#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:57:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179221 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/45/4314588.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_4314588
loop_
_publ_author_name
'Takuto Matsumoto'
'Takuya Shiga'
'Mao Noguchi'
'Tatsuya Onuki'
'Graham N. Newton'
'Norihisa Hoshino'
'Motohiro Nakano'
'Hiroki Oshio'
_publ_section_title
;
 Contrasting Magnetism of [MnIII4] and [MnII2MnIII2] Squares
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              368
_journal_page_last               370
_journal_paper_doi               10.1021/ic902052f
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C68 H56 Mn4 N12 O16, 2.5(H2O)'
_chemical_formula_sum            'C68 H61 Mn4 N12 O18.5'
_chemical_formula_weight         1562.03
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           48
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2bc'
_symmetry_space_group_name_H-M   'P n n n :2'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.135(2)
_cell_length_b                   20.145(2)
_cell_length_c                   17.2055(18)
_cell_measurement_reflns_used    6842
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.2905
_cell_measurement_theta_min      2.3675
_cell_volume                     6978.9(12)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            35094
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.9618
_exptl_absorpt_correction_T_min  0.7987
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         6328
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0713
_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)+(0.1325P)²+10.6978P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2068
_refine_ls_wR_factor_ref         0.2199
_reflns_number_gt                4660
_reflns_number_total             6328
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic902052f_si_001_1.cif
_cod_data_source_block           tm47mn
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        6978.8(12)
_cod_original_sg_symbol_H-M      'P n n n'
_cod_database_code               4314588
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x-1/2, -y, z-1/2'
'-x, 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
Mn1 Mn 0.19474(4) 0.35982(4) 0.51083(4) 0.0343(2) Uani 1 1 d . . .
Mn2 Mn 0.14011(4) 0.19477(4) 0.48915(4) 0.0344(2) Uani 1 1 d . . .
O1 O 0.09340(18) 0.12584(16) 0.5371(2) 0.0417(8) Uani 1 1 d . . .
O2 O 0.2516(3) 0.5885(2) 0.6218(4) 0.114(2) Uani 1 1 d . . .
O3 O 0.2742(2) 0.4936(2) 0.5654(3) 0.0575(11) Uani 1 1 d . . .
O4 O 0.12578(17) 0.40646(18) 0.4626(2) 0.0415(8) Uani 1 1 d . . .
O5 O -0.0888(2) 0.2517(3) 0.3785(4) 0.111(2) Uani 1 1 d . . .
O6 O 0.0065(2) 0.2742(2) 0.4347(3) 0.0575(11) Uani 1 1 d . . .
O7 O 0.18036(17) 0.26920(16) 0.44081(19) 0.0390(8) Uani 1 1 d DU . .
O8 O 0.26937(17) 0.31976(17) 0.55925(19) 0.0397(8) Uani 1 1 d DU . .
N1 N 0.10032(19) 0.25554(19) 0.5656(2) 0.0335(9) Uani 1 1 d . . .
N2 N 0.1286(2) 0.31491(19) 0.5810(2) 0.0335(9) Uani 1 1 d . . .
N3 N 0.1663(2) 0.4359(2) 0.6294(3) 0.0391(10) Uani 1 1 d . . .
N4 N 0.25531(19) 0.39953(19) 0.4343(2) 0.0340(9) Uani 1 1 d . . .
N5 N 0.18492(19) 0.1285(2) 0.4192(2) 0.0349(9) Uani 1 1 d . . .
N6 N 0.0639(2) 0.1664(2) 0.3704(3) 0.0397(10) Uani 1 1 d . . .
C1 C 0.0357(3) 0.1274(3) 0.5739(3) 0.0385(12) Uani 1 1 d . . .
C2 C -0.0020(3) 0.0690(3) 0.5777(3) 0.0531(15) Uani 1 1 d . . .
H2 H 0.0146 0.0299 0.5536 0.064 Uiso 1 1 calc R . .
C3 C -0.0614(3) 0.0668(3) 0.6148(4) 0.0652(18) Uani 1 1 d . . .
H3 H -0.0855 0.0262 0.6165 0.078 Uiso 1 1 calc R . .
C4 C -0.0872(3) 0.1224(3) 0.6501(4) 0.0615(17) Uani 1 1 d . . .
H4 H -0.1294 0.1206 0.6748 0.074 Uiso 1 1 calc R . .
C5 C -0.0513(3) 0.1812(3) 0.6491(3) 0.0455(13) Uani 1 1 d . . .
H5 H -0.0691 0.2197 0.6733 0.055 Uiso 1 1 calc R . .
C6 C 0.0113(3) 0.1844(2) 0.6127(3) 0.0368(11) Uani 1 1 d . . .
C7 C 0.0503(2) 0.2448(3) 0.6165(3) 0.0361(11) Uani 1 1 d . . .
C8 C 0.0463(2) 0.2993(2) 0.6659(3) 0.0346(11) Uani 1 1 d . . .
H8 H 0.0159 0.3059 0.7074 0.041 Uiso 1 1 calc R . .
C9 C 0.0961(2) 0.3417(2) 0.6418(3) 0.0357(11) Uani 1 1 d . . .
C10 C 0.1180(2) 0.4063(2) 0.6708(3) 0.0376(11) Uani 1 1 d . . .
C11 C 0.0898(3) 0.4349(3) 0.7369(3) 0.0502(14) Uani 1 1 d . . .
H11 H 0.0557 0.4126 0.7648 0.060 Uiso 1 1 calc R . .
C12 C 0.1122(3) 0.4956(3) 0.7610(4) 0.0661(18) Uani 1 1 d . . .
H12 H 0.0942 0.5156 0.8063 0.079 Uiso 1 1 calc R . .
C13 C 0.1608(3) 0.5276(3) 0.7194(4) 0.0659(18) Uani 1 1 d . . .
H13 H 0.1765 0.5700 0.7350 0.079 Uiso 1 1 calc R . .
C14 C 0.1864(3) 0.4963(3) 0.6538(4) 0.0507(14) Uani 1 1 d . . .
C15 C 0.2404(3) 0.5293(3) 0.6111(5) 0.0662(18) Uani 1 1 d . . .
C16 C 0.3276(4) 0.5245(5) 0.5258(6) 0.091(3) Uani 1 1 d . . .
H16A H 0.3108 0.5464 0.4789 0.136 Uiso 1 1 calc R . .
H16B H 0.3605 0.4909 0.5112 0.136 Uiso 1 1 calc R . .
H16C H 0.3483 0.5575 0.5599 0.136 Uiso 1 1 calc R . .
C17 C 0.1274(2) 0.4643(3) 0.4261(3) 0.0389(12) Uani 1 1 d . . .
C18 C 0.0692(3) 0.5015(3) 0.4222(3) 0.0538(15) Uani 1 1 d . . .
H18 H 0.0302 0.4848 0.4464 0.065 Uiso 1 1 calc R . .
C19 C 0.0663(3) 0.5609(3) 0.3850(4) 0.0633(18) Uani 1 1 d . . .
H19 H 0.0255 0.5846 0.3829 0.076 Uiso 1 1 calc R . .
C20 C 0.1226(4) 0.5872(3) 0.3500(4) 0.0635(18) Uani 1 1 d . . .
H20 H 0.1209 0.6295 0.3258 0.076 Uiso 1 1 calc R . .
C21 C 0.1812(3) 0.5511(3) 0.3508(3) 0.0457(13) Uani 1 1 d . . .
H21 H 0.2197 0.5688 0.3265 0.055 Uiso 1 1 calc R . .
C22 C 0.1843(3) 0.4886(3) 0.3871(3) 0.0378(11) Uani 1 1 d . . .
C23 C 0.2446(2) 0.4496(2) 0.3834(3) 0.0358(11) Uani 1 1 d . . .
C24 C 0.2991(2) 0.4537(2) 0.3341(3) 0.0349(11) Uani 1 1 d . . .
H24 H 0.3057 0.4841 0.2926 0.042 Uiso 1 1 calc R . .
C25 C 0.1582(2) 0.0960(2) 0.3584(3) 0.0357(11) Uani 1 1 d . . .
C26 C 0.0935(2) 0.1182(3) 0.3292(3) 0.0388(11) Uani 1 1 d . . .
C27 C 0.0653(3) 0.0897(3) 0.2626(3) 0.0496(14) Uani 1 1 d . . .
H27 H 0.0879 0.0559 0.2346 0.060 Uiso 1 1 calc R . .
C28 C 0.0040(3) 0.1120(3) 0.2388(4) 0.0657(18) Uani 1 1 d . . .
H28 H -0.0164 0.0936 0.1939 0.079 Uiso 1 1 calc R . .
C29 C -0.0275(3) 0.1608(3) 0.2801(4) 0.0640(18) Uani 1 1 d . . .
H29 H -0.0697 0.1768 0.2642 0.077 Uiso 1 1 calc R . .
C30 C 0.0035(3) 0.1864(3) 0.3460(4) 0.0500(14) Uani 1 1 d . . .
C31 C -0.0299(3) 0.2406(3) 0.3895(5) 0.0660(18) Uani 1 1 d . . .
C32 C -0.0250(5) 0.3278(4) 0.4736(5) 0.090(3) Uani 1 1 d . . .
H32A H -0.0583 0.3478 0.4392 0.136 Uiso 1 1 calc R . .
H32B H 0.0083 0.3612 0.4876 0.136 Uiso 1 1 calc R . .
H32C H -0.0467 0.3114 0.5208 0.136 Uiso 1 1 calc R . .
C33 C 0.1673(6) 0.2867(6) 0.3555(5) 0.118(3) Uani 1 1 d DU . .
H33A H 0.1748 0.2474 0.3230 0.177 Uiso 1 1 calc R . .
H33B H 0.1975 0.3223 0.3393 0.177 Uiso 1 1 calc R . .
H33C H 0.1212 0.3016 0.3495 0.177 Uiso 1 1 calc R . .
C34 C 0.2864(6) 0.3326(6) 0.6445(6) 0.123(4) Uani 1 1 d DU . .
H34A H 0.3021 0.3783 0.6506 0.185 Uiso 1 1 calc R . .
H34B H 0.3213 0.3018 0.6611 0.185 Uiso 1 1 calc R . .
H34C H 0.2467 0.3258 0.6765 0.185 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'
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
O4 Mn1 O8 174.75(15) . . ?
O4 Mn1 N4 87.66(16) . . ?
O8 Mn1 N4 88.61(15) . . ?
O4 Mn1 N2 90.03(16) . . ?
O8 Mn1 N2 93.99(15) . . ?
N4 Mn1 N2 174.74(17) . . ?
O4 Mn1 O7 94.36(15) . . ?
O8 Mn1 O7 89.53(14) . . ?
N4 Mn1 O7 93.02(15) . . ?
N2 Mn1 O7 82.44(14) . . ?
O1 Mn2 O7 174.87(15) . . ?
O1 Mn2 N1 87.83(16) . . ?
O7 Mn2 N1 88.58(15) . . ?
O1 Mn2 N5 89.83(16) . . ?
O7 Mn2 N5 94.04(15) . . ?
N1 Mn2 N5 174.77(17) . . ?
O1 Mn2 O8 94.33(15) . 2 ?
O7 Mn2 O8 89.52(14) . 2 ?
N1 Mn2 O8 93.08(15) . 2 ?
N5 Mn2 O8 82.44(14) . 2 ?
C1 O1 Mn2 129.4(3) . . ?
C15 O3 C16 117.2(6) . . ?
C17 O4 Mn1 129.3(3) . . ?
C31 O6 C32 115.9(5) . . ?
C33 O7 Mn2 121.9(5) . . ?
C33 O7 Mn1 110.8(5) . . ?
Mn2 O7 Mn1 118.09(16) . . ?
C34 O8 Mn1 121.8(5) . . ?
C34 O8 Mn2 111.2(5) . 2 ?
Mn1 O8 Mn2 118.08(16) . 2 ?
N2 N1 C7 109.2(4) . . ?
N2 N1 Mn2 120.7(3) . . ?
C7 N1 Mn2 129.5(3) . . ?
C9 N2 N1 107.6(4) . . ?
C9 N2 Mn1 127.4(3) . . ?
N1 N2 Mn1 124.0(3) . . ?
C10 N3 C14 116.9(4) . . ?
C23 N4 N5 109.1(4) . 2 ?
C23 N4 Mn1 129.7(3) . . ?
N5 N4 Mn1 120.7(3) 2 . ?
C25 N5 N4 107.5(4) . 2 ?
C25 N5 Mn2 127.5(3) . . ?
N4 N5 Mn2 124.1(3) 2 . ?
C26 N6 C30 116.9(5) . . ?
O1 C1 C2 118.5(5) . . ?
O1 C1 C6 123.3(4) . . ?
C2 C1 C6 118.1(5) . . ?
C3 C2 C1 121.8(6) . . ?
C2 C3 C4 120.9(6) . . ?
C3 C4 C5 119.5(5) . . ?
C4 C5 C6 120.7(5) . . ?
C5 C6 C1 118.9(5) . . ?
C5 C6 C7 120.2(5) . . ?
C1 C6 C7 120.9(4) . . ?
N1 C7 C8 108.2(4) . . ?
N1 C7 C6 120.6(4) . . ?
C8 C7 C6 131.2(4) . . ?
C9 C8 C7 105.2(4) . . ?
N2 C9 C8 109.8(4) . . ?
N2 C9 C10 118.3(4) . . ?
C8 C9 C10 131.8(4) . . ?
N3 C10 C11 122.9(5) . . ?
N3 C10 C9 115.6(4) . . ?
C11 C10 C9 121.5(5) . . ?
C12 C11 C10 118.7(5) . . ?
C11 C12 C13 119.8(6) . . ?
C12 C13 C14 118.3(5) . . ?
N3 C14 C13 123.3(5) . . ?
N3 C14 C15 118.3(5) . . ?
C13 C14 C15 118.3(5) . . ?
O2 C15 O3 123.2(7) . . ?
O2 C15 C14 120.0(7) . . ?
O3 C15 C14 116.8(5) . . ?
O4 C17 C18 118.3(5) . . ?
O4 C17 C22 123.3(4) . . ?
C18 C17 C22 118.3(5) . . ?
C19 C18 C17 122.1(6) . . ?
C18 C19 C20 120.4(5) . . ?
C21 C20 C19 119.4(5) . . ?
C20 C21 C22 120.7(5) . . ?
C21 C22 C17 118.9(5) . . ?
C21 C22 C23 120.2(5) . . ?
C17 C22 C23 120.8(5) . . ?
N4 C23 C24 108.3(4) . . ?
N4 C23 C22 120.7(4) . . ?
C24 C23 C22 131.1(4) . . ?
C25 C24 C23 105.3(4) 2 . ?
N5 C25 C24 109.8(4) . 2 ?
N5 C25 C26 118.2(4) . . ?
C24 C25 C26 132.0(4) 2 . ?
N6 C26 C27 123.2(5) . . ?
N6 C26 C25 115.7(4) . . ?
C27 C26 C25 121.0(5) . . ?
C28 C27 C26 118.2(5) . . ?
C29 C28 C27 119.8(6) . . ?
C28 C29 C30 118.7(5) . . ?
N6 C30 C29 123.1(5) . . ?
N6 C30 C31 118.1(5) . . ?
C29 C30 C31 118.7(5) . . ?
O5 C31 O6 124.1(7) . . ?
O5 C31 C30 119.8(7) . . ?
O6 C31 C30 116.1(5) . . ?
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
Mn1 O4 1.871(4) . ?
Mn1 O8 1.898(3) . ?
Mn1 N4 1.964(4) . ?
Mn1 N2 2.012(4) . ?
Mn1 O7 2.206(3) . ?
Mn2 O1 1.869(3) . ?
Mn2 O7 1.896(3) . ?
Mn2 N1 1.967(4) . ?
Mn2 N5 2.011(4) . ?
Mn2 O8 2.205(3) 2 ?
O1 C1 1.323(6) . ?
O2 C15 1.229(8) . ?
O3 C15 1.265(8) . ?
O3 C16 1.416(9) . ?
O4 C17 1.325(6) . ?
O5 C31 1.221(8) . ?
O6 C31 1.266(8) . ?
O6 C32 1.420(8) . ?
O7 C33 1.533(9) . ?
O8 C34 1.528(9) . ?
O8 Mn2 2.205(3) 2 ?
N1 N2 1.351(5) . ?
N1 C7 1.351(6) . ?
N2 C9 1.347(6) . ?
N3 C10 1.345(7) . ?
N3 C14 1.349(7) . ?
N4 C23 1.353(6) . ?
N4 N5 1.355(5) 2 ?
N5 C25 1.346(6) . ?
N5 N4 1.355(5) 2 ?
N6 C26 1.343(7) . ?
N6 C30 1.349(7) . ?
C1 C2 1.401(7) . ?
C1 C6 1.415(7) . ?
C2 C3 1.357(9) . ?
C3 C4 1.377(9) . ?
C4 C5 1.387(8) . ?
C5 C6 1.410(7) . ?
C6 C7 1.450(7) . ?
C7 C8 1.392(7) . ?
C8 C9 1.380(7) . ?
C9 C10 1.463(7) . ?
C10 C11 1.396(7) . ?
C11 C12 1.369(8) . ?
C12 C13 1.371(9) . ?
C13 C14 1.393(9) . ?
C14 C15 1.471(9) . ?
C17 C18 1.393(7) . ?
C17 C22 1.414(7) . ?
C18 C19 1.358(9) . ?
C19 C20 1.388(9) . ?
C20 C21 1.386(8) . ?
C21 C22 1.408(7) . ?
C22 C23 1.448(7) . ?
C23 C24 1.390(7) . ?
C24 C25 1.383(7) 2 ?
C25 C24 1.383(7) 2 ?
C25 C26 1.466(7) . ?
C26 C27 1.402(7) . ?
C27 C28 1.375(8) . ?
C28 C29 1.368(9) . ?
C29 C30 1.393(9) . ?
C30 C31 1.484(9) . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 0.750 0.086 405 50 'Corresponds to 5(H2O)'
2 0.750 0.250 -0.103 406 50 'Corresponds to 5(H2O)'
