#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:44:38 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179304 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/01/4320151.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_4320151
loop_
_publ_author_name
'Jae Yoo'
'Akira Yamaguchi'
'Motohiro Nakano'
'J. Krzystek'
'William E. Streib'
'Louis-Claude Brunel'
'Hidehiko Ishimoto'
'George Christou'
'David N. Hendrickson'
_publ_section_title
;
 Mixed-Valence Tetranuclear Manganese Single-Molecule Magnets
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4604
_journal_page_last               4616
_journal_paper_doi               10.1021/ic0012928
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C42 H48 Cl4 Mn4 N6 O6, 4(H2 O)'
_chemical_formula_sum            'C42 H56 Cl4 Mn4 N6 O10'
_chemical_formula_weight         1166.5
_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
'minor manual editing of SDT2CIF v. 1.2 BETA  output'
_cell_angle_alpha                90
_cell_angle_beta                 90.5495(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0852(4)
_cell_length_b                   20.8781(5)
_cell_length_c                   14.1835(3)
_cell_measurement_reflns_used    5278
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.38
_cell_volume                     5059.1(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT and SHELXTL'
_computing_molecular_graphics    'XTEL, local package'
_computing_publication_material  'XTEL, local package'
_computing_structure_refinement  'XTEL, local package'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_details
' The detector was operated in 4x4 "binning" mode.'
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
' 0.3 degree frames were measured with a counting time of 15.1 seconds each.'
_diffrn_measurement_device
'3-circle diffractometer with fixed chi of 54.74 degrees'
_diffrn_measurement_device_type  Bruker
_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  0.036
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29435
_diffrn_reflns_theta_full        27.469
_diffrn_reflns_theta_max         27.4917
_diffrn_reflns_theta_min         2.09798
_diffrn_standards_decay_%        0.0012
_diffrn_standards_interval_time  321
_diffrn_standards_number         3302
_exptl_absorpt_coefficient_mu    1.2454
_exptl_absorpt_correction_T_max  0.8311
_exptl_absorpt_correction_T_min  0.6286
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            rust
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular plate'
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.32
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       -0.000000018(9)
_refine_ls_extinction_expression
;
Larson, A. C. (1967).  Acta Cryst. 23, p. 664.  Eq. (3)
;
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_ref   0.9799
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         4369
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.1228
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w⁻¹=σ²(F)+(.07F)²
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0434
_reflns_number_gt                4369
_reflns_number_total             5824
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic0012928_2.cif
_cod_data_source_block           MSC99083(Complex3)
_cod_original_cell_volume        5059.1(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4320151
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2+x,1/2+y,z
-x,y,1/2-z
1/2-x,1/2+y,1/2-z
x,-y,1/2+z
1/2+x,1/2-y,1/2+z
-x,-y,-z
1/2-x,1/2-y,-z
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_disorder_group
_atom_site_disorder_assembly
MN1 MN 0.09347(3) 0.30244(2) 0.74237(3) 0.01529(14) Uani 1 0 .
MN2 MN 0.16081(3) 0.16955(2) 0.65721(3) 0.01856(15) Uani 1 0 .
O3 O 0.01623(13) 0.31904(11) 0.83557(14) 0.0197(7) Uani 1 0 .
C4 C 0.0345(2) 0.32029(17) 0.9325(2) 0.0218(10) Uani 1 0 .
C5 C 0.1222(2) 0.32317(15) 0.9498(2) 0.0206(9) Uani 1 0 .
C6 C 0.1530(2) 0.33057(16) 1.0414(2) 0.0239(10) Uani 1 0 .
C7 C 0.2331(2) 0.33567(16) 1.0506(2) 0.0276(11) Uani 1 0 .
C8 C 0.2799(2) 0.33333(16) 0.9715(3) 0.0256(10) Uani 1 0 .
C9 C 0.24598(19) 0.32441(15) 0.8830(2) 0.0221(9) Uani 1 0 .
N10 N 0.16695(16) 0.31984(12) 0.87353(18) 0.0188(8) Uani 1 0 .
C11 C 0.2940(2) 0.3189(2) 0.7963(3) 0.0279(11) Uani 1 0 .
O12 O 0.09499(13) 0.21176(10) 0.76423(15) 0.0191(6) Uani 1 0 .
C13 C 0.0669(2) 0.17739(16) 0.8416(2) 0.0192(9) Uani 1 0 .
C14 C 0.08224(19) 0.10721(16) 0.8300(2) 0.0216(9) Uani 1 0 .
C15 C 0.0597(2) 0.06445(19) 0.8992(3) 0.0317(12) Uani 1 0 .
C16 C 0.0731(3) 0.0002(2) 0.8863(3) 0.0395(13) Uani 1 0 .
C17 C 0.1082(2) -0.01999(18) 0.8052(3) 0.0371(13) Uani 1 0 .
C18 C 0.1304(2) 0.02433(17) 0.7374(3) 0.0292(11) Uani 1 0 .
N19 N 0.11735(16) 0.08783(13) 0.75057(19) 0.0215(8) Uani 1 0 .
C20 C 0.1704(3) 0.0050(2) 0.6481(3) 0.0422(16) Uani 1 0 .
O21 O 0.15508(13) 0.27360(10) 0.64301(15) 0.0203(7) Uani 1 0 .
C22 C 0.1761(2) 0.31624(16) 0.5707(3) 0.0230(10) Uani 1 0 .
C23 C 0.16491(19) 0.38416(16) 0.6013(2) 0.0218(9) Uani 1 0 .
C24 C 0.1918(2) 0.43472(18) 0.5481(3) 0.0332(12) Uani 1 0 .
C25 C 0.1832(3) 0.49579(19) 0.5820(3) 0.0403(14) Uani 1 0 .
C26 C 0.1498(2) 0.50528(18) 0.6693(3) 0.0346(12) Uani 1 0 .
C27 C 0.1236(2) 0.45328(16) 0.7209(2) 0.0241(10) Uani 1 0 .
N28 N 0.13091(16) 0.39274(13) 0.68625(19) 0.0196(8) Uani 1 0 .
C29 C 0.0884(3) 0.46246(19) 0.8161(3) 0.0301(12) Uani 1 0 .
CL30 CL 0.11535(5) 0.14820(4) 0.50135(6) 0.0282(3) Uani 1 0 .
CL31 CL 0.29598(5) 0.14928(4) 0.68486(6) 0.0301(3) Uani 1 0 .
O32 O -0.0069(2) 0.2063(3) 0.3504(3) 0.097(2) Uani 1 0 .
O33 O 0.4786(2) 0.1631(2) 0.6558(2) 0.0833(18) Uani 1 0 .
H1 H 0.011(2) 0.3581(17) 0.961(2) 0.016(9) Uiso 1 0 .
H2 H 0.014(2) 0.2824(17) 0.958(2) 0.018(9) Uiso 1 0 .
H3 H 0.1183(17) 0.3297(14) 1.095(2) 0.000(7) Uiso 1 0 .
H4 H 0.253(2) 0.3447(19) 1.109(3) 0.032(11) Uiso 1 0 .
H5 H 0.338(2) 0.3383(17) 0.968(3) 0.027(10) Uiso 1 0 .
H6 H 0.288(2) 0.283(2) 0.773(3) 0.027(11) Uiso 1 0 .
H7 H 0.279(3) 0.351(2) 0.753(3) 0.045(13) Uiso 1 0 .
H8 H 0.348(2) 0.3203(18) 0.811(3) 0.026(10) Uiso 1 0 .
H9 H 0.091(2) 0.1887(16) 0.887(2) 0.013(9) Uiso 1 0 .
H10 H 0.011(2) 0.1875(18) 0.851(3) 0.029(10) Uiso 1 0 .
H11 H 0.033(2) 0.081(2) 0.943(3) 0.037(12) Uiso 1 0 .
H12 H 0.054(3) -0.028(2) 0.926(3) 0.049(13) Uiso 1 0 .
H13 H 0.121(2) -0.064(2) 0.802(3) 0.043(12) Uiso 1 0 .
H14 H 0.163(3) -0.029(3) 0.631(4) 0.065(17) Uiso 1 0 .
H15 H 0.142(2) 0.0229(18) 0.594(3) 0.023(10) Uiso 1 0 .
H16 H 0.227(3) 0.015(2) 0.649(3) 0.055(15) Uiso 1 0 .
H17 H 0.223(2) 0.3106(16) 0.559(2) 0.016(9) Uiso 1 0 .
H18 H 0.150(2) 0.310(2) 0.526(3) 0.033(12) Uiso 1 0 .
H19 H 0.220(2) 0.426(2) 0.495(3) 0.039(12) Uiso 1 0 .
H20 H 0.202(2) 0.528(2) 0.553(3) 0.031(10) Uiso 1 0 .
H21 H 0.148(2) 0.5480(18) 0.699(3) 0.026(10) Uiso 1 0 .
H22 H 0.075(2) 0.503(2) 0.825(3) 0.029(11) Uiso 1 0 .
H23 H 0.047(2) 0.4386(19) 0.834(3) 0.027(10) Uiso 1 0 .
H24 H 0.119(2) 0.452(2) 0.856(3) 0.035(12) Uiso 1 0 .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
MN Mn 0.295 0.729 'International Tables Vol. IV (1974) Table 2.2B'
CL Cl 0.132 0.159 'International Tables Vol. IV (1974) Table 2.2B'
O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B'
N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B'
C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B'
H H 0 0 'International Tables Vol. IV (1974) Table 2.2B'
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 MN1 O3 74.18(9) 3_556 . . no
O3 MN1 O12 104.32(9) 3_556 . . no
O3 MN1 O12 94.34(9) . . . no
O3 MN1 O21 98.95(9) 3_556 . . no
O3 MN1 O21 168.54(10) . . . no
O3 MN1 N10 148.54(9) 3_556 . . no
O3 MN1 N10 77.49(9) . . . no
O3 MN1 N28 86.02(9) 3_556 . . no
O3 MN1 N28 107.93(10) . . . no
O12 MN1 O21 78.28(9) . . . no
O12 MN1 N10 91.09(9) . . . no
O12 MN1 N28 157.38(10) . . . no
O21 MN1 N10 111.09(10) . . . no
O21 MN1 N28 80.28(10) . . . no
N10 MN1 N28 89.94(10) . . . no
CL30 MN2 CL31 115.35(4) . . . no
CL30 MN2 O12 125.47(7) . . . no
CL30 MN2 O21 94.98(6) . . . no
CL30 MN2 N19 107.06(7) . . . no
CL31 MN2 O12 118.91(7) . . . no
CL31 MN2 O21 103.59(7) . . . no
CL31 MN2 N19 95.27(8) . . . no
O12 MN2 O21 67.92(8) . . . no
O12 MN2 N19 73.41(9) . . . no
O21 MN2 N19 141.32(9) . . . no
MN1 O3 MN1 102.43(9) 3_556 . . no
MN1 O3 C4 132.5(2) 3_556 . . no
MN1 O3 C4 122.11(19) . . . no
MN1 O12 MN2 107.75(10) . . . no
MN1 O12 C13 128.9(2) . . . no
MN2 O12 C13 122.93(19) . . . no
MN1 O21 MN2 106.04(10) . . . no
MN1 O21 C22 119.7(2) . . . no
MN2 O21 C22 133.3(2) . . . no
MN1 N10 C5 110.9(2) . . . no
MN1 N10 C9 129.4(2) . . . no
C5 N10 C9 119.6(3) . . . no
MN2 N19 C14 114.2(2) . . . no
MN2 N19 C18 126.5(2) . . . no
C14 N19 C18 119.0(3) . . . no
MN1 N28 C23 110.2(2) . . . no
MN1 N28 C27 130.8(2) . . . no
C23 N28 C27 119.0(3) . . . no
O3 C4 C5 111.6(3) . . . no
O3 C4 H1 109.4(19) . . . no
O3 C4 H2 107(2) . . . no
C5 C4 H1 108(2) . . . no
C5 C4 H2 110(2) . . . no
H1 C4 H2 111(3) . . . no
N10 C5 C4 116.2(3) . . . no
N10 C5 C6 122.9(3) . . . no
C4 C5 C6 120.9(3) . . . no
C5 C6 C7 117.4(3) . . . no
C5 C6 H3 119.6(17) . . . no
C7 C6 H3 123.0(17) . . . no
C6 C7 C8 120.0(3) . . . no
C6 C7 H4 118(3) . . . no
C8 C7 H4 122(3) . . . no
C7 C8 C9 119.8(3) . . . no
C7 C8 H5 128(2) . . . no
C9 C8 H5 112(2) . . . no
N10 C9 C8 120.3(3) . . . no
N10 C9 C11 117.9(3) . . . no
C8 C9 C11 121.8(3) . . . no
C9 C11 H6 109(3) . . . no
C9 C11 H7 110(3) . . . no
C9 C11 H8 111(2) . . . no
H6 C11 H7 111(4) . . . no
H6 C11 H8 104(3) . . . no
H7 C11 H8 112(3) . . . no
O12 C13 C14 110.7(3) . . . no
O12 C13 H9 108(3) . . . no
O12 C13 H10 110(2) . . . no
C14 C13 H9 107(2) . . . no
C14 C13 H10 113(2) . . . no
H9 C13 H10 108(3) . . . no
N19 C14 C13 117.8(3) . . . no
N19 C14 C15 122.0(3) . . . no
C13 C14 C15 120.2(3) . . . no
C14 C15 C16 119.2(4) . . . no
C14 C15 H11 114(3) . . . no
C16 C15 H11 127(3) . . . no
C15 C16 C17 119.2(4) . . . no
C15 C16 H12 120(3) . . . no
C17 C16 H12 120(3) . . . no
C16 C17 C18 120.1(4) . . . no
C16 C17 H13 117(3) . . . no
C18 C17 H13 123(3) . . . no
N19 C18 C17 120.6(3) . . . no
N19 C18 C20 117.1(3) . . . no
C17 C18 C20 122.3(4) . . . no
C18 C20 H14 116(4) . . . no
C18 C20 H15 109(2) . . . no
C18 C20 H16 113(3) . . . no
H14 C20 H15 92(4) . . . no
H14 C20 H16 110(5) . . . no
H15 C20 H16 114(3) . . . no
O21 C22 C23 110.8(3) . . . no
O21 C22 H17 108(2) . . . no
O21 C22 H18 109(3) . . . no
C23 C22 H17 109(2) . . . no
C23 C22 H18 109(3) . . . no
H17 C22 H18 111(4) . . . no
N28 C23 C22 116.1(3) . . . no
N28 C23 C24 122.2(3) . . . no
C22 C23 C24 121.6(3) . . . no
C23 C24 C25 118.9(4) . . . no
C23 C24 H19 119(3) . . . no
C25 C24 H19 122(3) . . . no
C24 C25 C26 119.6(4) . . . no
C24 C25 H20 121(3) . . . no
C26 C25 H20 119(3) . . . no
C25 C26 C27 119.9(3) . . . no
C25 C26 H21 122(2) . . . no
C27 C26 H21 118(2) . . . no
N28 C27 C26 120.4(3) . . . no
N28 C27 C29 118.9(3) . . . no
C26 C27 C29 120.7(3) . . . no
C27 C29 H22 111(2) . . . no
C27 C29 H23 121(2) . . . no
C27 C29 H24 110(3) . . . no
H22 C29 H23 106(4) . . . no
H22 C29 H24 110(4) . . . no
H23 C29 H24 99(4) . . . no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
MN1 O3 1.909(2) . . no
MN1 O3 2.194(2) . 3_556 no
MN1 O12 1.919(2) . . no
MN1 O21 1.867(2) . . no
MN1 N10 2.264(3) . . no
MN1 N28 2.146(3) . . no
MN2 CL30 2.3782(9) . . no
MN2 CL31 2.3768(10) . . no
MN2 O12 2.092(2) . . no
MN2 O21 2.184(2) . . no
MN2 N19 2.288(3) . . no
O3 C4 1.407(4) . . no
O12 C13 1.400(4) . . no
O21 C22 1.407(4) . . no
N10 C5 1.332(4) . . no
N10 C9 1.359(4) . . no
N19 C14 1.344(4) . . no
N19 C18 1.358(4) . . no
N28 C23 1.355(4) . . no
N28 C27 1.362(4) . . no
C4 C5 1.516(5) . . no
C4 H1 0.98(3) . . no
C4 H2 0.94(4) . . no
C5 C6 1.405(4) . . no
C6 C7 1.379(5) . . no
C6 H3 0.97(3) . . no
C7 C8 1.385(5) . . no
C7 H4 0.92(4) . . no
C8 C9 1.390(5) . . no
C8 H5 1.01(4) . . no
C9 C11 1.490(5) . . no
C11 H6 0.82(4) . . no
C11 H7 0.95(4) . . no
C11 H8 0.94(4) . . no
C13 C14 1.498(5) . . no
C13 H9 0.79(3) . . no
C13 H10 0.99(4) . . no
C14 C15 1.385(5) . . no
C15 C16 1.373(6) . . no
C15 H11 0.84(4) . . no
C16 C17 1.369(6) . . no
C16 H12 0.88(4) . . no
C17 C18 1.390(5) . . no
C17 H13 0.95(4) . . no
C18 C20 1.500(6) . . no
C20 H14 0.76(5) . . no
C20 H15 0.97(4) . . no
C20 H16 0.99(5) . . no
C22 C23 1.495(5) . . no
C22 H17 0.83(4) . . no
C22 H18 0.79(4) . . no
C23 C24 1.379(5) . . no
C24 C25 1.371(5) . . no
C24 H19 0.91(4) . . no
C25 C26 1.384(6) . . no
C25 H20 0.85(4) . . no
C26 C27 1.385(5) . . no
C26 H21 0.98(4) . . no
C27 C29 1.496(5) . . no
C29 H22 0.88(4) . . no
C29 H23 0.90(4) . . no
C29 H24 0.80(4) . . no
