6322(4) 0.03761(16) 0.0303(8) Uani 1 1 d . . .
O6 O 0.29758(17) 0.6391(4) 0.16666(17) 0.0279(8) Uani 1 1 d . . .
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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
O1 C1 C2 119.0(4) . . ?
O1 C1 C6 122.6(4) . . ?
C2 C1 C6 118.4(4) . . ?
C3 C2 C1 120.9(4) . . ?
C3 C2 H1 119.6 . . ?
C1 C2 H1 119.6 . . ?
C2 C3 C4 119.6(4) . . ?
C2 C3 H2 120.2 . . ?
C4 C3 H2 120.2 . . ?
C5 C4 C3 120.8(4) . . ?
C5 C4 Br1 120.5(3) . . ?
C3 C4 Br1 118.7(3) . . ?
C4 C5 C6 120.0(4) . . ?
C4 C5 H3 120.0 . . ?
C6 C5 H3 120.0 . . ?
C5 C6 C1 120.1(4) . . ?
C5 C6 C7 118.5(4) . . ?
C1 C6 C7 121.1(4) . . ?
N1 C7 C6 124.9(4) . . ?
N1 C7 H4 117.6 . . ?
C6 C7 H4 117.6 . . ?
C7 N1 C8 118.8(4) . . ?
C7 N1 Mn1 120.3(3) . . ?
C8 N1 Mn1 120.7(3) . . ?
N1 C8 C9 110.9(3) . . ?
N1 C8 H5 109.5 . . ?
C9 C8 H5 109.5 . . ?
N1 C8 H6 109.5 . . ?
C9 C8 H6 109.5 . . ?
H5 C8 H6 108.0 . . ?
C10 C9 C8 115.4(4) . . ?
C10 C9 H7 108.4 . . ?
C8 C9 H7 108.4 . . ?
C10 C9 H8 108.4 . . ?
C8 C9 H8 108.4 . . ?
H7 C9 H8 107.5 . . ?
N2 C10 C9 112.7(4) . . ?
N2 C10 H9 109.1 . . ?
C9 C10 H9 109.1 . . ?
N2 C10 H10 109.1 . . ?
C9 C10 H10 109.1 . . ?
H9 C10 H10 107.8 . . ?
C11 N2 C10 112.0(3) . . ?
C11 N2 Mn1 106.7(3) . . ?
C10 N2 Mn1 115.9(3) . . ?
C11 N2 H11 109(2) . . ?
C10 N2 H11 103(2) . . ?
Mn1 N2 H11 111(2) . . ?
N2 C11 C11 109.3(3) . 2 ?
N2 C11 H12 109.8 . . ?
C11 C11 H12 109.8 2 . ?
N2 C11 H13 109.8 . . ?
C11 C11 H13 109.8 2 . ?
H12 C11 H13 108.3 . . ?
O1 Mn1 O1 179.34(18) 2 . ?
O1 Mn1 N1 87.21(13) 2 2 ?
O1 Mn1 N1 92.41(13) . 2 ?
O1 Mn1 N1 92.41(13) 2 . ?
O1 Mn1 N1 87.21(13) . . ?
N1 Mn1 N1 110.96(19) 2 . ?
O1 Mn1 N2 86.59(14) 2 . ?
O1 Mn1 N2 93.92(14) . . ?
N1 Mn1 N2 163.26(14) 2 . ?
N1 Mn1 N2 84.83(14) . . ?
O1 Mn1 N2 93.92(14) 2 2 ?
O1 Mn1 N2 86.59(13) . 2 ?
N1 Mn1 N2 84.83(13) 2 2 ?
N1 Mn1 N2 163.26(14) . 2 ?
N2 Mn1 N2 80.1(2) . 2 ?
C1 O1 Mn1 122.4(3) . . ?
O2 C12 C13 119.3(4) . . ?
O2 C12 C17 122.1(4) . . ?
C13 C12 C17 118.5(4) . . ?
C14 C13 C12 121.5(4) . . ?
C14 C13 H14 119.3 . . ?
C12 C13 H14 119.3 . . ?
C13 C14 C15 118.9(4) . . ?
C13 C14 H15 120.5 . . ?
C15 C14 H15 120.5 . . ?
C16 C15 C14 121.1(4) . . ?
C16 C15 Br2 119.6(4) . . ?
C14 C15 Br2 119.3(4) . . ?
C15 C16 C17 119.7(4) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C12 C17 C16 120.0(4) . . ?
C12 C17 C18 121.0(4) . . ?
C16 C17 C18 118.5(4) . . ?
N3 C18 C17 124.3(4) . . ?
N3 C18 H17 117.8 . . ?
C17 C18 H17 117.8 . . ?
C18 N3 C19 116.9(4) . . ?
C18 N3 Mn2 122.1(3) . . ?
C19 N3 Mn2 120.2(3) . . ?
N3 C19 C20 110.2(4) . . ?
N3 C19 H18 109.6 . . ?
C20 C19 H18 109.6 . . ?
N3 C19 H19 109.6 . . ?
C20 C19 H19 109.6 . . ?
H18 C19 H19 108.1 . . ?
C21 C20 C19 114.6(4) . . ?
C21 C20 H20 108.6 . . ?
C19 C20 H20 108.6 . . ?
C21 C20 H21 108.6 . . ?
C19 C20 H21 108.6 . . ?
H20 C20 H21 107.6 . . ?
N4 C21 C20 112.7(4) . . ?
N4 C21 H22 109.0 . . ?
C20 C21 H22 109.0 . . ?
N4 C21 H23 109.0 . . ?
C20 C21 H23 109.0 . . ?
H22 C21 H23 107.8 . . ?
C21 N4 C22 112.0(4) . . ?
C21 N4 Mn2 118.2(3) . . ?
C22 N4 Mn2 106.2(3) . . ?
C21 N4 H24 108(3) . . ?
C22 N4 H24 106(3) . . ?
Mn2 N4 H24 106(3) . . ?
N4 C22 C22 108.7(3) . 2_655 ?
N4 C22 H25 110.0 . . ?
C22 C22 H25 110.0 2_655 . ?
N4 C22 H26 110.0 . . ?
C22 C22 H26 110.0 2_655 . ?
H25 C22 H26 108.3 . . ?
O2 Mn2 O2 176.83(19) . 2_655 ?
O2 Mn2 N3 88.67(14) . . ?
O2 Mn2 N3 93.41(14) 2_655 . ?
O2 Mn2 N3 93.41(14) . 2_655 ?
O2 Mn2 N3 88.67(14) 2_655 2_655 ?
N3 Mn2 N3 98.1(2) . 2_655 ?
O2 Mn2 N4 85.87(15) . 2_655 ?
O2 Mn2 N4 91.79(15) 2_655 2_655 ?
N3 Mn2 N4 171.48(16) . 2_655 ?
N3 Mn2 N4 88.75(16) 2_655 2_655 ?
O2 Mn2 N4 91.79(15) . . ?
O2 Mn2 N4 85.87(15) 2_655 . ?
N3 Mn2 N4 88.75(16) . . ?
N3 Mn2 N4 171.48(16) 2_655 . ?
N4 Mn2 N4 84.9(3) 2_655 . ?
C12 O2 Mn2 121.8(3) . . ?
O5 Cl1 O4 110.48(19) . . ?
O5 Cl1 O3 109.6(2) . . ?
O4 Cl1 O3 109.22(18) . . ?
O5 Cl1 O6 109.78(19) . . ?
O4 Cl1 O6 109.22(18) . . ?
O3 Cl1 O6 108.53(19) . . ?
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
C1 O1 1.332(5) . ?
C1 C2 1.399(6) . ?
C1 C6 1.413(6) . ?
C2 C3 1.384(6) . ?
C2 H1 0.9500 . ?
C3 C4 1.396(6) . ?
C3 H2 0.9500 . ?
C4 C5 1.367(6) . ?
C4 Br1 1.900(4) . ?
C5 C6 1.401(6) . ?
C5 H3 0.9500 . ?
C6 C7 1.443(6) . ?
C7 N1 1.286(5) . ?
C7 H4 0.9500 . ?
N1 C8 1.479(5) . ?
N1 Mn1 2.110(3) . ?
C8 C9 1.522(6) . ?
C8 H5 0.9900 . ?
C8 H6 0.9900 . ?
C9 C10 1.515(6) . ?
C9 H7 0.9900 . ?
C9 H8 0.9900 . ?
C10 N2 1.492(6) . ?
C10 H9 0.9900 . ?
C10 H10 0.9900 . ?
N2 C11 1.469(5) . ?
N2 Mn1 2.220(4) . ?
N2 H11 0.89(3) . ?
C11 C11 1.518(9) 2 ?
C11 H12 0.9900 . ?
C11 H13 0.9900 . ?
Mn1 O1 1.867(3) 2 ?
Mn1 O1 1.867(3) . ?
Mn1 N1 2.110(3) 2 ?
Mn1 N2 2.220(4) 2 ?
C12 O2 1.333(5) . ?
C12 C13 1.396(6) . ?
C12 C17 1.399(6) . ?
C13 C14 1.377(6) . ?
C13 H14 0.9500 . ?
C14 C15 1.401(6) . ?
C14 H15 0.9500 . ?
C15 C16 1.362(6) . ?
C15 Br2 1.911(5) . ?
C16 C17 1.409(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.440(6) . ?
C18 N3 1.291(5) . ?
C18 H17 0.9500 . ?
N3 C19 1.468(5) . ?
N3 Mn2 1.999(4) . ?
C19 C20 1.527(6) . ?
C19 H18 0.9900 . ?
C19 H19 0.9900 . ?
C20 C21 1.519(7) . ?
C20 H20 0.9900 . ?
C20 H21 0.9900 . ?
C21 N4 1.464(6) . ?
C21 H22 0.9900 . ?
C21 H23 0.9900 . ?
N4 C22 1.475(6) . ?
N4 Mn2 2.060(4) . ?
N4 H24 0.77(4) . ?
C22 C22 1.497(10) 2_655 ?
C22 H25 0.9900 . ?
C22 H26 0.9900 . ?
Mn2 O2 1.881(3) . ?
Mn2 O2 1.881(3) 2_655 ?
Mn2 N3 1.999(4) 2_655 ?
Mn2 N4 2.060(4) 2_655 ?
Cl1 O5 1.424(3) . ?
Cl1 O4 1.435(3) . ?
Cl1 O3 1.438(3) . ?
Cl1 O6 1.451(3) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139132605
