# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_formula_moiety         'C24 H20 Mn N4 O4, 2(H2 O)'
_chemical_formula_sum            'C24 H24 Mn N4 O6'
_chemical_formula_weight         519.41

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'
Mn Mn 0.3368 0.7283 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.852(3)
_cell_length_b                   9.292(2)
_cell_length_c                   15.791(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.57(3)
_cell_angle_gamma                90.00
_cell_volume                     2248.8(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10667
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      27.16

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1076
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_process_details   'Stoe, X-area ver. 1.54'

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  IPDS2
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25571
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0876
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.33
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3950
_reflns_number_gt                2401
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3950
_refine_ls_number_parameters     317
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0270
_refine_ls_wR_factor_ref         0.0397
_refine_ls_wR_factor_gt          0.0383
_refine_ls_goodness_of_fit_ref   0.813
_refine_ls_restrained_S_all      0.813
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.25422(3) 0.37667(4) 0.13357(2) 0.01682(9) Uani 1 1 d . . .
O1 O 0.31066(10) 0.46098(16) 0.28019(10) 0.0228(4) Uani 1 1 d . . .
O2 O 0.31699(11) 0.22326(17) 0.28539(10) 0.0248(4) Uani 1 1 d . . .
O3 O 0.19197(9) 0.35060(17) -0.02872(10) 0.0222(4) Uani 1 1 d . . .
O4 O 0.22418(10) 0.15483(16) 0.05724(10) 0.0211(4) Uani 1 1 d . . .
C1 C 0.33094(15) 0.3441(3) 0.32592(15) 0.0184(6) Uani 1 1 d . . .
C2 C 0.37159(14) 0.3516(3) 0.42853(14) 0.0237(6) Uani 1 1 d . . .
H2A H 0.3386 0.4184 0.4496 0.036 Uiso 1 1 calc R . .
H2B H 0.4319 0.3856 0.4498 0.036 Uiso 1 1 calc R . .
H2C H 0.3714 0.2557 0.4543 0.036 Uiso 1 1 calc R . .
C3 C 0.19326(14) 0.2133(3) -0.02115(15) 0.0182(6) Uani 1 1 d . . .
C4 C 0.15515(14) 0.1240(3) -0.10827(14) 0.0229(6) Uani 1 1 d . . .
H4A H 0.1614 0.0216 -0.0917 0.034 Uiso 1 1 calc R . .
H4B H 0.1860 0.1447 -0.1475 0.034 Uiso 1 1 calc R . .
H4C H 0.0932 0.1473 -0.1424 0.034 Uiso 1 1 calc R . .
N1 N 0.12641(12) 0.3165(2) 0.14854(11) 0.0182(5) Uani 1 1 d . . .
N2 N 0.16324(12) 0.57505(19) 0.10484(12) 0.0171(5) Uani 1 1 d . . .
N3 N 0.31889(12) 0.57803(19) 0.10269(12) 0.0175(5) Uani 1 1 d . . .
N4 N 0.39392(12) 0.3224(2) 0.14637(12) 0.0189(5) Uani 1 1 d . . .
C11 C 0.11236(15) 0.1843(2) 0.17289(14) 0.0202(6) Uani 1 1 d . . .
H11 H 0.1554 0.1124 0.1828 0.024 Uiso 1 1 calc R . .
C12 C 0.03753(14) 0.1479(3) 0.18427(14) 0.0220(6) Uani 1 1 d . . .
H12 H 0.0308 0.0539 0.2040 0.026 Uiso 1 1 calc R . .
C13 C -0.02689(16) 0.2499(3) 0.16662(15) 0.0239(6) Uani 1 1 d . . .
H13 H -0.0792 0.2267 0.1727 0.029 Uiso 1 1 calc R . .
C14 C -0.01398(14) 0.3865(3) 0.13992(14) 0.0208(6) Uani 1 1 d . . .
H14 H -0.0577 0.4582 0.1264 0.025 Uiso 1 1 calc R . .
C15 C 0.06408(15) 0.4175(2) 0.13307(14) 0.0181(6) Uani 1 1 d . . .
C16 C 0.08553(15) 0.5628(2) 0.10810(15) 0.0170(5) Uani 1 1 d . . .
C17 C 0.02872(15) 0.6796(2) 0.09020(14) 0.0207(6) Uani 1 1 d . . .
H17 H -0.0272 0.6683 0.0905 0.025 Uiso 1 1 calc R . .
C18 C 0.05561(15) 0.8120(3) 0.07209(15) 0.0228(6) Uani 1 1 d . . .
H18 H 0.0184 0.8933 0.0605 0.027 Uiso 1 1 calc R . .
C19 C 0.13690(15) 0.8261(2) 0.07087(14) 0.0219(6) Uani 1 1 d . . .
H19 H 0.1564 0.9166 0.0591 0.026 Uiso 1 1 calc R . .
C20 C 0.18949(15) 0.7039(2) 0.08744(14) 0.0171(5) Uani 1 1 d . . .
C21 C 0.27758(15) 0.7059(2) 0.08693(15) 0.0184(5) Uani 1 1 d . . .
C22 C 0.31597(15) 0.8305(2) 0.07233(15) 0.0256(6) Uani 1 1 d . . .
H22 H 0.2865 0.9203 0.0620 0.031 Uiso 1 1 calc R . .
C23 C 0.39831(16) 0.8201(3) 0.07317(16) 0.0299(6) Uani 1 1 d . . .
H23 H 0.4257 0.9033 0.0626 0.036 Uiso 1 1 calc R . .
C24 C 0.44050(16) 0.6897(3) 0.08930(15) 0.0255(6) Uani 1 1 d . . .
H24 H 0.4971 0.6818 0.0904 0.031 Uiso 1 1 calc R . .
C25 C 0.39873(15) 0.5695(2) 0.10402(15) 0.0184(6) Uani 1 1 d . . .
C26 C 0.44076(15) 0.4252(3) 0.12652(15) 0.0201(6) Uani 1 1 d . . .
C27 C 0.52301(15) 0.3979(3) 0.12954(16) 0.0279(6) Uani 1 1 d . . .
H27 H 0.5545 0.4717 0.1153 0.033 Uiso 1 1 calc R . .
C28 C 0.55824(16) 0.2615(3) 0.15351(16) 0.0289(7) Uani 1 1 d . . .
H28 H 0.6143 0.2405 0.1558 0.035 Uiso 1 1 calc R . .
C29 C 0.51142(14) 0.1572(3) 0.17383(14) 0.0232(6) Uani 1 1 d . . .
H29 H 0.5346 0.0631 0.1909 0.028 Uiso 1 1 calc R . .
C30 C 0.42934(14) 0.1913(2) 0.16906(14) 0.0223(6) Uani 1 1 d . . .
H30 H 0.3969 0.1182 0.1825 0.027 Uiso 1 1 calc R . .
O1W O 0.21367(11) 0.69503(18) 0.32334(12) 0.0400(5) Uani 1 1 d . . .
H1W1 H 0.2469 0.6422 0.3119 0.060 Uiso 1 1 d R . .
H1W2 H 0.2333 0.7771 0.3321 0.060 Uiso 1 1 d R . .
O2W O 0.27312(11) -0.01394(17) 0.37070(11) 0.0371(5) Uani 1 1 d . . .
H2W1 H 0.2858 0.0489 0.3420 0.056 Uiso 1 1 d R . .
H2W2 H 0.2464 0.0278 0.3966 0.056 Uiso 1 1 d R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 2.2467(16) . ?
Mn1 N3 2.3170(19) . ?
Mn1 N2 2.3187(19) . ?
Mn1 N1 2.330(2) . ?
Mn1 N4 2.333(2) . ?
Mn1 O4 2.3347(15) . ?
Mn1 O3 2.3433(16) . ?
O1 C1 1.270(3) . ?
O2 C1 1.265(3) . ?
O3 C3 1.281(3) . ?
O4 C3 1.250(3) . ?
C1 C2 1.475(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.503(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
N1 C11 1.338(3) . ?
N1 C15 1.352(3) . ?
N2 C16 1.337(3) . ?
N2 C20 1.344(3) . ?
N3 C25 1.339(3) . ?
N3 C21 1.347(3) . ?
N4 C30 1.338(3) . ?
N4 C26 1.356(3) . ?
C11 C12 1.388(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.379(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.383(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.394(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.493(3) . ?
C16 C17 1.396(3) . ?
C17 C18 1.381(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.384(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.397(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.488(3) . ?
C21 C22 1.391(3) . ?
C22 C23 1.386(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.374(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.391(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.489(3) . ?
C26 C27 1.390(3) . ?
C27 C28 1.383(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.370(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.390(3) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
O1W H1W1 0.8196 . ?
O1W H1W2 0.8195 . ?
O2W H2W1 0.8199 . ?
O2W H2W2 0.8201 . ?

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 N3 84.30(6) . . ?
O1 Mn1 N2 83.48(6) . . ?
N3 Mn1 N2 69.35(7) . . ?
O1 Mn1 N1 89.55(6) . . ?
N3 Mn1 N1 138.62(7) . . ?
N2 Mn1 N1 69.30(7) . . ?
O1 Mn1 N4 90.38(7) . . ?
N3 Mn1 N4 69.31(7) . . ?
N2 Mn1 N4 138.61(7) . . ?
N1 Mn1 N4 151.82(6) . . ?
O1 Mn1 O4 138.41(6) . . ?
N3 Mn1 O4 128.63(6) . . ?
N2 Mn1 O4 128.11(6) . . ?
N1 Mn1 O4 80.19(6) . . ?
N4 Mn1 O4 81.27(6) . . ?
O1 Mn1 O3 165.52(6) . . ?
N3 Mn1 O3 83.64(6) . . ?
N2 Mn1 O3 84.79(6) . . ?
N1 Mn1 O3 94.23(6) . . ?
N4 Mn1 O3 92.82(6) . . ?
O4 Mn1 O3 56.06(5) . . ?
C1 O1 Mn1 100.74(14) . . ?
C3 O3 Mn1 91.06(13) . . ?
C3 O4 Mn1 92.25(14) . . ?
O2 C1 O1 121.5(2) . . ?
O2 C1 C2 120.1(2) . . ?
O1 C1 C2 118.5(2) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O4 C3 O3 120.6(2) . . ?
O4 C3 C4 120.7(2) . . ?
O3 C3 C4 118.7(2) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C11 N1 C15 118.2(2) . . ?
C11 N1 Mn1 122.06(16) . . ?
C15 N1 Mn1 119.77(15) . . ?
C16 N2 C20 119.7(2) . . ?
C16 N2 Mn1 120.24(15) . . ?
C20 N2 Mn1 120.08(15) . . ?
C25 N3 C21 119.6(2) . . ?
C25 N3 Mn1 120.41(15) . . ?
C21 N3 Mn1 119.94(16) . . ?
C30 N4 C26 117.7(2) . . ?
C30 N4 Mn1 122.80(16) . . ?
C26 N4 Mn1 119.42(15) . . ?
N1 C11 C12 122.7(2) . . ?
N1 C11 H11 118.6 . . ?
C12 C11 H11 118.6 . . ?
C13 C12 C11 119.2(2) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C12 C13 C14 118.8(2) . . ?
C12 C13 H13 120.6 . . ?
C14 C13 H13 120.6 . . ?
C13 C14 C15 119.1(2) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
N1 C15 C14 122.0(2) . . ?
N1 C15 C16 114.8(2) . . ?
C14 C15 C16 123.2(2) . . ?
N2 C16 C17 121.8(2) . . ?
N2 C16 C15 115.8(2) . . ?
C17 C16 C15 122.4(2) . . ?
C18 C17 C16 118.5(2) . . ?
C18 C17 H17 120.7 . . ?
C16 C17 H17 120.7 . . ?
C17 C18 C19 119.9(2) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C18 C19 C20 118.4(2) . . ?
C18 C19 H19 120.8 . . ?
C20 C19 H19 120.8 . . ?
N2 C20 C19 121.7(2) . . ?
N2 C20 C21 115.2(2) . . ?
C19 C20 C21 123.1(2) . . ?
N3 C21 C22 121.6(2) . . ?
N3 C21 C20 115.3(2) . . ?
C22 C21 C20 123.0(2) . . ?
C23 C22 C21 118.3(2) . . ?
C23 C22 H22 120.9 . . ?
C21 C22 H22 120.9 . . ?
C24 C23 C22 120.1(2) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 118.7(2) . . ?
C23 C24 H24 120.6 . . ?
C25 C24 H24 120.6 . . ?
N3 C25 C24 121.7(2) . . ?
N3 C25 C26 115.6(2) . . ?
C24 C25 C26 122.7(2) . . ?
N4 C26 C27 122.1(2) . . ?
N4 C26 C25 115.1(2) . . ?
C27 C26 C25 122.8(2) . . ?
C28 C27 C26 119.0(2) . . ?
C28 C27 H27 120.5 . . ?
C26 C27 H27 120.5 . . ?
C29 C28 C27 119.3(2) . . ?
C29 C28 H28 120.4 . . ?
C27 C28 H28 120.4 . . ?
C28 C29 C30 118.9(2) . . ?
C28 C29 H29 120.6 . . ?
C30 C29 H29 120.6 . . ?
N4 C30 C29 123.0(2) . . ?
N4 C30 H30 118.5 . . ?
C29 C30 H30 118.5 . . ?
H1W1 O1W H1W2 109.2 . . ?
H2W1 O2W H2W2 105.2 . . ?

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
O1W H1W1 O1 0.82 2.17 2.965(2) 165 .
O1W H1W2 O2W 0.82 2.06 2.873(2) 170 1_565
O2W H2W1 O2 0.82 2.02 2.837(2) 172 .
O2W H2W2 O3 0.82 2.10 2.916(2) 173 4_566

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.30
_refine_diff_density_rms         0.06
_database_code_depnum_ccdc_archive 'CCDC 946224'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_formula_moiety         'C36 H24 Mn N4 O5, 4(H2 O)'
_chemical_formula_sum            'C36 H32 Mn N4 O9'
_chemical_formula_weight         719.60

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.731(3)
_cell_length_b                   12.876(3)
_cell_length_c                   22.096(4)
_cell_angle_alpha                93.88(3)
_cell_angle_beta                 100.00(3)
_cell_angle_gamma                107.99(3)
_cell_volume                     3364.1(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    22055
_cell_measurement_theta_min      1.56
_cell_measurement_theta_max      27.23

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1492
_exptl_absorpt_coefficient_mu    0.455
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.922
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_process_details   'Stoe, X-area ver. 1.54'

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  IPDS2
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            48816
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_sigmaI/netI    0.0894
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         25.00
_reflns_number_total             11853
_reflns_number_gt                6667
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11853
_refine_ls_number_parameters     901
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0403
_refine_ls_wR_factor_gt          0.0376
_refine_ls_goodness_of_fit_ref   0.842
_refine_ls_restrained_S_all      0.842
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
O1W O 0.11180(15) 0.98041(14) 0.05434(9) 0.0185(4) Uani 1 1 d . . .
H1W1 H 0.1198 1.0310 0.0331 0.028 Uiso 1 1 d R . .
H1W2 H 0.0698 0.9230 0.0333 0.028 Uiso 1 1 d R . .
O2W O 0.87775(15) 0.51352(13) 0.44909(9) 0.0187(4) Uani 1 1 d . . .
H2W1 H 0.8740 0.4632 0.4703 0.028 Uiso 1 1 d R . .
H2W2 H 0.9208 0.5701 0.4705 0.028 Uiso 1 1 d R . .
O3W O 0.94199(17) 0.49490(15) 0.61681(10) 0.0290(5) Uani 1 1 d . . .
H3W1 H 0.9166 0.4475 0.5865 0.043 Uiso 1 1 d R . .
H3W2 H 1.0030 0.5289 0.6089 0.043 Uiso 1 1 d R . .
O4W O 0.92541(17) 0.98621(15) 0.11494(10) 0.0278(5) Uani 1 1 d . . .
H4W1 H 0.8952 0.9409 0.0840 0.042 Uiso 1 1 d R . .
H4W2 H 0.9901 1.0155 0.1103 0.042 Uiso 1 1 d R . .
O5W O 0.86405(16) 0.64759(15) 0.67458(9) 0.0287(5) Uani 1 1 d . . .
H5W1 H 0.8854 0.6002 0.6587 0.043 Uiso 1 1 d R . .
H5W2 H 0.8886 0.6997 0.6559 0.043 Uiso 1 1 d R . .
O6W O 0.12179(16) 0.85786(15) 0.80736(9) 0.0321(5) Uani 1 1 d . . .
H6W1 H 0.1160 0.9093 0.8291 0.048 Uiso 1 1 d R . .
H6W2 H 0.0618 0.8089 0.8058 0.048 Uiso 1 1 d R . .
O7W O 0.05367(15) 0.18320(14) 0.39706(8) 0.0254(4) Uani 1 1 d . . .
H7W1 H 0.0367 0.2176 0.4243 0.038 Uiso 1 1 d R . .
H7W2 H -0.0055 0.1554 0.3715 0.038 Uiso 1 1 d R . .
O8W O 0.94648(15) 0.34213(14) 0.08296(8) 0.0286(5) Uani 1 1 d . . .
H8W1 H 0.9664 0.3014 0.0606 0.043 Uiso 1 1 d R . .
H8W2 H 0.9762 0.3371 0.1181 0.043 Uiso 1 1 d R . .
O9W O 0.08222(13) 0.31434(13) 0.19724(7) 0.0273(4) Uani 1 1 d . . .
H9W1 H 0.1276 0.2955 0.1806 0.041 Uiso 1 1 d R . .
H9W2 H 0.1034 0.3268 0.2350 0.041 Uiso 1 1 d R . .
O10W O 0.84777(13) 0.11567(12) 0.31435(7) 0.0279(4) Uani 1 1 d . . .
H0W1 H 0.8266 0.1625 0.3309 0.042 Uiso 1 1 d R . .
H0W2 H 0.8590 0.1282 0.2798 0.042 Uiso 1 1 d R . .
Mn1 Mn 0.25729(3) 0.97739(3) 0.11781(2) 0.01476(10) Uani 1 1 d . . .
O11 O 0.34082(15) 1.14515(13) 0.11724(9) 0.0185(4) Uani 1 1 d . . .
O21 O 0.20728(16) 1.21828(14) 0.13236(9) 0.0205(4) Uani 1 1 d . . .
O31 O 0.17257(15) 1.16289(13) -0.00451(9) 0.0176(4) Uani 1 1 d . . .
O41 O 0.02123(15) 1.21016(14) 0.00659(9) 0.0209(5) Uani 1 1 d . . .
C11 C 0.2961(2) 1.2217(2) 0.11528(13) 0.0158(6) Uani 1 1 d . . .
C21 C 0.3639(2) 1.3263(2) 0.09462(13) 0.0161(6) Uani 1 1 d . . .
C31 C 0.4776(2) 1.3671(2) 0.11991(13) 0.0181(6) Uani 1 1 d . . .
H31 H 0.5117 1.3224 0.1433 0.022 Uiso 1 1 calc R . .
C41 C 0.5448(2) 1.4723(2) 0.11220(14) 0.0250(7) Uani 1 1 d . . .
H41 H 0.6235 1.4973 0.1292 0.030 Uiso 1 1 calc R . .
C51 C 0.4969(2) 1.5382(2) 0.08043(14) 0.0244(7) Uani 1 1 d . . .
H51 H 0.5418 1.6109 0.0771 0.029 Uiso 1 1 calc R . .
C61 C 0.3810(2) 1.5002(2) 0.05222(13) 0.0190(6) Uani 1 1 d . . .
C71 C 0.3320(2) 1.5694(2) 0.01931(13) 0.0222(7) Uani 1 1 d . . .
H71 H 0.3778 1.6421 0.0167 0.027 Uiso 1 1 calc R . .
C81 C 0.2210(2) 1.5353(2) -0.00878(13) 0.0230(7) Uani 1 1 d . . .
H81 H 0.1885 1.5845 -0.0287 0.028 Uiso 1 1 calc R . .
C91 C 0.1553(2) 1.4255(2) -0.00765(13) 0.0185(6) Uani 1 1 d . . .
H91 H 0.0783 1.4009 -0.0283 0.022 Uiso 1 1 calc R . .
C101 C 0.1979(2) 1.35268(19) 0.02213(13) 0.0151(6) Uani 1 1 d . . .
C111 C 0.1254(2) 1.2326(2) 0.00870(13) 0.0152(6) Uani 1 1 d . . .
C121 C 0.3124(2) 1.3906(2) 0.05632(13) 0.0155(6) Uani 1 1 d . . .
N111 N 0.42512(19) 0.95683(17) 0.16379(11) 0.0175(5) Uani 1 1 d . . .
N211 N 0.32684(18) 0.91133(16) 0.04102(11) 0.0155(5) Uani 1 1 d . . .
C12 C 0.4732(2) 0.9793(2) 0.22362(14) 0.0241(7) Uani 1 1 d . . .
H12 H 0.4355 1.0061 0.2514 0.029 Uiso 1 1 calc R . .
C22 C 0.5767(2) 0.9657(2) 0.24797(15) 0.0295(7) Uani 1 1 d . . .
H22 H 0.6079 0.9824 0.2912 0.035 Uiso 1 1 calc R . .
C32 C 0.6317(2) 0.9278(2) 0.20807(15) 0.0287(7) Uani 1 1 d . . .
H32 H 0.7021 0.9183 0.2235 0.034 Uiso 1 1 calc R . .
C42 C 0.5841(2) 0.9028(2) 0.14443(14) 0.0200(6) Uani 1 1 d . . .
C52 C 0.6379(2) 0.8654(2) 0.09965(15) 0.0230(7) Uani 1 1 d . . .
H52 H 0.7071 0.8522 0.1135 0.028 Uiso 1 1 calc R . .
C62 C 0.5931(2) 0.8484(2) 0.03853(14) 0.0206(7) Uani 1 1 d . . .
H62 H 0.6320 0.8262 0.0098 0.025 Uiso 1 1 calc R . .
C72 C 0.4865(2) 0.8638(2) 0.01664(14) 0.0169(6) Uani 1 1 d . . .
C82 C 0.4357(2) 0.8471(2) -0.04701(14) 0.0202(7) Uani 1 1 d . . .
H82 H 0.4729 0.8268 -0.0773 0.024 Uiso 1 1 calc R . .
C92 C 0.3336(2) 0.8603(2) -0.06469(14) 0.0200(7) Uani 1 1 d . . .
H92 H 0.2983 0.8483 -0.1073 0.024 Uiso 1 1 calc R . .
C102 C 0.2804(2) 0.8920(2) -0.01920(13) 0.0172(6) Uani 1 1 d . . .
H102 H 0.2084 0.8999 -0.0321 0.021 Uiso 1 1 calc R . .
C112 C 0.4292(2) 0.89720(19) 0.05916(13) 0.0154(6) Uani 1 1 d . . .
C122 C 0.4797(2) 0.91889(19) 0.12421(13) 0.0161(6) Uani 1 1 d . . .
N121 N 0.17933(18) 0.79864(17) 0.13817(11) 0.0165(5) Uani 1 1 d . . .
N221 N 0.20742(18) 0.98768(17) 0.21091(11) 0.0173(5) Uani 1 1 d . . .
C13 C 0.1631(2) 0.7062(2) 0.10178(14) 0.0213(7) Uani 1 1 d . . .
H13 H 0.1724 0.7108 0.0602 0.026 Uiso 1 1 calc R . .
C23 C 0.1327(2) 0.6018(2) 0.12215(14) 0.0229(7) Uani 1 1 d . . .
H23 H 0.1219 0.5374 0.0949 0.027 Uiso 1 1 calc R . .
C33 C 0.1190(2) 0.5946(2) 0.18184(14) 0.0223(7) Uani 1 1 d . . .
H33 H 0.0992 0.5248 0.1964 0.027 Uiso 1 1 calc R . .
C43 C 0.1342(2) 0.6903(2) 0.22176(13) 0.0173(6) Uani 1 1 d . . .
C53 C 0.1167(2) 0.6889(2) 0.28405(14) 0.0228(7) Uani 1 1 d . . .
H53 H 0.0969 0.6208 0.3005 0.027 Uiso 1 1 calc R . .
C63 C 0.1276(2) 0.7815(2) 0.31952(13) 0.0231(7) Uani 1 1 d . . .
H63 H 0.1156 0.7779 0.3607 0.028 Uiso 1 1 calc R . .
C73 C 0.1572(2) 0.8864(2) 0.29654(13) 0.0196(6) Uani 1 1 d . . .
C83 C 0.1646(2) 0.9847(2) 0.33028(14) 0.0257(7) Uani 1 1 d . . .
H83 H 0.1502 0.9847 0.3710 0.031 Uiso 1 1 calc R . .
C93 C 0.1927(2) 1.0817(2) 0.30496(14) 0.0252(7) Uani 1 1 d . . .
H93 H 0.1975 1.1490 0.3276 0.030 Uiso 1 1 calc R . .
C103 C 0.2141(2) 1.0789(2) 0.24477(14) 0.0223(7) Uani 1 1 d . . .
H103 H 0.2345 1.1461 0.2275 0.027 Uiso 1 1 calc R . .
C113 C 0.1779(2) 0.8913(2) 0.23558(13) 0.0155(6) Uani 1 1 d . . .
C123 C 0.1647(2) 0.7911(2) 0.19751(14) 0.0168(6) Uani 1 1 d . . .
Mn2 Mn 0.73421(3) 0.50864(3) 0.38157(2) 0.01514(10) Uani 1 1 d . . .
O12 O 0.65368(15) 0.34231(14) 0.39024(9) 0.0187(4) Uani 1 1 d . . .
O22 O 0.79451(15) 0.28124(13) 0.37537(9) 0.0177(4) Uani 1 1 d . . .
O32 O 0.83933(15) 0.33235(13) 0.51123(9) 0.0173(4) Uani 1 1 d . . .
O42 O 0.99121(15) 0.29548(14) 0.49010(9) 0.0196(4) Uani 1 1 d . . .
C14 C 0.7040(2) 0.2710(2) 0.39253(13) 0.0156(6) Uani 1 1 d . . .
C24 C 0.6442(2) 0.16251(19) 0.41338(13) 0.0145(6) Uani 1 1 d . . .
C34 C 0.5302(2) 0.1158(2) 0.39021(13) 0.0228(7) Uani 1 1 d . . .
H34 H 0.4907 0.1579 0.3682 0.027 Uiso 1 1 calc R . .
C44 C 0.4706(2) 0.0079(2) 0.39806(14) 0.0268(7) Uani 1 1 d . . .
H44 H 0.3915 -0.0219 0.3825 0.032 Uiso 1 1 calc R . .
C54 C 0.5272(2) -0.0537(2) 0.42818(14) 0.0252(7) Uani 1 1 d . . .
H54 H 0.4875 -0.1280 0.4318 0.030 Uiso 1 1 calc R . .
C64 C 0.6439(2) -0.0095(2) 0.45425(13) 0.0188(6) Uani 1 1 d . . .
C74 C 0.7021(2) -0.0750(2) 0.48506(13) 0.0211(7) Uani 1 1 d . . .
H74 H 0.6615 -0.1492 0.4884 0.025 Uiso 1 1 calc R . .
C84 C 0.8140(2) -0.0346(2) 0.50979(13) 0.0214(6) Uani 1 1 d . . .
H84 H 0.8521 -0.0809 0.5284 0.026 Uiso 1 1 calc R . .
C94 C 0.8733(2) 0.0770(2) 0.50771(12) 0.0177(6) Uani 1 1 d . . .
H94 H 0.9515 0.1056 0.5258 0.021 Uiso 1 1 calc R . .
C104 C 0.8206(2) 0.1455(2) 0.48014(12) 0.0150(6) Uani 1 1 d . . .
C114 C 0.8885(2) 0.2677(2) 0.49332(13) 0.0166(6) Uani 1 1 d . . .
C124 C 0.7053(2) 0.1026(2) 0.44937(13) 0.0160(6) Uani 1 1 d . . .
N112 N 0.78685(18) 0.48910(16) 0.28905(11) 0.0156(5) Uani 1 1 d . . .
N212 N 0.81176(18) 0.68303(17) 0.35565(11) 0.0176(5) Uani 1 1 d . . .
C15 C 0.7829(2) 0.3953(2) 0.25803(13) 0.0204(6) Uani 1 1 d . . .
H15 H 0.7592 0.3295 0.2762 0.025 Uiso 1 1 calc R . .
C25 C 0.8119(2) 0.3885(2) 0.20000(13) 0.0202(6) Uani 1 1 d . . .
H25 H 0.8099 0.3200 0.1802 0.024 Uiso 1 1 calc R . .
C35 C 0.8431(2) 0.4818(2) 0.17227(13) 0.0196(6) Uani 1 1 d . . .
H35 H 0.8630 0.4787 0.1329 0.024 Uiso 1 1 calc R . .
C45 C 0.8455(2) 0.5825(2) 0.20252(13) 0.0171(6) Uani 1 1 d . . .
C55 C 0.8751(2) 0.6840(2) 0.17618(13) 0.0201(6) Uani 1 1 d . . .
H55 H 0.8892 0.6836 0.1354 0.024 Uiso 1 1 calc R . .
C65 C 0.8831(2) 0.7799(2) 0.20835(13) 0.0198(6) Uani 1 1 d . . .
H65 H 0.9025 0.8458 0.1898 0.024 Uiso 1 1 calc R . .
C75 C 0.8628(2) 0.7837(2) 0.27005(13) 0.0174(6) Uani 1 1 d . . .
C85 C 0.8756(2) 0.8818(2) 0.30649(13) 0.0190(6) Uani 1 1 d . . .
H85 H 0.8977 0.9499 0.2902 0.023 Uiso 1 1 calc R . .
C95 C 0.8564(2) 0.8797(2) 0.36538(14) 0.0218(7) Uani 1 1 d . . .
H95 H 0.8641 0.9459 0.3902 0.026 Uiso 1 1 calc R . .
C105 C 0.8251(2) 0.7785(2) 0.38862(13) 0.0193(6) Uani 1 1 d . . .
H105 H 0.8127 0.7778 0.4298 0.023 Uiso 1 1 calc R . .
C115 C 0.8309(2) 0.6855(2) 0.29679(13) 0.0149(6) Uani 1 1 d . . .
C125 C 0.8197(2) 0.5827(2) 0.26193(13) 0.0145(6) Uani 1 1 d . . .
N122 N 0.66407(18) 0.58353(16) 0.45582(11) 0.0151(5) Uani 1 1 d . . .
N222 N 0.56479(18) 0.52368(17) 0.33361(11) 0.0173(5) Uani 1 1 d . . .
C16 C 0.7091(2) 0.6089(2) 0.51580(14) 0.0170(6) Uani 1 1 d . . .
H16 H 0.7811 0.6016 0.5298 0.020 Uiso 1 1 calc R . .
C26 C 0.6575(2) 0.6459(2) 0.55983(14) 0.0187(7) Uani 1 1 d . . .
H26 H 0.6936 0.6628 0.6024 0.022 Uiso 1 1 calc R . .
C36 C 0.5540(2) 0.65737(19) 0.54040(13) 0.0175(6) Uani 1 1 d . . .
H36 H 0.5167 0.6811 0.5695 0.021 Uiso 1 1 calc R . .
C46 C 0.5031(2) 0.6336(2) 0.47679(14) 0.0166(6) Uani 1 1 d . . .
C56 C 0.3954(2) 0.6450(2) 0.45298(14) 0.0193(7) Uani 1 1 d . . .
H56 H 0.3566 0.6706 0.4805 0.023 Uiso 1 1 calc R . .
C66 C 0.3487(2) 0.6196(2) 0.39180(14) 0.0225(7) Uani 1 1 d . . .
H66 H 0.2782 0.6293 0.3768 0.027 Uiso 1 1 calc R . .
C76 C 0.4041(2) 0.5782(2) 0.34908(14) 0.0194(6) Uani 1 1 d . . .
C86 C 0.3563(2) 0.5458(2) 0.28596(14) 0.0268(7) Uani 1 1 d . . .
H86 H 0.2851 0.5526 0.2694 0.032 Uiso 1 1 calc R . .
C96 C 0.4123(3) 0.5042(2) 0.24812(15) 0.0305(7) Uani 1 1 d . . .
H96 H 0.3810 0.4825 0.2051 0.037 Uiso 1 1 calc R . .
C106 C 0.5165(2) 0.4942(2) 0.27406(14) 0.0247(7) Uani 1 1 d . . .
H106 H 0.5548 0.4649 0.2477 0.030 Uiso 1 1 calc R . .
C116 C 0.5095(2) 0.56528(19) 0.37116(13) 0.0157(6) Uani 1 1 d . . .
C126 C 0.5611(2) 0.59582(19) 0.43629(13) 0.0146(6) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
O1W Mn1 2.133(2) . ?
O1W H1W1 0.8192 . ?
O1W H1W2 0.8195 . ?
O2W Mn2 2.130(2) . ?
O2W H2W1 0.8194 . ?
O2W H2W2 0.8197 . ?
O3W H3W1 0.8197 . ?
O3W H3W2 0.8202 . ?
O4W H4W1 0.8193 . ?
O4W H4W2 0.8207 . ?
O5W H5W1 0.8216 . ?
O5W H5W2 0.8190 . ?
O6W H6W1 0.8206 . ?
O6W H6W2 0.8197 . ?
O7W H7W1 0.8210 . ?
O7W H7W2 0.8201 . ?
O8W H8W1 0.8216 . ?
O8W H8W2 0.8195 . ?
O9W H9W1 0.8222 . ?
O9W H9W2 0.8192 . ?
O10W H0W1 0.8217 . ?
O10W H0W2 0.8190 . ?
Mn1 O11 2.0944(18) . ?
Mn1 N221 2.263(2) . ?
Mn1 N211 2.276(3) . ?
Mn1 N111 2.302(2) . ?
Mn1 N121 2.317(2) . ?
O11 C11 1.282(3) . ?
O21 C11 1.242(3) . ?
O31 C111 1.269(3) . ?
O41 C111 1.259(3) . ?
C11 C21 1.506(4) . ?
C21 C31 1.376(4) . ?
C21 C121 1.438(4) . ?
C31 C41 1.401(4) . ?
C31 H31 0.9500 . ?
C41 C51 1.355(4) . ?
C41 H41 0.9500 . ?
C51 C61 1.413(4) . ?
C51 H51 0.9500 . ?
C61 C71 1.409(3) . ?
C61 C121 1.431(3) . ?
C71 C81 1.360(4) . ?
C71 H71 0.9500 . ?
C81 C91 1.407(4) . ?
C81 H81 0.9500 . ?
C91 C101 1.371(4) . ?
C91 H91 0.9500 . ?
C101 C121 1.436(4) . ?
C101 C111 1.514(3) . ?
N111 C12 1.328(4) . ?
N111 C122 1.360(4) . ?
N211 C102 1.332(4) . ?
N211 C112 1.367(3) . ?
C12 C22 1.401(4) . ?
C12 H12 0.9500 . ?
C22 C32 1.369(5) . ?
C22 H22 0.9500 . ?
C32 C42 1.404(4) . ?
C32 H32 0.9500 . ?
C42 C122 1.410(4) . ?
C42 C52 1.433(4) . ?
C52 C62 1.346(4) . ?
C52 H52 0.9500 . ?
C62 C72 1.437(4) . ?
C62 H62 0.9500 . ?
C72 C112 1.406(4) . ?
C72 C82 1.414(4) . ?
C82 C92 1.356(4) . ?
C82 H82 0.9500 . ?
C92 C102 1.410(4) . ?
C92 H92 0.9500 . ?
C102 H102 0.9500 . ?
C112 C122 1.439(4) . ?
N121 C13 1.329(4) . ?
N121 C123 1.362(4) . ?
N221 C103 1.320(4) . ?
N221 C113 1.361(3) . ?
C13 C23 1.408(4) . ?
C13 H13 0.9500 . ?
C23 C33 1.365(4) . ?
C23 H23 0.9500 . ?
C33 C43 1.406(4) . ?
C33 H33 0.9500 . ?
C43 C123 1.407(3) . ?
C43 C53 1.433(4) . ?
C53 C63 1.337(4) . ?
C53 H53 0.9500 . ?
C63 C73 1.439(4) . ?
C63 H63 0.9500 . ?
C73 C83 1.393(4) . ?
C73 C113 1.418(4) . ?
C83 C93 1.375(4) . ?
C83 H83 0.9500 . ?
C93 C103 1.404(4) . ?
C93 H93 0.9500 . ?
C103 H103 0.9500 . ?
C113 C123 1.438(4) . ?
Mn2 O12 2.1077(18) . ?
Mn2 N112 2.281(2) . ?
Mn2 N122 2.290(3) . ?
Mn2 N222 2.303(2) . ?
Mn2 N212 2.312(2) . ?
O12 C14 1.270(3) . ?
O22 C14 1.247(3) . ?
O32 C114 1.267(3) . ?
O42 C114 1.261(3) . ?
C14 C24 1.516(3) . ?
C24 C34 1.374(4) . ?
C24 C124 1.440(4) . ?
C34 C44 1.401(4) . ?
C34 H34 0.9500 . ?
C44 C54 1.360(4) . ?
C44 H44 0.9500 . ?
C54 C64 1.414(4) . ?
C54 H54 0.9500 . ?
C64 C74 1.418(4) . ?
C64 C124 1.435(3) . ?
C74 C84 1.354(4) . ?
C74 H74 0.9500 . ?
C84 C94 1.410(3) . ?
C84 H84 0.9500 . ?
C94 C104 1.377(4) . ?
C94 H94 0.9500 . ?
C104 C124 1.423(4) . ?
C104 C114 1.522(3) . ?
N112 C15 1.330(4) . ?
N112 C125 1.364(3) . ?
N212 C105 1.333(4) . ?
N212 C115 1.365(4) . ?
C15 C25 1.399(4) . ?
C15 H15 0.9500 . ?
C25 C35 1.366(3) . ?
C25 H25 0.9500 . ?
C35 C45 1.408(4) . ?
C35 H35 0.9500 . ?
C45 C125 1.408(4) . ?
C45 C55 1.436(3) . ?
C55 C65 1.348(4) . ?
C55 H55 0.9500 . ?
C65 C75 1.431(4) . ?
C65 H65 0.9500 . ?
C75 C85 1.400(4) . ?
C75 C115 1.408(3) . ?
C85 C95 1.366(4) . ?
C85 H85 0.9500 . ?
C95 C105 1.401(3) . ?
C95 H95 0.9500 . ?
C105 H105 0.9500 . ?
C115 C125 1.439(4) . ?
N122 C16 1.324(4) . ?
N122 C126 1.368(3) . ?
N222 C106 1.327(4) . ?
N222 C116 1.359(4) . ?
C16 C26 1.399(4) . ?
C16 H16 0.9500 . ?
C26 C36 1.369(4) . ?
C26 H26 0.9500 . ?
C36 C46 1.411(4) . ?
C36 H36 0.9500 . ?
C46 C126 1.405(4) . ?
C46 C56 1.435(4) . ?
C56 C66 1.352(4) . ?
C56 H56 0.9500 . ?
C66 C76 1.438(4) . ?
C66 H66 0.9500 . ?
C76 C86 1.400(4) . ?
C76 C116 1.410(4) . ?
C86 C96 1.370(4) . ?
C86 H86 0.9500 . ?
C96 C106 1.398(4) . ?
C96 H96 0.9500 . ?
C106 H106 0.9500 . ?
C116 C126 1.446(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
Mn1 O1W H1W1 117.3 . . ?
Mn1 O1W H1W2 119.1 . . ?
H1W1 O1W H1W2 109.6 . . ?
Mn2 O2W H2W1 119.7 . . ?
Mn2 O2W H2W2 123.6 . . ?
H2W1 O2W H2W2 107.2 . . ?
H3W1 O3W H3W2 100.2 . . ?
H4W1 O4W H4W2 104.6 . . ?
H5W1 O5W H5W2 102.0 . . ?
H6W1 O6W H6W2 102.9 . . ?
H7W1 O7W H7W2 104.5 . . ?
H8W1 O8W H8W2 104.1 . . ?
H9W1 O9W H9W2 111.5 . . ?
H0W1 O10W H0W2 112.0 . . ?
O11 Mn1 O1W 92.37(7) . . ?
O11 Mn1 N221 98.70(8) . . ?
O1W Mn1 N221 103.26(8) . . ?
O11 Mn1 N211 97.51(8) . . ?
O1W Mn1 N211 92.32(8) . . ?
N221 Mn1 N211 156.94(7) . . ?
O11 Mn1 N111 89.79(8) . . ?
O1W Mn1 N111 165.36(9) . . ?
N221 Mn1 N111 90.71(9) . . ?
N211 Mn1 N111 73.03(9) . . ?
O11 Mn1 N121 169.25(8) . . ?
O1W Mn1 N121 95.85(8) . . ?
N221 Mn1 N121 72.69(8) . . ?
N211 Mn1 N121 89.09(8) . . ?
N111 Mn1 N121 84.00(8) . . ?
C11 O11 Mn1 126.47(17) . . ?
O21 C11 O11 125.5(2) . . ?
O21 C11 C21 119.1(2) . . ?
O11 C11 C21 115.3(2) . . ?
C31 C21 C121 119.6(2) . . ?
C31 C21 C11 117.5(2) . . ?
C121 C21 C11 122.5(2) . . ?
C21 C31 C41 122.1(2) . . ?
C21 C31 H31 119.0 . . ?
C41 C31 H31 119.0 . . ?
C51 C41 C31 119.7(3) . . ?
C51 C41 H41 120.2 . . ?
C31 C41 H41 120.2 . . ?
C41 C51 C61 120.9(2) . . ?
C41 C51 H51 119.5 . . ?
C61 C51 H51 119.5 . . ?
C71 C61 C51 120.5(2) . . ?
C71 C61 C121 119.3(3) . . ?
C51 C61 C121 120.3(2) . . ?
C81 C71 C61 122.0(2) . . ?
C81 C71 H71 119.0 . . ?
C61 C71 H71 119.0 . . ?
C71 C81 C91 118.5(2) . . ?
C71 C81 H81 120.7 . . ?
C91 C81 H81 120.7 . . ?
C101 C91 C81 122.6(2) . . ?
C101 C91 H91 118.7 . . ?
C81 C91 H91 118.7 . . ?
C91 C101 C121 119.2(2) . . ?
C91 C101 C111 116.6(2) . . ?
C121 C101 C111 123.6(2) . . ?
O41 C111 O31 124.6(2) . . ?
O41 C111 C101 117.6(2) . . ?
O31 C111 C101 117.5(2) . . ?
C61 C121 C101 118.0(2) . . ?
C61 C121 C21 117.1(2) . . ?
C101 C121 C21 124.8(2) . . ?
C12 N111 C122 118.0(3) . . ?
C12 N111 Mn1 127.0(2) . . ?
C122 N111 Mn1 115.03(18) . . ?
C102 N211 C112 118.2(3) . . ?
C102 N211 Mn1 126.06(19) . . ?
C112 N211 Mn1 115.63(18) . . ?
N111 C12 C22 123.5(3) . . ?
N111 C12 H12 118.2 . . ?
C22 C12 H12 118.2 . . ?
C32 C22 C12 118.4(3) . . ?
C32 C22 H22 120.8 . . ?
C12 C22 H22 120.8 . . ?
C22 C32 C42 120.1(3) . . ?
C22 C32 H32 119.9 . . ?
C42 C32 H32 119.9 . . ?
C32 C42 C122 117.4(3) . . ?
C32 C42 C52 123.3(3) . . ?
C122 C42 C52 119.2(3) . . ?
C62 C52 C42 121.8(3) . . ?
C62 C52 H52 119.1 . . ?
C42 C52 H52 119.1 . . ?
C52 C62 C72 120.2(3) . . ?
C52 C62 H62 119.9 . . ?
C72 C62 H62 119.9 . . ?
C112 C72 C82 117.6(3) . . ?
C112 C72 C62 119.9(3) . . ?
C82 C72 C62 122.5(3) . . ?
C92 C82 C72 119.7(3) . . ?
C92 C82 H82 120.1 . . ?
C72 C82 H82 120.1 . . ?
C82 C92 C102 119.3(3) . . ?
C82 C92 H92 120.3 . . ?
C102 C92 H92 120.3 . . ?
N211 C102 C92 122.7(3) . . ?
N211 C102 H102 118.6 . . ?
C92 C102 H102 118.6 . . ?
N211 C112 C72 122.4(3) . . ?
N211 C112 C122 118.1(3) . . ?
C72 C112 C122 119.5(3) . . ?
N111 C122 C42 122.5(3) . . ?
N111 C122 C112 118.1(2) . . ?
C42 C122 C112 119.4(3) . . ?
C13 N121 C123 118.2(2) . . ?
C13 N121 Mn1 127.15(19) . . ?
C123 N121 Mn1 113.99(17) . . ?
C103 N221 C113 118.3(2) . . ?
C103 N221 Mn1 125.84(18) . . ?
C113 N221 Mn1 115.57(19) . . ?
N121 C13 C23 122.9(3) . . ?
N121 C13 H13 118.6 . . ?
C23 C13 H13 118.6 . . ?
C33 C23 C13 118.8(3) . . ?
C33 C23 H23 120.6 . . ?
C13 C23 H23 120.6 . . ?
C23 C33 C43 120.2(2) . . ?
C23 C33 H33 119.9 . . ?
C43 C33 H33 119.9 . . ?
C33 C43 C123 117.1(3) . . ?
C33 C43 C53 123.4(2) . . ?
C123 C43 C53 119.4(3) . . ?
C63 C53 C43 121.3(2) . . ?
C63 C53 H53 119.3 . . ?
C43 C53 H53 119.3 . . ?
C53 C63 C73 121.3(3) . . ?
C53 C63 H63 119.4 . . ?
C73 C63 H63 119.4 . . ?
C83 C73 C113 117.2(2) . . ?
C83 C73 C63 123.8(3) . . ?
C113 C73 C63 119.0(3) . . ?
C93 C83 C73 120.4(3) . . ?
C93 C83 H83 119.8 . . ?
C73 C83 H83 119.8 . . ?
C83 C93 C103 118.3(3) . . ?
C83 C93 H93 120.9 . . ?
C103 C93 H93 120.9 . . ?
N221 C103 C93 123.4(2) . . ?
N221 C103 H103 118.3 . . ?
C93 C103 H103 118.3 . . ?
N221 C113 C73 122.3(3) . . ?
N221 C113 C123 118.3(2) . . ?
C73 C113 C123 119.4(2) . . ?
N121 C123 C43 122.8(3) . . ?
N121 C123 C113 117.6(2) . . ?
C43 C123 C113 119.6(3) . . ?
O12 Mn2 O2W 90.94(8) . . ?
O12 Mn2 N112 100.26(8) . . ?
O2W Mn2 N112 104.33(8) . . ?
O12 Mn2 N122 96.82(8) . . ?
O2W Mn2 N122 90.52(8) . . ?
N112 Mn2 N122 157.06(7) . . ?
O12 Mn2 N222 90.53(8) . . ?
O2W Mn2 N222 163.22(9) . . ?
N112 Mn2 N222 91.85(9) . . ?
N122 Mn2 N222 72.71(9) . . ?
O12 Mn2 N212 171.06(8) . . ?
O2W Mn2 N212 95.75(8) . . ?
N112 Mn2 N212 72.37(8) . . ?
N122 Mn2 N212 89.05(8) . . ?
N222 Mn2 N212 84.78(8) . . ?
C14 O12 Mn2 123.01(17) . . ?
O22 C14 O12 125.0(2) . . ?
O22 C14 C24 118.1(2) . . ?
O12 C14 C24 116.8(2) . . ?
C34 C24 C124 120.3(2) . . ?
C34 C24 C14 117.5(2) . . ?
C124 C24 C14 121.8(2) . . ?
C24 C34 C44 122.0(3) . . ?
C24 C34 H34 119.0 . . ?
C44 C34 H34 119.0 . . ?
C54 C44 C34 119.3(3) . . ?
C54 C44 H44 120.4 . . ?
C34 C44 H44 120.4 . . ?
C44 C54 C64 121.4(2) . . ?
C44 C54 H54 119.3 . . ?
C64 C54 H54 119.3 . . ?
C54 C64 C74 120.8(2) . . ?
C54 C64 C124 120.1(2) . . ?
C74 C64 C124 119.1(2) . . ?
C84 C74 C64 121.6(2) . . ?
C84 C74 H74 119.2 . . ?
C64 C74 H74 119.2 . . ?
C74 C84 C94 119.3(2) . . ?
C74 C84 H84 120.4 . . ?
C94 C84 H84 120.4 . . ?
C104 C94 C84 121.6(3) . . ?
C104 C94 H94 119.2 . . ?
C84 C94 H94 119.2 . . ?
C94 C104 C124 120.0(2) . . ?
C94 C104 C114 115.2(2) . . ?
C124 C104 C114 124.2(2) . . ?
O42 C114 O32 125.1(2) . . ?
O42 C114 C104 117.6(3) . . ?
O32 C114 C104 117.1(2) . . ?
C104 C124 C64 117.9(2) . . ?
C104 C124 C24 125.3(2) . . ?
C64 C124 C24 116.7(2) . . ?
C15 N112 C125 117.6(2) . . ?
C15 N112 Mn2 126.42(17) . . ?
C125 N112 Mn2 115.91(18) . . ?
C105 N212 C115 117.8(2) . . ?
C105 N212 Mn2 126.8(2) . . ?
C115 N212 Mn2 114.80(17) . . ?
N112 C15 C25 123.5(2) . . ?
N112 C15 H15 118.3 . . ?
C25 C15 H15 118.3 . . ?
C35 C25 C15 119.1(3) . . ?
C35 C25 H25 120.4 . . ?
C15 C25 H25 120.4 . . ?
C25 C35 C45 119.5(3) . . ?
C25 C35 H35 120.2 . . ?
C45 C35 H35 120.2 . . ?
C125 C45 C35 117.6(2) . . ?
C125 C45 C55 119.2(3) . . ?
C35 C45 C55 123.2(3) . . ?
C65 C55 C45 121.2(3) . . ?
C65 C55 H55 119.4 . . ?
C45 C55 H55 119.4 . . ?
C55 C65 C75 120.9(2) . . ?
C55 C65 H65 119.5 . . ?
C75 C65 H65 119.5 . . ?
C85 C75 C115 117.4(3) . . ?
C85 C75 C65 123.1(2) . . ?
C115 C75 C65 119.5(3) . . ?
C95 C85 C75 120.1(2) . . ?
C95 C85 H85 120.0 . . ?
C75 C85 H85 120.0 . . ?
C85 C95 C105 119.0(3) . . ?
C85 C95 H95 120.5 . . ?
C105 C95 H95 120.5 . . ?
N212 C105 C95 123.1(3) . . ?
N212 C105 H105 118.5 . . ?
C95 C105 H105 118.5 . . ?
N212 C115 C75 122.7(3) . . ?
N212 C115 C125 117.7(2) . . ?
C75 C115 C125 119.6(3) . . ?
N112 C125 C45 122.6(2) . . ?
N112 C125 C115 117.9(2) . . ?
C45 C125 C115 119.4(2) . . ?
C16 N122 C126 117.2(3) . . ?
C16 N122 Mn2 126.77(19) . . ?
C126 N122 Mn2 115.86(18) . . ?
C106 N222 C116 118.0(3) . . ?
C106 N222 Mn2 126.4(2) . . ?
C116 N222 Mn2 115.55(18) . . ?
N122 C16 C26 124.1(3) . . ?
N122 C16 H16 117.9 . . ?
C26 C16 H16 117.9 . . ?
C36 C26 C16 118.7(3) . . ?
C36 C26 H26 120.6 . . ?
C16 C26 H26 120.6 . . ?
C26 C36 C46 119.5(3) . . ?
C26 C36 H36 120.2 . . ?
C46 C36 H36 120.2 . . ?
C126 C46 C36 117.5(3) . . ?
C126 C46 C56 119.9(3) . . ?
C36 C46 C56 122.6(3) . . ?
C66 C56 C46 120.8(3) . . ?
C66 C56 H56 119.6 . . ?
C46 C56 H56 119.6 . . ?
C56 C66 C76 121.0(3) . . ?
C56 C66 H66 119.5 . . ?
C76 C66 H66 119.5 . . ?
C86 C76 C116 117.5(3) . . ?
C86 C76 C66 122.9(3) . . ?
C116 C76 C66 119.5(3) . . ?
C96 C86 C76 119.9(3) . . ?
C96 C86 H86 120.0 . . ?
C76 C86 H86 120.0 . . ?
C86 C96 C106 118.6(3) . . ?
C86 C96 H96 120.7 . . ?
C106 C96 H96 120.7 . . ?
N222 C106 C96 123.4(3) . . ?
N222 C106 H106 118.3 . . ?
C96 C106 H106 118.3 . . ?
N222 C116 C76 122.5(3) . . ?
N222 C116 C126 118.1(2) . . ?
C76 C116 C126 119.4(3) . . ?
N122 C126 C46 122.9(3) . . ?
N122 C126 C116 117.7(3) . . ?
C46 C126 C116 119.4(3) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.24
_refine_diff_density_min         -0.37
_refine_diff_density_rms         0.05
_database_code_depnum_ccdc_archive 'CCDC 946225'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-97
_chemical_formula_moiety         '(C5 H10 Mn N2 O8), 1.5(H2 O)'
_chemical_formula_sum            'C5 H13 Mn N2 O9.50'
_chemical_formula_weight         308.11

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'
Mn Mn 0.3368 0.7283 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbcn
_symmetry_space_group_name_Hall  '-P 2n 2ab'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   20.318(4)
_cell_length_b                   11.781(3)
_cell_length_c                   9.576(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2292.2(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    14150
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      26.9

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_absorpt_coefficient_mu    1.198
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_process_details   'Stoe, X-area ver. 1.54'

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  IPDS2
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38702
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         26.75
_reflns_number_total             2435
_reflns_number_gt                1646
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2435
_refine_ls_number_parameters     159
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0271
_refine_ls_wR_factor_ref         0.0404
_refine_ls_wR_factor_gt          0.0375
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_restrained_S_all      0.959
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.646648(14) 0.72869(3) 0.21881(3) 0.01433(7) Uani 1 1 d . . .
O1W O 0.70773(6) 0.58291(11) 0.21967(16) 0.0198(3) Uani 1 1 d . . .
H1W1 H 0.6932 0.5205 0.2414 0.030 Uiso 1 1 d R . .
H1W2 H 0.7333 0.5668 0.1566 0.030 Uiso 1 1 d R . .
O2W O 0.72442(7) 0.79939(12) 0.08258(14) 0.0201(4) Uani 1 1 d . . .
H2W1 H 0.7232 0.8663 0.0499 0.030 Uiso 1 1 d R . .
H2W2 H 0.7495 0.7650 0.0258 0.030 Uiso 1 1 d R . .
O3W O 0.58275(7) 0.63582(13) 0.35550(16) 0.0224(4) Uani 1 1 d . . .
H3W1 H 0.5588 0.5844 0.3285 0.034 Uiso 1 1 d R . .
H3W2 H 0.5708 0.6535 0.4372 0.034 Uiso 1 1 d R . .
O4W O 0.58658(7) 0.67443(13) 0.04348(15) 0.0203(4) Uani 1 1 d . . .
H4W1 H 0.5591 0.7221 0.0219 0.030 Uiso 1 1 d R . .
H4W2 H 0.6086 0.6568 -0.0247 0.030 Uiso 1 1 d R . .
O5W O 0.66349(6) 0.36864(11) 0.29997(16) 0.0204(3) Uani 1 1 d . . .
H5W1 H 0.6391 0.3373 0.2440 0.031 Uiso 1 1 d R . .
H5W2 H 0.6986 0.3353 0.2923 0.031 Uiso 1 1 d R . .
O6W O 0.5000 0.46828(16) 0.2500 0.0197(5) Uani 1 2 d S . .
H6W1 H 0.5181 0.4202 0.2016 0.030 Uiso 1 1 d R . .
C1 C 0.64040(9) 0.97544(16) 0.31443(19) 0.0132(5) Uani 1 1 d . . .
C2 C 0.62600(9) 1.08934(17) 0.2913(2) 0.0147(5) Uani 1 1 d . . .
H2 H 0.6431 1.1532 0.3398 0.018 Uiso 1 1 calc R . .
C3 C 0.58137(10) 1.08940(17) 0.1821(2) 0.0130(5) Uani 1 1 d . . .
C4 C 0.68654(10) 0.92004(19) 0.4134(2) 0.0138(5) Uani 1 1 d . . .
C5 C 0.54837(10) 1.1841(2) 0.1059(2) 0.0137(5) Uani 1 1 d . . .
O1 O 0.69542(6) 0.81380(13) 0.39748(15) 0.0167(3) Uani 1 1 d . . .
O2 O 0.71423(6) 0.97939(12) 0.50440(15) 0.0158(3) Uani 1 1 d . . .
O3 O 0.50293(7) 1.15865(11) 0.02278(16) 0.0178(4) Uani 1 1 d . . .
O4 O 0.56868(6) 1.28348(13) 0.12833(14) 0.0166(3) Uani 1 1 d . . .
N1 N 0.60639(8) 0.90788(13) 0.22582(19) 0.0143(4) Uani 1 1 d . . .
N2 N 0.57064(8) 0.98002(15) 0.14781(18) 0.0144(4) Uani 1 1 d . . .
H2N H 0.5460 0.9467 0.0877 0.022 Uiso 1 1 d R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 O1W 2.1189(13) . ?
Mn1 O3W 2.1437(15) . ?
Mn1 O4W 2.1719(15) . ?
Mn1 O2W 2.2119(14) . ?
Mn1 O1 2.2169(15) . ?
Mn1 N1 2.2650(16) . ?
O1W H1W1 0.8190 . ?
O1W H1W2 0.8186 . ?
O2W H2W1 0.8484 . ?
O2W H2W2 0.8485 . ?
O3W H3W1 0.8188 . ?
O3W H3W2 0.8451 . ?
O4W H4W1 0.8184 . ?
O4W H4W2 0.8184 . ?
O5W H5W1 0.8185 . ?
O5W H5W2 0.8178 . ?
O6W H6W1 0.8192 . ?
C1 N1 1.353(2) . ?
C1 C2 1.391(3) . ?
C1 C4 1.484(3) . ?
C2 C3 1.384(3) . ?
C2 H2 0.9500 . ?
C3 N2 1.348(3) . ?
C3 C5 1.492(3) . ?
C4 O2 1.251(3) . ?
C4 O1 1.274(2) . ?
C5 O3 1.255(2) . ?
C5 O4 1.260(2) . ?
N1 N2 1.345(2) . ?
N2 H2N 0.8579 . ?

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
O1W Mn1 O3W 86.48(6) . . ?
O1W Mn1 O4W 95.37(6) . . ?
O3W Mn1 O4W 88.94(6) . . ?
O1W Mn1 O2W 83.63(6) . . ?
O3W Mn1 O2W 170.04(6) . . ?
O4W Mn1 O2W 93.23(6) . . ?
O1W Mn1 O1 95.84(6) . . ?
O3W Mn1 O1 91.74(6) . . ?
O4W Mn1 O1 168.79(6) . . ?
O2W Mn1 O1 88.03(5) . . ?
O1W Mn1 N1 165.21(5) . . ?
O3W Mn1 N1 103.82(6) . . ?
O4W Mn1 N1 95.41(6) . . ?
O2W Mn1 N1 85.67(6) . . ?
O1 Mn1 N1 73.56(6) . . ?
Mn1 O1W H1W1 121.2 . . ?
Mn1 O1W H1W2 123.8 . . ?
H1W1 O1W H1W2 102.0 . . ?
Mn1 O2W H2W1 123.2 . . ?
Mn1 O2W H2W2 128.9 . . ?
H2W1 O2W H2W2 103.0 . . ?
Mn1 O3W H3W1 123.0 . . ?
Mn1 O3W H3W2 127.9 . . ?
H3W1 O3W H3W2 107.6 . . ?
Mn1 O4W H4W1 112.1 . . ?
Mn1 O4W H4W2 112.5 . . ?
H4W1 O4W H4W2 110.3 . . ?
H5W1 O5W H5W2 104.6 . . ?
N1 C1 C2 111.09(17) . . ?
N1 C1 C4 117.66(18) . . ?
C2 C1 C4 131.21(19) . . ?
C3 C2 C1 105.00(18) . . ?
C3 C2 H2 127.5 . . ?
C1 C2 H2 127.5 . . ?
N2 C3 C2 106.84(17) . . ?
N2 C3 C5 121.52(18) . . ?
C2 C3 C5 131.63(19) . . ?
O2 C4 O1 124.7(2) . . ?
O2 C4 C1 118.89(19) . . ?
O1 C4 C1 116.44(19) . . ?
O3 C5 O4 124.80(19) . . ?
O3 C5 C3 117.54(19) . . ?
O4 C5 C3 117.65(18) . . ?
C4 O1 Mn1 118.25(13) . . ?
N2 N1 C1 104.63(16) . . ?
N2 N1 Mn1 140.15(14) . . ?
C1 N1 Mn1 112.48(12) . . ?
N1 N2 C3 112.43(16) . . ?
N1 N2 H2N 113.5 . . ?
C3 N2 H2N 134.1 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.27
_refine_diff_density_rms         0.06
_database_code_depnum_ccdc_archive 'CCDC 946226'
