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#$Date: 2019-11-25 07:21:44 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240347 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/96/4129673.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_4129673
loop_
_publ_author_name
'Pinkowicz, Dawid'
'Southerland, Heather I.'
'Avendaño, Carolina'
'Prosvirin, Andrey'
'Sanders, Codi'
'Wernsdorfer, Wolfgang'
'Pedersen, Kasper S.'
'Dreiser, Jan'
'Clérac, Rodolphe'
'Nehrkorn, Joscha'
'Simeoni, Giovanna G.'
'Schnegg, Alexander'
'Holldack, Karsten'
'Dunbar, Kim R.'
_publ_section_title
;
 Cyanide Single-Molecule Magnets Exhibiting Solvent Dependent Reversible
 "On" and "Off" Exchange Bias Behavior.
;
_journal_issue                   45
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14406
_journal_page_last               14422
_journal_paper_doi               10.1021/jacs.5b09378
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C91 H64 Fe Mn2 N11 O13 P2'
_chemical_formula_weight         1747.20
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 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                90.000
_cell_angle_beta                 102.970(11)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   17.237(12)
_cell_length_b                   13.990(9)
_cell_length_c                   37.687(26)
_cell_measurement_temperature    293(2)
_cell_volume                     8856(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.687
_diffrn_measured_fraction_theta_max 0.687
_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  0.0649
_diffrn_reflns_av_sigmaI/netI    0.1165
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            6687
_diffrn_reflns_theta_full        23.24
_diffrn_reflns_theta_max         23.24
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3588
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         4371
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.0631
_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)+(0.0686P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1549
_reflns_number_gt                2523
_reflns_number_total             4371
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ja5b09378_si_005.cif
_cod_data_source_block           mn2fe_wet_xprep
_cod_original_cell_volume        8856(4)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4129673
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Fe01 Fe 0.2500 0.2500 0.0000 0.0332(5) Uani 1 2 d S
Mn02 Mn 0.01268(6) 0.28340(8) 0.05299(3) 0.0353(4) Uani 1 1 d .
P003 P 0.08609(12) 0.68778(18) 0.24977(6) 0.0465(7) Uani 1 1 d .
C1 C 0.1418(4) 0.2682(5) 0.0051(2) 0.032(2) Uani 1 1 d .
C2 C 0.2597(4) 0.1338(7) 0.0295(2) 0.043(2) Uani 1 1 d .
O2 O 0.0859(3) 0.3654(4) 0.08151(14) 0.0465(16) Uani 1 1 d .
C42 C 0.1216(5) 0.7286(6) 0.3232(2) 0.059(3) Uani 1 1 d .
H42 H 0.0673 0.7400 0.3199 0.071 Uiso 1 1 calc R
O52 O 0.1757(3) 0.4307(4) 0.40103(16) 0.0635(18) Uani 1 1 d .
O1 O 0.0632(3) 0.1756(4) 0.07725(14) 0.0456(15) Uani 1 1 d .
N1 N 0.0792(3) 0.2811(5) 0.00904(18) 0.046(2) Uani 1 1 d .
N5 N -0.0738(3) 0.2057(5) 0.02234(16) 0.0335(17) Uani 1 1 d .
O3 O -0.0655(3) 0.2971(4) 0.09753(14) 0.0571(17) Uani 1 1 d .
C31 C 0.1276(5) 0.7609(7) 0.2192(2) 0.046(3) Uani 1 1 d .
N4 N -0.0567(3) 0.3911(5) 0.03016(16) 0.0340(17) Uani 1 1 d .
C25 C 0.0893(4) 0.5650(6) 0.2356(2) 0.044(2) Uani 1 1 d .
N3 N 0.3026(4) 0.3786(6) 0.06804(19) 0.058(2) Uani 1 1 d .
N2 N 0.2674(4) 0.0658(6) 0.0463(2) 0.064(2) Uani 1 1 d .
C18 C 0.0162(4) 0.5143(6) 0.0690(2) 0.035(2) Uani 1 1 d .
C10 C -0.0771(4) 0.1145(6) 0.0234(2) 0.037(2) Uani 1 1 d .
C6 C 0.0932(5) -0.0796(6) 0.0804(2) 0.046(2) Uani 1 1 d .
H6 H 0.1316 -0.1225 0.0922 0.055 Uiso 1 1 calc R
C3 C 0.2837(4) 0.3297(6) 0.0427(2) 0.042(2) Uani 1 1 d .
C4 C 0.0489(4) 0.0851(6) 0.0696(2) 0.032(2) Uani 1 1 d .
C26 C 0.1114(5) 0.4926(7) 0.2607(3) 0.066(3) Uani 1 1 d .
H26 H 0.1299 0.5081 0.2851 0.079 Uiso 1 1 calc R
C8 C -0.0305(5) -0.0491(6) 0.0391(2) 0.046(2) Uani 1 1 d .
H8 H -0.0764 -0.0713 0.0233 0.055 Uiso 1 1 calc R
C7 C 0.0260(5) -0.1145(6) 0.0567(2) 0.050(2) Uani 1 1 d .
H7 H 0.0188 -0.1798 0.0527 0.060 Uiso 1 1 calc R
C9 C -0.0195(4) 0.0501(6) 0.0445(2) 0.033(2) Uani 1 1 d .
C15 C -0.1726(4) 0.4231(6) -0.0213(2) 0.044(2) Uani 1 1 d .
H15 H -0.1656 0.4888 -0.0190 0.053 Uiso 1 1 calc R
N26 N 0.0000 0.7249(7) 0.2500 0.049(3) Uani 1 2 d S
C36 C 0.0972(5) 0.8521(8) 0.2118(3) 0.070(3) Uani 1 1 d .
H36 H 0.0545 0.8732 0.2210 0.084 Uiso 1 1 calc R
C5 C 0.1050(4) 0.0158(6) 0.0871(2) 0.040(2) Uani 1 1 d .
H5 H 0.1508 0.0360 0.1034 0.049 Uiso 1 1 calc R
C23 C 0.0811(4) 0.4578(6) 0.0870(2) 0.038(2) Uani 1 1 d .
C32 C 0.1899(6) 0.7321(8) 0.2053(3) 0.063(3) Uani 1 1 d .
H32 H 0.2101 0.6707 0.2104 0.076 Uiso 1 1 calc R
C30 C 0.0648(5) 0.5410(7) 0.1992(2) 0.058(3) Uani 1 1 d .
H30 H 0.0499 0.5886 0.1818 0.069 Uiso 1 1 calc R
C24 C -0.0609(5) 0.2370(7) 0.1269(2) 0.076(3) Uani 1 1 d .
H24A H -0.0980 0.2575 0.1409 0.114 Uiso 1 1 calc R
H24B H -0.0079 0.2386 0.1419 0.114 Uiso 1 1 calc R
H24C H -0.0736 0.1729 0.1184 0.114 Uiso 1 1 calc R
C16 C -0.1222(4) 0.3599(6) 0.00193(19) 0.034(2) Uani 1 1 d .
C17 C -0.0472(4) 0.4803(7) 0.0407(2) 0.039(2) Uani 1 1 d .
C21 C 0.1397(5) 0.5969(7) 0.1198(2) 0.055(3) Uani 1 1 d .
H21 H 0.1816 0.6249 0.1364 0.067 Uiso 1 1 calc R
C13 C -0.2426(4) 0.2852(7) -0.0515(2) 0.049(3) Uani 1 1 d .
H13 H -0.2843 0.2605 -0.0691 0.059 Uiso 1 1 calc R
C19 C 0.0151(5) 0.6125(6) 0.0779(2) 0.058(3) Uani 1 1 d .
H19 H -0.0273 0.6504 0.0662 0.069 Uiso 1 1 calc R
C12 C -0.1917(4) 0.2241(6) -0.0296(2) 0.044(2) Uani 1 1 d .
H12 H -0.1976 0.1583 -0.0327 0.053 Uiso 1 1 calc R
C22 C 0.1431(4) 0.5021(6) 0.1121(2) 0.044(2) Uani 1 1 d .
H22 H 0.1870 0.4664 0.1236 0.052 Uiso 1 1 calc R
C41 C 0.1706(6) 0.7417(6) 0.3571(2) 0.073(3) Uani 1 1 d .
H41 H 0.1489 0.7604 0.3765 0.088 Uiso 1 1 calc R
C20 C 0.0755(5) 0.6524(6) 0.1033(2) 0.064(3) Uani 1 1 d .
H20 H 0.0732 0.7165 0.1095 0.077 Uiso 1 1 calc R
C29 C 0.0624(5) 0.4462(9) 0.1888(3) 0.074(3) Uani 1 1 d .
H29 H 0.0460 0.4306 0.1643 0.088 Uiso 1 1 calc R
C52 C 0.1451(6) 0.4923(8) 0.3705(3) 0.087(4) Uani 1 1 d .
C27 C 0.1068(6) 0.3980(8) 0.2504(3) 0.088(4) Uani 1 1 d .
H27 H 0.1189 0.3499 0.2678 0.105 Uiso 1 1 calc R
C33 C 0.2243(6) 0.7915(11) 0.1836(3) 0.076(3) Uani 1 1 d .
H33 H 0.2666 0.7704 0.1741 0.091 Uiso 1 1 calc R
C11 C -0.1309(4) 0.2617(6) -0.00263(19) 0.032(2) Uani 1 1 d .
C40 C 0.2494(7) 0.7276(7) 0.3624(3) 0.082(4) Uani 1 1 d .
H40 H 0.2821 0.7373 0.3854 0.099 Uiso 1 1 calc R
C14 C -0.2335(4) 0.3843(7) -0.0479(2) 0.053(3) Uani 1 1 d .
H14 H -0.2684 0.4245 -0.0635 0.063 Uiso 1 1 calc R
C28 C 0.0837(6) 0.3755(7) 0.2137(3) 0.074(3) Uani 1 1 d .
H28 H 0.0827 0.3121 0.2062 0.089 Uiso 1 1 calc R
C38 C 0.2324(5) 0.6845(7) 0.2994(3) 0.078(3) Uani 1 1 d .
H38 H 0.2541 0.6653 0.2801 0.093 Uiso 1 1 calc R
C39 C 0.2816(6) 0.6990(9) 0.3341(3) 0.090(4) Uani 1 1 d .
H39 H 0.3362 0.6891 0.3379 0.108 Uiso 1 1 calc R
C34 C 0.1947(7) 0.8820(12) 0.1767(3) 0.092(4) Uani 1 1 d .
H34 H 0.2175 0.9235 0.1627 0.111 Uiso 1 1 calc R
C35 C 0.1321(7) 0.9114(9) 0.1902(3) 0.103(5) Uani 1 1 d .
H35 H 0.1120 0.9727 0.1849 0.124 Uiso 1 1 calc R
C37 C 0.1518(5) 0.6990(6) 0.2943(2) 0.047(3) Uani 1 1 d .
O50 O 0.3593(3) 0.4915(5) 0.12823(15) 0.0720(19) Uani 1 1 d .
C50 C 0.4425(5) 0.4657(7) 0.1381(3) 0.075(3) Uani 1 1 d .
O51 O 0.1835(4) 1.0566(7) 0.3115(2) 0.114(3) Uani 1 1 d .
O53 O 0.0000 0.126(2) 0.2500 0.337(12) Uiso 1 2 d S
C53 C 0.089(2) 0.152(4) 0.2555(11) 0.250(19) Uiso 0.50 1 d P
C51 C 0.2031(9) 0.9726(11) 0.2931(3) 0.131(5) Uani 1 1 d .
H17 H -0.082(4) 0.536(6) 0.0275(19) 0.06(2) Uiso 1 1 d .
H11 H -0.115(4) 0.078(5) 0.0075(17) 0.03(2) Uiso 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'
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'
P P 0.1023 0.0942 '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'
Fe Fe 0.3463 0.8444 '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'
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
C1 Fe01 C1 180.0(4) . 7
C1 Fe01 C3 92.4(3) . 7
C1 Fe01 C3 87.6(3) 7 7
C1 Fe01 C3 87.6(3) . .
C1 Fe01 C3 92.4(3) 7 .
C3 Fe01 C3 180.0(6) 7 .
C1 Fe01 C2 89.2(3) . 7
C1 Fe01 C2 90.8(3) 7 7
C3 Fe01 C2 92.0(3) 7 7
C3 Fe01 C2 88.0(3) . 7
C1 Fe01 C2 90.8(3) . .
C1 Fe01 C2 89.2(3) 7 .
C3 Fe01 C2 88.0(3) 7 .
C3 Fe01 C2 92.0(3) . .
C2 Fe01 C2 180.0(5) 7 .
O2 Mn02 O1 91.9(2) . .
O2 Mn02 N5 174.3(2) . .
O1 Mn02 N5 92.8(2) . .
O2 Mn02 N4 92.7(2) . .
O1 Mn02 N4 170.5(2) . .
N5 Mn02 N4 82.2(2) . .
O2 Mn02 N1 92.5(2) . .
O1 Mn02 N1 95.2(2) . .
N5 Mn02 N1 90.2(2) . .
N4 Mn02 N1 92.8(2) . .
O2 Mn02 O3 87.8(2) . .
O1 Mn02 O3 89.7(2) . .
N5 Mn02 O3 89.1(2) . .
N4 Mn02 O3 82.2(2) . .
N1 Mn02 O3 175.0(2) . .
N26 P003 C25 114.1(4) . .
N26 P003 C31 109.0(4) . .
C25 P003 C31 108.0(4) . .
N26 P003 C37 111.2(4) . .
C25 P003 C37 107.6(4) . .
C31 P003 C37 106.7(4) . .
N1 C1 Fe01 177.6(7) . .
N2 C2 Fe01 177.9(8) . .
C23 O2 Mn02 129.8(4) . .
C37 C42 C41 121.0(9) . .
C4 O1 Mn02 128.9(4) . .
C1 N1 Mn02 140.0(6) . .
C10 N5 C11 122.6(6) . .
C10 N5 Mn02 123.9(5) . .
C11 N5 Mn02 113.4(5) . .
C24 O3 Mn02 125.2(5) . .
C32 C31 C36 119.4(9) . .
C32 C31 P003 122.7(8) . .
C36 C31 P003 117.7(8) . .
C17 N4 C16 122.6(6) . .
C17 N4 Mn02 124.6(5) . .
C16 N4 Mn02 112.7(5) . .
C26 C25 C30 118.5(9) . .
C26 C25 P003 121.3(7) . .
C30 C25 P003 120.1(7) . .
C23 C18 C19 118.7(7) . .
C23 C18 C17 124.3(8) . .
C19 C18 C17 116.9(7) . .
N5 C10 C9 127.8(7) . .
C5 C6 C7 122.2(7) . .
N3 C3 Fe01 178.6(8) . .
O1 C4 C5 118.9(6) . .
O1 C4 C9 124.4(7) . .
C5 C4 C9 116.7(8) . .
C27 C26 C25 121.6(9) . .
C7 C8 C9 121.4(7) . .
C6 C7 C8 118.2(8) . .
C8 C9 C4 120.0(7) . .
C8 C9 C10 118.8(7) . .
C4 C9 C10 121.2(8) . .
C14 C15 C16 117.9(8) . .
P003 N26 P003 141.4(7) 2 .
C31 C36 C35 118.4(10) . .
C6 C5 C4 121.6(7) . .
O2 C23 C22 118.5(7) . .
O2 C23 C18 123.0(7) . .
C22 C23 C18 118.5(9) . .
C31 C32 C33 122.0(10) . .
C29 C30 C25 119.8(9) . .
C11 C16 C15 120.8(7) . .
C11 C16 N4 116.0(6) . .
C15 C16 N4 123.2(8) . .
N4 C17 C18 124.6(7) . .
C22 C21 C20 121.4(8) . .
C12 C13 C14 121.4(7) . .
C20 C19 C18 121.0(8) . .
C13 C12 C11 118.8(8) . .
C21 C22 C23 120.8(8) . .
C40 C41 C42 120.6(11) . .
C19 C20 C21 119.6(9) . .
C28 C29 C30 121.2(10) . .
C26 C27 C28 119.0(10) . .
C34 C33 C32 118.4(11) . .
C16 C11 C12 120.5(7) . .
C16 C11 N5 114.9(6) . .
C12 C11 N5 124.6(8) . .
C41 C40 C39 120.1(10) . .
C15 C14 C13 120.4(7) . .
C29 C28 C27 119.7(10) . .
C37 C38 C39 119.3(11) . .
C40 C39 C38 120.1(10) . .
C35 C34 C33 120.3(13) . .
C34 C35 C36 121.6(12) . .
C42 C37 C38 118.9(8) . .
C42 C37 P003 119.6(6) . .
C38 C37 P003 121.4(8) . .
C53 O53 C53 152(4) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe01 C1 1.933(7) .
Fe01 C1 1.933(7) 7
Fe01 C3 1.937(9) 7
Fe01 C3 1.937(9) .
Fe01 C2 1.956(9) 7
Fe01 C2 1.956(9) .
Mn02 O2 1.859(5) .
Mn02 O1 1.874(5) .
Mn02 N5 1.991(6) .
Mn02 N4 1.994(6) .
Mn02 N1 2.216(7) .
Mn02 O3 2.384(6) .
P003 N26 1.574(4) .
P003 C25 1.803(9) .
P003 C31 1.804(9) .
P003 C37 1.807(8) .
C1 N1 1.137(8) .
C2 N2 1.133(9) .
O2 C23 1.314(9) .
C42 C37 1.375(11) .
C42 C41 1.375(10) .
O52 C52 1.440(10) .
O1 C4 1.310(8) .
N5 C10 1.278(9) .
N5 C11 1.432(8) .
O3 C24 1.380(9) .
C31 C32 1.357(11) .
C31 C36 1.384(12) .
N4 C17 1.309(9) .
N4 C16 1.434(8) .
C25 C26 1.378(11) .
C25 C30 1.384(10) .
N3 C3 1.161(9) .
C18 C23 1.414(10) .
C18 C19 1.415(11) .
C18 C17 1.425(10) .
C10 C9 1.440(10) .
C6 C5 1.365(10) .
C6 C7 1.383(9) .
C4 C5 1.422(10) .
C4 C9 1.423(9) .
C26 C27 1.376(12) .
C8 C7 1.392(10) .
C8 C9 1.410(10) .
C15 C14 1.388(10) .
C15 C16 1.401(10) .
N26 P003 1.574(4) 2
C36 C35 1.389(13) .
C23 C22 1.402(9) .
C32 C33 1.389(13) .
C30 C29 1.380(12) .
C16 C11 1.389(10) .
C21 C22 1.361(11) .
C21 C20 1.380(11) .
C13 C12 1.362(10) .
C13 C14 1.398(11) .
C19 C20 1.366(10) .
C12 C11 1.390(9) .
C41 C40 1.343(13) .
C29 C28 1.357(12) .
C27 C28 1.386(13) .
C33 C34 1.367(14) .
C40 C39 1.368(14) .
C38 C37 1.374(11) .
C38 C39 1.406(11) .
C34 C35 1.356(15) .
O50 C50 1.446(9) .
O51 C51 1.442(14) .
O53 C53 1.55(4) .
O53 C53 1.55(4) 2
