#------------------------------------------------------------------------------
#$Date: 2016-03-21 19:11:46 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178839 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/93/4109348.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_4109348
loop_
_publ_author_name
'Masayuki Nihei'
'Lingqin Han'
'Hiroki Oshio'
_publ_section_title
;
 Magnetic Bistability and Single-Crystal-to-Single-Crystal Transformation
 Induced by Guest Desorption
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5312
_journal_page_last               5313
_journal_paper_doi               10.1021/ja069120i
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C50 H38 B2 F8 Fe3 N10 O'
_chemical_formula_weight         1136.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_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                90.00
_cell_angle_beta                 126.364(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.04(2)
_cell_length_b                   12.792(12)
_cell_length_c                   19.806(19)
_cell_measurement_temperature    100
_cell_volume                     5109(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.893
_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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0860
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14068
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.918
_exptl_absorpt_correction_T_max  0.9138
_exptl_absorpt_correction_T_min  0.8377
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       lozenge
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.992
_refine_diff_density_min         -1.371
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1650
_refine_ls_R_factor_gt           0.1317
_refine_ls_shift/su_max          1.148
_refine_ls_shift/su_mean         0.049
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1336P)²+159.4841P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3394
_refine_ls_wR_factor_ref         0.3631
_reflns_number_gt                3739
_reflns_number_total             5520
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja069120isi20070103_122218.cif
_cod_data_source_block           Et2O_110K
_cod_original_cell_volume        5108(8)
_cod_database_code               4109348
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.15606(13) 0.2500 0.0280(4) Uani 1 2 d S . .
Fe2 Fe 0.39914(7) 0.15847(11) 0.26736(10) 0.0416(5) Uani 1 1 d . . .
F1 F 0.1162(3) 0.4088(7) 0.0587(5) 0.077(2) Uani 1 1 d . A .
F3 F 0.218(3) 0.362(5) 0.160(4) 0.056(13) Uani 0.4(2) 1 d P A 1
F3' F 0.226(2) 0.365(3) 0.145(4) 0.063(13) Uani 0.6(2) 1 d P A 2
F2 F 0.1906(4) 0.4618(7) 0.0379(6) 0.083(2) Uani 1 1 d . A .
F4 F 0.1630(6) 0.2915(7) 0.0235(6) 0.117(4) Uani 1 1 d . A .
N1 N 0.0729(3) 0.1528(6) 0.2452(5) 0.0346(16) Uani 1 1 d . . .
C1 C 0.0719(5) 0.2086(8) 0.1858(7) 0.043(2) Uani 1 1 d . . .
C2 C 0.11876(16) 0.2031(2) 0.1717(2) 0.062(3) Uani 1 1 d . . .
H2 H 0.1154 0.2425 0.1300 0.074 Uiso 1 1 calc R . .
C3 C 0.17189(16) 0.1359(2) 0.2225(2) 0.063(3) Uani 1 1 d R . .
C4 C 0.17531(16) 0.0778(2) 0.2842(2) 0.065(4) Uani 1 1 d R . .
H4 H 0.2109 0.0329 0.3182 0.078 Uiso 1 1 d R . .
C5 C 0.12559(16) 0.0868(2) 0.2952(2) 0.045(2) Uani 1 1 d R . .
N3 N 0.11586(16) 0.0358(2) 0.3474(2) 0.043(2) Uani 1 1 d R . .
N2 N 0.05622(16) 0.0490(2) 0.3368(2) 0.0399(18) Uani 1 1 d R . .
N5 N 0.01585(16) 0.2713(2) 0.1433(2) 0.046(2) Uani 1 1 d R . .
N4 N -0.02792(16) 0.2635(2) 0.1625(2) 0.0383(18) Uani 1 1 d R . .
C9 C -0.00774(16) 0.3462(2) 0.0801(2) 0.079(5) Uani 1 1 d R . .
H9 H 0.0125 0.3675 0.0554 0.095 Uiso 1 1 d R . .
C10 C -0.0666(9) 0.3822(10) 0.0618(8) 0.080(5) Uani 1 1 d . . .
H10 H -0.0945 0.4322 0.0220 0.096 Uiso 1 1 calc R . .
C11 C -0.0755(7) 0.3307(8) 0.1128(7) 0.059(3) Uani 1 1 d . . .
H11 H -0.1120 0.3412 0.1133 0.071 Uiso 1 1 calc R . .
C6 C 0.1558(7) -0.0324(10) 0.4119(9) 0.073(4) Uani 1 1 d . . .
H6 H 0.1987 -0.0523 0.4329 0.088 Uiso 1 1 calc R . .
C7 C 0.1208(8) -0.0641(11) 0.4382(8) 0.078(5) Uani 1 1 d . . .
H7 H 0.1347 -0.1131 0.4803 0.094 Uiso 1 1 calc R . .
C12 C 0.2204(7) 0.1256(10) 0.2013(11) 0.074(4) Uani 1 1 d . . .
H12 H 0.2086 0.1610 0.1532 0.089 Uiso 1 1 calc R . .
C8 C 0.0604(6) -0.0131(10) 0.3934(7) 0.058(3) Uani 1 1 d . . .
H8 H 0.0277 -0.0212 0.4016 0.070 Uiso 1 1 calc R . .
C13 C 0.2702(9) 0.0802(12) 0.2358(15) 0.104(7) Uani 1 1 d . . .
C14 C 0.3169(7) 0.0685(9) 0.2164(10) 0.066(4) Uani 1 1 d . . .
C18 C 0.3184(6) 0.1145(10) 0.1509(9) 0.060(3) Uani 1 1 d . . .
H18 H 0.2868 0.1588 0.1085 0.072 Uiso 1 1 calc R . .
C17 C 0.3784(6) 0.0785(10) 0.1640(9) 0.063(4) Uani 1 1 d . . .
H17 H 0.3927 0.0950 0.1315 0.076 Uiso 1 1 calc R . .
C16 C 0.4110(7) 0.0139(9) 0.2350(10) 0.066(4) Uani 1 1 d . . .
H16 H 0.4514 -0.0196 0.2583 0.079 Uiso 1 1 calc R . .
C15 C 0.3739(9) 0.0083(9) 0.2638(13) 0.090(6) Uani 1 1 d . . .
H15 H 0.3853 -0.0312 0.3100 0.108 Uiso 1 1 calc R . .
C23 C 0.3865(5) 0.3080(9) 0.2923(8) 0.056(3) Uani 1 1 d . . .
H23 H 0.3464 0.3439 0.2636 0.067 Uiso 1 1 calc R . .
C22 C 0.4328(6) 0.3061(9) 0.2727(8) 0.054(3) Uani 1 1 d . . .
H22 H 0.4287 0.3416 0.2288 0.065 Uiso 1 1 calc R . .
C21 C 0.4859(6) 0.2409(12) 0.3316(8) 0.067(4) Uani 1 1 d . . .
H21 H 0.5226 0.2252 0.3325 0.080 Uiso 1 1 calc R . .
C20 C 0.4750(7) 0.2050(14) 0.3863(8) 0.078(4) Uani 1 1 d . . .
H20 H 0.5033 0.1612 0.4315 0.094 Uiso 1 1 calc R . .
C19 C 0.4133(7) 0.2445(13) 0.3639(8) 0.070(4) Uani 1 1 d . . .
H19 H 0.3942 0.2310 0.3914 0.084 Uiso 1 1 calc R . .
O1S O 0.2696(15) 0.747(4) 0.009(5) 0.225(15) Uani 1 1 d . . .
C1S C 0.233(2) 0.8269(14) 0.095(2) 0.19(2) Uani 0.92(5) 1 d P . .
H1S1 H 0.2118 0.8942 0.0833 0.284 Uiso 0.92(5) 1 calc PR . .
H1S2 H 0.2744 0.8282 0.1500 0.284 Uiso 0.92(5) 1 calc PR . .
H1S3 H 0.2044 0.7749 0.0943 0.284 Uiso 0.92(5) 1 calc PR . .
C2S C 0.240(2) 0.809(5) 0.0517(19) 0.25(3) Uani 0.92(5) 1 d P . .
B1 B 0.1727(7) 0.3814(10) 0.0669(9) 0.057(3) 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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'
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
N1 Fe1 N1 177.5(5) . 2
N1 Fe1 N4 102.0(3) . 2
N1 Fe1 N4 79.7(3) 2 2
N1 Fe1 N4 79.7(3) . .
N1 Fe1 N4 102.0(3) 2 .
N4 Fe1 N4 92.4(2) 2 .
N1 Fe1 N2 98.7(3) . 2
N1 Fe1 N2 79.5(3) 2 2
N4 Fe1 N2 159.21(19) 2 2
N4 Fe1 N2 91.1 . 2
N1 Fe1 N2 79.5(3) . .
N1 Fe1 N2 98.7(3) 2 .
N4 Fe1 N2 91.1 2 .
N4 Fe1 N2 159.21(19) . .
N2 Fe1 N2 92.8(2) 2 .
C15 Fe2 C14 40.1(6) . .
C15 Fe2 C16 39.0(5) . .
C14 Fe2 C16 67.9(5) . .
C15 Fe2 C21 135.3(7) . .
C14 Fe2 C21 173.3(6) . .
C16 Fe2 C21 111.4(5) . .
C15 Fe2 C19 115.1(7) . .
C14 Fe2 C19 109.4(5) . .
C16 Fe2 C19 143.7(6) . .
C21 Fe2 C19 67.0(5) . .
C15 Fe2 C23 144.2(5) . .
C14 Fe2 C23 113.1(5) . .
C16 Fe2 C23 175.8(6) . .
C21 Fe2 C23 68.1(5) . .
C19 Fe2 C23 40.3(6) . .
C15 Fe2 C18 67.5(7) . .
C14 Fe2 C18 41.6(6) . .
C16 Fe2 C18 68.1(6) . .
C21 Fe2 C18 144.9(6) . .
C19 Fe2 C18 135.2(5) . .
C23 Fe2 C18 109.8(5) . .
C15 Fe2 C22 174.6(5) . .
C14 Fe2 C22 144.6(5) . .
C16 Fe2 C22 136.2(5) . .
C21 Fe2 C22 40.3(5) . .
C19 Fe2 C22 67.5(6) . .
C23 Fe2 C22 40.8(5) . .
C18 Fe2 C22 114.4(5) . .
C15 Fe2 C20 112.1(8) . .
C14 Fe2 C20 135.3(7) . .
C16 Fe2 C20 114.6(6) . .
C21 Fe2 C20 38.4(6) . .
C19 Fe2 C20 40.6(5) . .
C23 Fe2 C20 67.8(6) . .
C18 Fe2 C20 175.6(5) . .
C22 Fe2 C20 66.4(6) . .
C15 Fe2 C17 66.5(6) . .
C14 Fe2 C17 69.0(5) . .
C16 Fe2 C17 40.0(6) . .
C21 Fe2 C17 115.1(5) . .
C19 Fe2 C17 175.6(6) . .
C23 Fe2 C17 136.1(6) . .
C18 Fe2 C17 41.0(5) . .
C22 Fe2 C17 111.3(5) . .
C20 Fe2 C17 143.3(5) . .
C1 N1 C5 117.6(7) . .
C1 N1 Fe1 120.6(6) . .
C5 N1 Fe1 121.5(5) . .
C2 C1 N1 125.0(9) . .
C2 C1 N5 126.2(8) . .
N1 C1 N5 108.8(7) . .
C1 C2 C3 117.1(5) . .
C2 C3 C4 120.0 . .
C2 C3 C12 115.9(7) . .
C4 C3 C12 124.0(7) . .
C3 C4 C5 120.0 . .
N3 C5 N1 108.4(3) . .
N3 C5 C4 131.3 . .
N1 C5 C4 120.3(3) . .
C5 N3 C6 130.8(7) . .
C5 N3 N2 119.2 . .
C6 N3 N2 110.0(7) . .
C8 N2 N3 105.1(6) . .
C8 N2 Fe1 143.6(6) . .
N3 N2 Fe1 111.17(10) . .
N4 N5 C1 118.7(4) . .
N4 N5 C9 108.5 . .
C1 N5 C9 132.8(4) . .
C11 N4 N5 105.3(7) . .
C11 N4 Fe1 142.9(7) . .
N5 N4 Fe1 111.72(10) . .
C10 C9 N5 106.5(6) . .
C11 C10 C9 105.7(10) . .
N4 C11 C10 113.9(13) . .
C7 C6 N3 106.0(11) . .
C6 C7 C8 109.3(12) . .
C13 C12 C3 129.8(17) . .
N2 C8 C7 109.4(12) . .
C12 C13 C14 131(2) . .
C15 C14 C13 123.5(15) . .
C15 C14 C18 105.5(10) . .
C13 C14 C18 131.0(15) . .
C15 C14 Fe2 69.1(8) . .
C13 C14 Fe2 123.6(10) . .
C18 C14 Fe2 69.8(6) . .
C17 C18 C14 106.8(12) . .
C17 C18 Fe2 70.0(7) . .
C14 C18 Fe2 68.6(8) . .
C16 C17 C18 107.2(11) . .
C16 C17 Fe2 69.1(8) . .
C18 C17 Fe2 69.0(7) . .
C15 C16 C17 108.4(12) . .
C15 C16 Fe2 69.4(7) . .
C17 C16 Fe2 70.9(7) . .
C16 C15 C14 112.1(15) . .
C16 C15 Fe2 71.6(7) . .
C14 C15 Fe2 70.7(7) . .
C19 C23 C22 106.5(10) . .
C19 C23 Fe2 69.8(7) . .
C22 C23 Fe2 69.6(6) . .
C21 C22 C23 107.8(11) . .
C21 C22 Fe2 69.8(8) . .
C23 C22 Fe2 69.7(6) . .
C20 C21 C22 109.1(11) . .
C20 C21 Fe2 71.1(9) . .
C22 C21 Fe2 69.9(7) . .
C21 C20 C19 109.2(13) . .
C21 C20 Fe2 70.5(8) . .
C19 C20 Fe2 69.5(8) . .
C23 C19 C20 107.5(12) . .
C23 C19 Fe2 69.9(7) . .
C20 C19 Fe2 69.9(8) . .
O1S O1S C2S 97(10) 7_565 7_565
O1S O1S C2S 53(10) 7_565 .
C2S O1S C2S 150(2) 7_565 .
C1S C2S O1S 153(8) . 7_565
C1S C2S O1S 158(5) . .
O1S C2S O1S 30(2) 7_565 .
F3' B1 F4 106(3) . .
F3' B1 F1 115(5) . .
F4 B1 F1 110.8(11) . .
F3' B1 F2 105(3) . .
F4 B1 F2 110.2(13) . .
F1 B1 F2 109.2(11) . .
F3' B1 F3 17(4) . .
F4 B1 F3 111(2) . .
F1 B1 F3 99(3) . .
F2 B1 F3 116(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 1.884(7) .
Fe1 N1 1.884(7) 2
Fe1 N4 1.986(4) 2
Fe1 N4 1.986(4) .
Fe1 N2 1.985(4) 2
Fe1 N2 1.985(4) .
Fe2 C15 2.010(13) .
Fe2 C14 2.031(12) .
Fe2 C16 2.037(12) .
Fe2 C21 2.043(13) .
Fe2 C19 2.046(13) .
Fe2 C23 2.047(11) .
Fe2 C18 2.047(13) .
Fe2 C22 2.045(11) .
Fe2 C20 2.050(14) .
Fe2 C17 2.061(12) .
F1 B1 1.369(17) .
F3 B1 1.50(7) .
F3' B1 1.33(4) .
F2 B1 1.376(15) .
F4 B1 1.369(17) .
N1 C1 1.363(13) .
N1 C5 1.373(8) .
C1 C2 1.359(10) .
C1 N5 1.386(11) .
C2 C3 1.3900 .
C3 C4 1.3900 .
C3 C12 1.507(12) .
C4 C5 1.3900 .
C5 N3 1.3601 .
N3 C6 1.370(12) .
N3 N2 1.3901 .
N2 C8 1.327(12) .
N5 N4 1.3611 .
N5 C9 1.3991 .
N4 C11 1.319(11) .
C9 C10 1.372(18) .
C10 C11 1.33(2) .
C6 C7 1.32(2) .
C7 C8 1.382(19) .
C12 C13 1.16(2) .
C13 C14 1.438(17) .
C14 C15 1.39(2) .
C14 C18 1.447(19) .
C18 C17 1.439(16) .
C17 C16 1.40(2) .
C16 C15 1.351(17) .
C23 C19 1.410(19) .
C23 C22 1.426(16) .
C22 C21 1.409(18) .
C21 C20 1.35(2) .
C20 C19 1.423(17) .
O1S O1S 0.82(9) 7_565
O1S C2S 1.30(10) 7_565
O1S C2S 1.62(10) .
C1S C2S 1.02(4) .
C2S O1S 1.30(10) 7_565
