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#$Date: 2016-03-21 19:06:25 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178835 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/89/4108984.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_4108984
loop_
_publ_author_name
'Chen-I Yang'
'Wolfgang Wernsdorfer'
'Gene-Hsiang Lee'
'Hui-Lien Tsai'
_publ_section_title
;
 A Pentanuclear Manganese Single-Molecule Magnet with a Large Anisotropy
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              456
_journal_page_last               457
_journal_paper_doi               10.1021/ja066533a
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C45 H75 Cl2 Mn5 N24 O7'
_chemical_formula_weight         1409.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           161
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.4646(2)
_cell_length_b                   13.4646(2)
_cell_length_c                   59.9213(10)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.00
_cell_volume                     9408.0(3)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        DENZO-SMN
_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      150(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       'ω 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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       77
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            25200
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    1.130
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             4368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.015(16)
_refine_ls_extinction_coef       0.00042(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4023
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0374
_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)+(0.0520P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0855
_reflns_number_gt                3479
_reflns_number_total             4023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja066533asi20060913_094724.cif
_cod_data_source_block           ic11641
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4108984
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
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
Mn1 Mn 0.11226(4) -0.04583(4) 0.161148(8) 0.03331(14) Uani 1 1 d . . .
Mn2 Mn 0.0000 0.0000 0.212650(14) 0.02946(19) Uani 1 3 d S . .
Mn3 Mn 0.0000 0.0000 0.109189(15) 0.0400(2) Uani 1 3 d S . .
Cl1 Cl 0.0000 0.0000 0.25132(3) 0.0460(4) Uani 1 3 d S . .
Cl2 Cl 0.0000 0.0000 0.07060(3) 0.0436(4) Uani 1 3 d S . .
O1 O 0.0000 0.0000 0.16172(8) 0.0340(8) Uani 1 3 d S . .
O2 O 0.23008(19) -0.08081(19) 0.16126(4) 0.0396(6) Uani 1 1 d . . .
O3 O 0.20514(19) 0.20234(19) 0.16376(4) 0.0357(5) Uani 1 1 d . . .
N1 N 0.2299(2) 0.1188(2) 0.15675(5) 0.0338(6) Uani 1 1 d . . .
N2 N 0.1365(3) -0.0151(3) 0.19949(5) 0.0349(6) Uani 1 1 d . . .
N3 N 0.2290(3) 0.0136(2) 0.20662(5) 0.0376(7) Uani 1 1 d . . .
N4 N 0.3198(3) 0.0392(3) 0.21297(6) 0.0559(9) Uani 1 1 d . . .
N5 N 0.0954(3) -0.0744(3) 0.12157(6) 0.0490(9) Uani 1 1 d D A .
N6 N 0.0839(4) -0.1518(4) 0.11647(6) 0.0580(11) Uani 1 1 d D . .
N7 N 0.0535(7) -0.2511(6) 0.10932(12) 0.065(2) Uiso 0.60 1 d PD A 1
N7' N 0.1029(12) -0.2250(10) 0.1115(2) 0.077(4) Uiso 0.40 1 d PD A 2
C1 C 0.3240(3) -0.0311(3) 0.14889(5) 0.0380(8) Uani 1 1 d . . .
C2 C 0.3778(3) -0.0942(3) 0.14358(6) 0.0445(9) Uani 1 1 d . . .
H2A H 0.3453 -0.1712 0.1486 0.053 Uiso 1 1 calc R . .
C3 C 0.4785(3) -0.0454(4) 0.13105(7) 0.0500(10) Uani 1 1 d . . .
H3A H 0.5143 -0.0891 0.1277 0.060 Uiso 1 1 calc R . .
C4 C 0.5263(3) 0.0657(4) 0.12354(7) 0.0473(9) Uani 1 1 d . . .
H4A H 0.5939 0.0980 0.1147 0.057 Uiso 1 1 calc R . .
C5 C 0.4761(3) 0.1297(3) 0.12888(6) 0.0421(8) Uani 1 1 d . . .
H5A H 0.5103 0.2067 0.1238 0.051 Uiso 1 1 calc R . .
C6 C 0.3760(3) 0.0843(3) 0.14162(5) 0.0367(7) Uani 1 1 d . . .
C7 C 0.3290(3) 0.1564(3) 0.14761(6) 0.0337(7) Uani 1 1 d . . .
H7A H 0.3738 0.2362 0.1446 0.040 Uiso 1 1 calc R . .
N8 N 0.2818(2) -0.0667(2) 0.04875(5) 0.0392(7) Uani 1 1 d . . .
C8 C 0.3397(3) -0.0957(3) 0.03031(6) 0.0425(8) Uani 1 1 d . . .
H8A H 0.3642 -0.0361 0.0186 0.051 Uiso 1 1 calc R . .
H8B H 0.4098 -0.0919 0.0365 0.051 Uiso 1 1 calc R . .
C9 C 0.2682(3) -0.2109(3) 0.01958(7) 0.0501(9) Uani 1 1 d . . .
H9A H 0.3131 -0.2217 0.0079 0.075 Uiso 1 1 calc R . .
H9B H 0.1997 -0.2152 0.0129 0.075 Uiso 1 1 calc R . .
H9C H 0.2452 -0.2711 0.0309 0.075 Uiso 1 1 calc R . .
C10 C 0.2437(3) -0.1536(3) 0.06759(6) 0.0505(9) Uani 1 1 d . . .
H10A H 0.2084 -0.1299 0.0794 0.061 Uiso 1 1 calc R . .
H10B H 0.1834 -0.2287 0.0618 0.061 Uiso 1 1 calc R . .
C11 C 0.3361(5) -0.1695(4) 0.07802(8) 0.0711(13) Uani 1 1 d . . .
H11A H 0.3047 -0.2211 0.0909 0.107 Uiso 1 1 calc R . .
H11B H 0.3989 -0.0951 0.0830 0.107 Uiso 1 1 calc R . .
H11C H 0.3650 -0.2028 0.0670 0.107 Uiso 1 1 calc R . .
C12 C 0.1759(3) -0.0680(3) 0.04019(7) 0.0454(9) Uani 1 1 d . . .
H12A H 0.1365 -0.0560 0.0530 0.055 Uiso 1 1 calc R . .
H12B H 0.1234 -0.1451 0.0340 0.055 Uiso 1 1 calc R . .
C13 C 0.1965(3) 0.0203(4) 0.02248(7) 0.0524(10) Uani 1 1 d . . .
H13A H 0.1228 0.0111 0.0176 0.079 Uiso 1 1 calc R . .
H13B H 0.2356 0.0096 0.0097 0.079 Uiso 1 1 calc R . .
H13C H 0.2443 0.0974 0.0286 0.079 Uiso 1 1 calc R . .
C14 C 0.3694(3) 0.0529(3) 0.05730(7) 0.0445(9) Uani 1 1 d . . .
H14A H 0.4364 0.0497 0.0633 0.053 Uiso 1 1 calc R . .
H14B H 0.3965 0.1064 0.0445 0.053 Uiso 1 1 calc R . .
C15 C 0.3275(4) 0.1015(3) 0.07497(7) 0.0532(10) Uani 1 1 d . . .
H15A H 0.3906 0.1760 0.0798 0.080 Uiso 1 1 calc R . .
H15B H 0.2991 0.0490 0.0877 0.080 Uiso 1 1 calc R . .
H15C H 0.2653 0.1113 0.0689 0.080 Uiso 1 1 calc R . .
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'
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
O2 Mn1 O1 176.06(9) . .
O2 Mn1 O3 91.75(9) . 3
O1 Mn1 O3 91.88(7) . 3
O2 Mn1 N1 88.76(11) . .
O1 Mn1 N1 87.69(8) . .
O3 Mn1 N1 177.04(11) 3 .
O2 Mn1 N2 88.85(10) . .
O1 Mn1 N2 89.32(16) . .
O3 Mn1 N2 94.65(10) 3 .
N1 Mn1 N2 88.28(11) . .
O2 Mn1 N5 89.27(12) . .
O1 Mn1 N5 92.47(17) . .
O3 Mn1 N5 86.71(11) 3 .
N1 Mn1 N5 90.38(12) . .
N2 Mn1 N5 177.72(12) . .
N2 Mn2 N2 106.78(9) 3 .
N2 Mn2 N2 106.78(9) 3 2
N2 Mn2 N2 106.78(9) . 2
N2 Mn2 Cl1 112.04(8) 3 .
N2 Mn2 Cl1 112.04(8) . .
N2 Mn2 Cl1 112.04(8) 2 .
N5 Mn3 N5 108.42(11) 2 3
N5 Mn3 N5 108.42(12) 2 .
N5 Mn3 N5 108.42(11) 3 .
N5 Mn3 Cl2 110.50(11) 2 .
N5 Mn3 Cl2 110.50(11) 3 .
N5 Mn3 Cl2 110.50(11) . .
Mn1 O1 Mn1 119.967(11) 3 2
Mn1 O1 Mn1 119.967(11) 3 .
Mn1 O1 Mn1 119.967(11) 2 .
C1 O2 Mn1 126.0(2) . .
N1 O3 Mn1 113.99(18) . 2
C7 N1 O3 115.6(3) . .
C7 N1 Mn1 125.6(2) . .
O3 N1 Mn1 118.80(19) . .
N3 N2 Mn2 131.4(2) . .
N3 N2 Mn1 116.5(2) . .
Mn2 N2 Mn1 109.62(13) . .
N4 N3 N2 177.4(4) . .
N6 N5 Mn3 124.0(3) . .
N6 N5 Mn1 114.5(3) . .
Mn3 N5 Mn1 107.58(19) . .
N5 N6 N7' 161.4(9) . .
N5 N6 N7 170.7(6) . .
N7' N6 N7 27.8(7) . .
O2 C1 C2 118.3(3) . .
O2 C1 C6 123.4(3) . .
C2 C1 C6 118.3(3) . .
C3 C2 C1 120.8(4) . .
C4 C3 C2 120.4(4) . .
C5 C4 C3 119.7(3) . .
C4 C5 C6 121.6(4) . .
C5 C6 C1 119.2(3) . .
C5 C6 C7 119.5(3) . .
C1 C6 C7 121.3(3) . .
N1 C7 C6 123.9(3) . .
C12 N8 C8 110.8(3) . .
C12 N8 C10 106.9(3) . .
C8 N8 C10 111.3(3) . .
C12 N8 C14 110.7(3) . .
C8 N8 C14 106.8(3) . .
C10 N8 C14 110.3(3) . .
C9 C8 N8 115.7(3) . .
C11 C10 N8 115.8(3) . .
N8 C12 C13 115.4(3) . .
C15 C14 N8 115.8(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O2 1.867(2) .
Mn1 O1 1.8973(5) .
Mn1 O3 1.924(2) 3
Mn1 N1 1.996(3) .
Mn1 N2 2.328(3) .
Mn1 N5 2.395(4) .
Mn2 N2 2.101(3) 3
Mn2 N2 2.101(3) .
Mn2 N2 2.101(3) 2
Mn2 Cl1 2.3174(17) .
Mn3 N5 2.119(4) 2
Mn3 N5 2.119(4) 3
Mn3 N5 2.119(4) .
Mn3 Cl2 2.3126(18) .
O1 Mn1 1.8973(5) 3
O1 Mn1 1.8973(5) 2
O2 C1 1.323(4) .
O3 N1 1.388(4) .
O3 Mn1 1.924(2) 2
N1 C7 1.290(4) .
N2 N3 1.183(4) .
N3 N4 1.156(4) .
N5 N6 1.021(4) .
N6 N7' 1.174(9) .
N6 N7 1.261(7) .
C1 C2 1.402(5) .
C1 C6 1.416(5) .
C2 C3 1.394(5) .
C3 C4 1.375(6) .
C4 C5 1.373(6) .
C5 C6 1.396(5) .
C6 C7 1.444(5) .
N8 C12 1.506(5) .
N8 C8 1.512(4) .
N8 C10 1.519(5) .
N8 C14 1.532(4) .
C8 C9 1.501(5) .
C10 C11 1.500(7) .
C12 C13 1.512(6) .
C14 C15 1.496(6) .
