#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:10:58 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179097 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/59/4305971.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_4305971
loop_
_publ_author_name
'Jonathan P. Hill'
'Humberto Palza'
'Sher Alam'
'Katsuhiko Ariga'
'Amy Lea Schumacher'
'Francis D'Souza'
'Christopher E. Anson'
'Annie K. Powell'
_publ_contact_author
; 
'Jonathan P. Hill'
;
_publ_contact_author_email       jonathan.hill@nims.go.jp
_publ_contact_author_phone       '+81 29 860 4832'
_publ_section_title
;
Decomposition of Dinuclear Manganese Complexes for the Preparation of
Nanostructured Oxide Materials
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8306
_journal_page_last               8314
_journal_paper_doi               10.1021/ic8008915
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C21 H40 Mn3 N13 O2 S5'
_chemical_formula_weight         831.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 114.510(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.2699(10)
_cell_length_b                   11.2384(6)
_cell_length_c                   18.6432(9)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.94
_cell_measurement_theta_min      2.32
_cell_volume                     3483.0(4)
_computing_cell_refinement       'IPDS 2.92 (Stoe & Cie GmbH, 1999)'
_computing_data_collection       'IPDS 2.92 (Stoe & Cie GmbH, 1999)'
_computing_data_reduction        'IPDS 2.92 (Stoe & Cie GmbH, 1999)'
_computing_molecular_graphics    'SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_computing_publication_material  'SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_computing_structure_refinement  'SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_computing_structure_solution    'SHELXTL 5.1 (Bruker AXS Inc., 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'area detector'
_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  0.0839
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11050
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    1.413
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         3195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0536
_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)+(0.0696P)²+8.5915P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1425
_reflns_number_gt                2903
_reflns_number_total             3195
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8008915_si_001.cif
_cod_data_source_block           jon37
_cod_original_cell_volume        3483.0(3)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4305971
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -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 0.18104(3) 0.30623(4) 0.20681(3) 0.02736(18) Uani 1 1 d . . .
O1 O 0.23306(16) 0.2505(3) 0.30603(16) 0.0417(6) Uani 1 1 d . . .
N1 N 0.1300(2) 0.3634(4) 0.0909(2) 0.0502(10) Uani 1 1 d . . .
H1 H 0.158(3) 0.345(5) 0.075(3) 0.060 Uiso 1 1 d . . .
C1 C 0.1235(3) 0.4920(5) 0.0865(3) 0.0637(14) Uani 1 1 d . . .
H1A H 0.0762 0.5176 0.0935 0.076 Uiso 1 1 calc R . .
H1B H 0.1189 0.5196 0.0355 0.076 Uiso 1 1 calc R . .
C2 C 0.1983(3) 0.5427(5) 0.1512(4) 0.080(2) Uani 1 1 d . . .
H2A H 0.2449 0.5244 0.1408 0.096 Uiso 1 1 calc R A .
H2B H 0.1937 0.6285 0.1529 0.096 Uiso 1 1 calc R . .
N2 N 0.2084(2) 0.4913(3) 0.2268(3) 0.0585(11) Uani 1 1 d . . .
H2 H 0.251(4) 0.496(5) 0.258(4) 0.070 Uiso 1 1 d . . .
C3 C 0.1541(3) 0.5453(5) 0.2617(3) 0.078(2) Uani 1 1 d . . .
H3A H 0.1847 0.6000 0.3037 0.094 Uiso 1 1 calc R A .
H3B H 0.1108 0.5893 0.2215 0.094 Uiso 1 1 calc R . .
C4 C 0.1199(3) 0.4478(6) 0.2936(3) 0.0700(16) Uani 1 1 d . A .
H4A H 0.1618 0.4113 0.3394 0.084 Uiso 1 1 calc R . .
H4B H 0.0788 0.4789 0.3087 0.084 Uiso 1 1 calc R . .
N3 N 0.0861(2) 0.3630(3) 0.2312(2) 0.0492(9) Uani 1 1 d . . .
H3 H 0.040(3) 0.406(4) 0.185(3) 0.059 Uiso 1 1 d . . .
C5A C 0.0601(5) 0.2681(8) 0.2638(6) 0.0407(18) Uiso 0.50 1 d P A 1
H5A1 H 0.0159 0.2915 0.2767 0.049 Uiso 0.50 1 calc PR A 1
H5A2 H 0.1036 0.2369 0.3107 0.049 Uiso 0.50 1 calc PR A 1
C6A C 0.0339(5) 0.1806(8) 0.1978(7) 0.046(2) Uiso 0.50 1 d P A 1
H6A1 H -0.0179 0.2053 0.1580 0.055 Uiso 0.50 1 calc PR A 1
H6A2 H 0.0267 0.1037 0.2177 0.055 Uiso 0.50 1 calc PR A 1
C5B C 0.0450(4) 0.2356(7) 0.2363(5) 0.0293(15) Uiso 0.50 1 d P A 2
H5B1 H 0.0812 0.1908 0.2816 0.035 Uiso 0.50 1 calc PR A 2
H5B2 H -0.0045 0.2494 0.2424 0.035 Uiso 0.50 1 calc PR A 2
C6B C 0.0277(5) 0.1665(7) 0.1620(6) 0.0401(18) Uiso 0.50 1 d P A 2
H6B1 H 0.0102 0.0863 0.1662 0.048 Uiso 0.50 1 calc PR A 2
H6B2 H -0.0136 0.2054 0.1169 0.048 Uiso 0.50 1 calc PR A 2
N4 N 0.0980(2) 0.1653(4) 0.1557(3) 0.0705(14) Uani 1 1 d . . .
H4 H 0.121(4) 0.090(6) 0.165(4) 0.085 Uiso 1 1 d . . .
C7A C 0.0633(7) 0.1616(10) 0.0822(8) 0.062(3) Uiso 0.50 1 d P A 1
H7A1 H 0.0131 0.1183 0.0663 0.074 Uiso 0.50 1 calc PR A 1
H7A2 H 0.0969 0.1200 0.0615 0.074 Uiso 0.50 1 calc PR A 1
C8A C 0.0470(6) 0.2838(9) 0.0493(6) 0.048(2) Uiso 0.50 1 d P A 1
H8A1 H 0.0041 0.3196 0.0599 0.057 Uiso 0.50 1 calc PR A 1
H8A2 H 0.0301 0.2813 -0.0073 0.057 Uiso 0.50 1 calc PR A 1
C7B C 0.0772(5) 0.1798(7) 0.0590(5) 0.0399(18) Uiso 0.50 1 d P A 2
H7B1 H 0.1212 0.1484 0.0485 0.048 Uiso 0.50 1 calc PR A 2
H7B2 H 0.0288 0.1359 0.0274 0.048 Uiso 0.50 1 calc PR A 2
C8B C 0.0655(5) 0.3104(8) 0.0385(5) 0.0390(18) Uiso 0.50 1 d P A 2
H8B1 H 0.0612 0.3239 -0.0145 0.047 Uiso 0.50 1 calc PR A 2
H8B2 H 0.0172 0.3401 0.0419 0.047 Uiso 0.50 1 calc PR A 2
Mn2 Mn 0.2500 -0.15560(8) 0.0000 0.0412(2) Uani 1 2 d S . .
N11 N 0.1662(3) -0.1501(4) 0.0572(3) 0.0654(11) Uani 1 1 d . . .
C11 C 0.1393(2) -0.1431(4) 0.1028(3) 0.0468(10) Uani 1 1 d . . .
S11 S 0.10414(9) -0.13307(11) 0.16879(9) 0.0649(4) Uani 1 1 d . . .
N12 N 0.2500 0.0306(5) 0.0000 0.0647(15) Uani 1 2 d S . .
C12 C 0.2500 0.1332(6) 0.0000 0.0487(14) Uani 1 2 d S . .
S12 S 0.2676(2) 0.27430(19) 0.0120(3) 0.0572(12) Uani 0.50 1 d P . .
N13 N 0.3288(2) -0.2712(4) 0.0876(2) 0.0562(10) Uani 1 1 d . . .
C13 C 0.3605(2) -0.3608(4) 0.1058(2) 0.0412(9) Uani 1 1 d . . .
S13 S 0.40634(6) -0.48948(10) 0.13171(7) 0.0500(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'
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'
S S 0.1246 0.1234 '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
O1 Mn1 O1 84.02(13) 7 . ?
O1 Mn1 N3 174.78(13) 7 . ?
O1 Mn1 N3 90.87(13) . . ?
O1 Mn1 N1 90.63(13) 7 . ?
O1 Mn1 N1 174.64(13) . . ?
N3 Mn1 N1 94.47(14) . . ?
O1 Mn1 N4 100.16(16) 7 . ?
O1 Mn1 N4 100.09(16) . . ?
N3 Mn1 N4 79.67(18) . . ?
N1 Mn1 N4 80.49(19) . . ?
O1 Mn1 N2 102.37(15) 7 . ?
O1 Mn1 N2 100.02(16) . . ?
N3 Mn1 N2 79.51(16) . . ?
N1 Mn1 N2 81.42(17) . . ?
N4 Mn1 N2 151.11(14) . . ?
Mn1 O1 Mn1 95.98(13) 7 . ?
C8B N1 C1 112.5(5) . . ?
C1 N1 C8A 118.5(4) . . ?
C8B N1 Mn1 120.6(5) . . ?
C1 N1 Mn1 111.0(3) . . ?
C8A N1 Mn1 104.5(4) . . ?
C8B N1 H1 98(5) . . ?
C1 N1 H1 108(5) . . ?
C8A N1 H1 109(5) . . ?
Mn1 N1 H1 105(5) . . ?
N1 C1 C2 107.8(4) . . ?
N1 C1 H1A 110.1 . . ?
C2 C1 H1A 110.1 . . ?
N1 C1 H1B 110.1 . . ?
C2 C1 H1B 110.1 . . ?
H1A C1 H1B 108.5 . . ?
N2 C2 C1 109.3(4) . . ?
N2 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
N2 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?
C2 N2 C3 114.3(4) . . ?
C2 N2 Mn1 106.9(4) . . ?
C3 N2 Mn1 108.5(3) . . ?
C2 N2 H2 114(5) . . ?
C3 N2 H2 106(5) . . ?
Mn1 N2 H2 107(4) . . ?
C4 C3 N2 109.3(4) . . ?
C4 C3 H3A 109.8 . . ?
N2 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
N2 C3 H3B 109.8 . . ?
H3A C3 H3B 108.3 . . ?
N3 C4 C3 106.0(4) . . ?
N3 C4 H4A 110.5 . . ?
C3 C4 H4A 110.5 . . ?
N3 C4 H4B 110.5 . . ?
C3 C4 H4B 110.5 . . ?
H4A C4 H4B 108.7 . . ?
C5A N3 C4 105.3(6) . . ?
C4 N3 C5B 126.0(5) . . ?
C5A N3 Mn1 109.0(4) . . ?
C4 N3 Mn1 105.4(3) . . ?
C5B N3 Mn1 100.9(3) . . ?
C5A N3 H3 114(3) . . ?
C4 N3 H3 107(3) . . ?
C5B N3 H3 103(3) . . ?
Mn1 N3 H3 115(3) . . ?
N3 C5A C6A 101.2(7) . . ?
N3 C5A H5A1 111.5 . . ?
C6A C5A H5A1 111.5 . . ?
N3 C5A H5A2 111.5 . . ?
C6A C5A H5A2 111.5 . . ?
H5A1 C5A H5A2 109.4 . . ?
C5A C6A N4 114.2(6) . . ?
C5A C6A H6A1 108.7 . . ?
N4 C6A H6A1 108.7 . . ?
C5A C6A H6A2 108.7 . . ?
N4 C6A H6A2 108.7 . . ?
H6A1 C6A H6A2 107.6 . . ?
C6B C5B N3 108.9(6) . . ?
C6B C5B H5B1 109.9 . . ?
N3 C5B H5B1 109.9 . . ?
C6B C5B H5B2 109.9 . . ?
N3 C5B H5B2 109.9 . . ?
H5B1 C5B H5B2 108.3 . . ?
N4 C6B C5B 104.2(6) . . ?
N4 C6B H6B1 110.9 . . ?
C5B C6B H6B1 110.9 . . ?
N4 C6B H6B2 110.9 . . ?
C5B C6B H6B2 110.9 . . ?
H6B1 C6B H6B2 108.9 . . ?
C7A N4 C6A 112.7(7) . . ?
C6B N4 C7B 107.1(6) . . ?
C7A N4 Mn1 117.3(6) . . ?
C6B N4 Mn1 119.0(5) . . ?
C6A N4 Mn1 102.8(4) . . ?
C7B N4 Mn1 102.1(4) . . ?
C7A N4 H4 99(4) . . ?
C6B N4 H4 112(4) . . ?
C6A N4 H4 112(4) . . ?
C7B N4 H4 99(4) . . ?
Mn1 N4 H4 114(4) . . ?
N4 C7A C8A 110.3(9) . . ?
N4 C7A H7A1 109.6 . . ?
C8A C7A H7A1 109.6 . . ?
N4 C7A H7A2 109.6 . . ?
C8A C7A H7A2 109.6 . . ?
H7A1 C7A H7A2 108.1 . . ?
C7A C8A N1 108.7(7) . . ?
C7A C8A H8A1 110.0 . . ?
N1 C8A H8A1 110.0 . . ?
C7A C8A H8A2 110.0 . . ?
N1 C8A H8A2 110.0 . . ?
H8A1 C8A H8A2 108.3 . . ?
C8B C7B N4 108.1(6) . . ?
C8B C7B H7B1 110.1 . . ?
N4 C7B H7B1 110.1 . . ?
C8B C7B H7B2 110.1 . . ?
N4 C7B H7B2 110.1 . . ?
H7B1 C7B H7B2 108.4 . . ?
N1 C8B C7B 105.2(6) . . ?
N1 C8B H8B1 110.7 . . ?
C7B C8B H8B1 110.7 . . ?
N1 C8B H8B2 110.7 . . ?
C7B C8B H8B2 110.7 . . ?
H8B1 C8B H8B2 108.8 . . ?
N12 Mn2 N13 127.90(12) . 2 ?
N12 Mn2 N13 127.90(12) . . ?
N13 Mn2 N13 104.2(2) 2 . ?
N12 Mn2 N11 88.41(12) . 2 ?
N13 Mn2 N11 91.74(16) 2 2 ?
N13 Mn2 N11 90.22(17) . 2 ?
N12 Mn2 N11 88.41(12) . . ?
N13 Mn2 N11 90.22(17) 2 . ?
N13 Mn2 N11 91.74(16) . . ?
N11 Mn2 N11 176.8(2) 2 . ?
C11 N11 Mn2 163.5(4) . . ?
N11 C11 S11 178.4(4) . . ?
C12 N12 Mn2 180.0 . . ?
N12 C12 S12 169.08(13) . . ?
C13 N13 Mn2 150.5(4) . . ?
N13 C13 S13 179.7(4) . . ?
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 O1 1.799(3) 7 ?
Mn1 O1 1.805(3) . ?
Mn1 N3 2.068(3) . ?
Mn1 N1 2.070(4) . ?
Mn1 N4 2.126(4) . ?
Mn1 N2 2.136(4) . ?
Mn1 Mn1 2.6783(9) 7 ?
O1 Mn1 1.799(3) 7 ?
N1 C8B 1.319(10) . ?
N1 C1 1.450(6) . ?
N1 C8A 1.652(11) . ?
N1 H1 0.72(6) . ?
C1 C2 1.509(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.462(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
N2 C3 1.520(7) . ?
N2 H2 0.75(6) . ?
C3 C4 1.501(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N3 1.430(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
N3 C5A 1.405(9) . ?
N3 C5B 1.638(9) . ?
N3 H3 1.04(5) . ?
C5A C6A 1.491(13) . ?
C5A H5A1 0.9700 . ?
C5A H5A2 0.9700 . ?
C6A N4 1.667(12) . ?
C6A H6A1 0.9700 . ?
C6A H6A2 0.9700 . ?
C5B C6B 1.503(12) . ?
C5B H5B1 0.9700 . ?
C5B H5B2 0.9700 . ?
C6B N4 1.338(10) . ?
C6B H6B1 0.9700 . ?
C6B H6B2 0.9700 . ?
N4 C7A 1.249(13) . ?
N4 C7B 1.688(11) . ?
N4 H4 0.93(7) . ?
C7A C8A 1.482(15) . ?
C7A H7A1 0.9700 . ?
C7A H7A2 0.9700 . ?
C8A H8A1 0.9700 . ?
C8A H8A2 0.9700 . ?
C7B C8B 1.510(12) . ?
C7B H7B1 0.9700 . ?
C7B H7B2 0.9700 . ?
C8B H1 1.59(6) . ?
C8B H8B1 0.9700 . ?
C8B H8B2 0.9700 . ?
Mn2 N12 2.092(6) . ?
Mn2 N13 2.116(4) 2 ?
Mn2 N13 2.116(4) . ?
Mn2 N11 2.200(5) 2 ?
Mn2 N11 2.200(5) . ?
N11 C11 1.148(6) . ?
C11 S11 1.611(5) . ?
N12 C12 1.154(8) . ?
C12 S12 1.615(7) . ?
N13 C13 1.141(6) . ?
C13 S13 1.640(5) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 S12 0.72(6) 2.82(6) 3.542(8) 180(6) .
N1 H1 S12 0.72(6) 2.63(6) 3.341(8) 168(6) 2
N2 H2 S11 0.75(6) 2.88(6) 3.540(4) 148(6) 7
N3 H3 S13 1.04(5) 2.41(5) 3.345(3) 149(4) 6
N4 H4 S11 0.93(7) 2.54(7) 3.360(4) 148(5) .
