# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 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_global


data_global1


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H16 Co N4 O8 S'
_chemical_formula_weight         411.26

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R3c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   23.5913(5)
_cell_length_b                   23.5913(5)
_cell_length_c                   13.7609(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6632.6(4)
_cell_formula_units_Z            18
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3798
_exptl_absorpt_coefficient_mu    1.358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6860
_exptl_absorpt_correction_T_max  0.7824
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4724
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         26.37
_reflns_number_total             1996
_reflns_number_gt                1864
_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 F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0650P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         1996
_refine_ls_number_parameters     217
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0921
_refine_ls_wR_factor_gt          0.0883
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.028
_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
C1 C 0.7233(2) 0.3283(2) 0.0691(3) 0.0173(9) Uani 1 1 d . . .
H1A H 0.7610 0.3251 0.0693 0.021 Uiso 1 1 calc R . .
C2 C 0.6620(2) 0.27274(19) 0.0690(3) 0.0150(9) Uani 1 1 d . . .
C3 C 0.3947(2) -0.3292(2) 0.1476(3) 0.0168(9) Uani 1 1 d . . .
H2A H 0.4354 -0.3265 0.1484 0.020 Uiso 1 1 calc R . .
C4 C 0.3896(2) -0.27316(19) 0.1471(3) 0.0151(9) Uani 1 1 d . . .
C5 C 0.6815(2) 0.1329(2) 0.0562(4) 0.0290(12) Uani 1 1 d . . .
H5A H 0.7044 0.1110 0.0450 0.035 Uiso 1 1 calc R . .
C6 C 0.7062(2) 0.1972(2) 0.0458(4) 0.0245(10) Uani 1 1 d . . .
H6A H 0.7485 0.2275 0.0263 0.029 Uiso 1 1 calc R . .
C7 C 0.5116(2) -0.1987(2) 0.1538(4) 0.0291(12) Uani 1 1 d . . .
H7A H 0.5249 -0.2293 0.1645 0.035 Uiso 1 1 calc R . .
C8 C 0.5501(2) -0.1342(2) 0.1439(4) 0.0309(12) Uani 1 1 d . . .
H8A H 0.5955 -0.1123 0.1465 0.037 Uiso 1 1 calc R . .
C9 C 0.4526(2) -0.1517(2) 0.1304(4) 0.0207(9) Uani 1 1 d . . .
H4A H 0.4168 -0.1456 0.1224 0.025 Uiso 1 1 calc R . .
C10 C 0.6041(2) 0.1517(2) 0.0927(3) 0.0210(10) Uani 1 1 d . . .
H10A H 0.5638 0.1464 0.1111 0.025 Uiso 1 1 calc R . .
Co1 Co 0.55924(2) 0.00052(3) 0.11532(5) 0.01642(16) Uani 1 1 d . . .
N1 N 0.61639(19) 0.10315(18) 0.0860(3) 0.0214(9) Uani 1 1 d . . .
N2 N 0.51362(17) -0.10458(17) 0.1294(3) 0.0199(8) Uani 1 1 d . . .
N3 N 0.65648(17) 0.20982(18) 0.0697(3) 0.0182(8) Uani 1 1 d . . .
N4 N 0.44804(17) -0.21122(17) 0.1449(3) 0.0177(8) Uani 1 1 d . . .
O1 O 0.4243(2) 0.04221(16) 0.9253(3) 0.0350(8) Uani 1 1 d . . .
O2 O 0.4295(2) 0.11957(17) 0.8088(3) 0.0385(9) Uani 1 1 d . . .
O3 O 0.3852(2) 0.1158(2) 0.9665(3) 0.0486(11) Uani 1 1 d . . .
O4 O 0.49962(19) 0.15768(18) 0.9470(4) 0.0499(10) Uani 1 1 d . . .
O1W O 0.52748(15) 0.01124(17) 0.2547(3) 0.0318(8) Uani 1 1 d D . .
H1WA H 0.4888 -0.0107 0.2771 0.038 Uiso 1 1 d RD . .
H1WB H 0.5454 0.0315 0.3070 0.038 Uiso 1 1 d RD . .
O2W O 0.64302(14) 0.01279(14) 0.1951(2) 0.0226(7) Uani 1 1 d D . .
H2WA H 0.6748 0.0209 0.1576 0.027 Uiso 1 1 d RD . .
H2WB H 0.6583 0.0515 0.2164 0.027 Uiso 1 1 d RD . .
O3W O 0.59435(17) -0.01478(18) -0.0142(2) 0.0366(9) Uani 1 1 d D . .
H3WA H 0.6329 0.0046 -0.0374 0.044 Uiso 1 1 d RD . .
H3WB H 0.5744 -0.0271 -0.0682 0.044 Uiso 1 1 d RD . .
O4W O 0.47402(16) -0.00870(19) 0.0595(3) 0.0447(11) Uani 1 1 d D . .
H4WA H 0.4669 0.0132 0.0172 0.054 Uiso 1 1 d RD . .
H4WB H 0.4378 -0.0236 0.0893 0.054 Uiso 1 1 d RD . .
S1 S 0.43554(5) 0.10927(5) 0.91271(8) 0.0188(2) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.017(2) 0.015(2) 0.021(2) 0.0040(18) 0.0017(17) 0.0089(18)
C2 0.013(2) 0.015(2) 0.019(2) -0.0003(16) -0.0001(16) 0.0085(17)
C3 0.013(2) 0.016(2) 0.024(2) 0.0002(18) -0.0016(17) 0.0098(17)
C4 0.016(2) 0.011(2) 0.015(2) -0.0005(16) -0.0015(17) 0.0042(18)
C5 0.019(2) 0.025(2) 0.047(3) 0.003(2) 0.009(2) 0.014(2)
C6 0.017(2) 0.025(2) 0.035(3) 0.005(2) 0.0059(19) 0.013(2)
C7 0.016(2) 0.014(2) 0.061(4) -0.003(2) -0.005(2) 0.0098(19)
C8 0.015(2) 0.018(2) 0.055(4) -0.002(2) -0.004(2) 0.0056(19)
C9 0.016(2) 0.014(2) 0.030(2) 0.0036(19) -0.0005(19) 0.0063(18)
C10 0.012(2) 0.018(2) 0.033(3) 0.0013(19) 0.0042(19) 0.0063(18)
Co1 0.0121(3) 0.0126(2) 0.0233(3) 0.0016(2) 0.0010(2) 0.0052(2)
N1 0.018(2) 0.016(2) 0.031(2) 0.0056(17) 0.0051(16) 0.0092(17)
N2 0.0177(18) 0.0141(19) 0.028(2) -0.0004(16) -0.0009(17) 0.0081(16)
N3 0.0114(17) 0.0164(19) 0.026(2) -0.0027(15) 0.0031(15) 0.0063(15)
N4 0.0108(17) 0.0101(17) 0.030(2) -0.0014(15) 0.0007(16) 0.0034(15)
O1 0.047(2) 0.0197(17) 0.040(2) 0.0054(16) -0.0052(17) 0.0178(16)
O2 0.060(3) 0.0295(19) 0.030(2) -0.0001(16) -0.0007(18) 0.0260(19)
O3 0.047(2) 0.069(3) 0.049(3) 0.019(2) 0.022(2) 0.044(2)
O4 0.035(2) 0.037(2) 0.058(2) -0.004(2) -0.016(2) 0.0032(17)
O1W 0.0229(17) 0.0350(19) 0.035(2) -0.0059(16) 0.0050(15) 0.0129(16)
O2W 0.0198(15) 0.0174(15) 0.0317(17) -0.0037(13) 0.0000(13) 0.0101(13)
O3W 0.0289(18) 0.036(2) 0.0252(18) -0.0051(15) 0.0098(15) 0.0018(16)
O4W 0.0202(18) 0.047(2) 0.061(3) 0.030(2) -0.0022(17) 0.0128(17)
S1 0.0184(5) 0.0164(5) 0.0222(5) 0.0007(4) -0.0004(4) 0.0092(4)

_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
C1 C2 1.383(6) . ?
C1 C2 1.394(6) 2_655 ?
C1 H1A 0.9300 . ?
C2 C1 1.394(6) 3_665 ?
C2 N3 1.423(5) . ?
C3 C4 1.387(6) . ?
C3 C4 1.391(6) 3_655 ?
C3 H2A 0.9300 . ?
C4 C3 1.391(6) 2_545 ?
C4 N4 1.422(5) . ?
C5 C6 1.331(7) . ?
C5 N1 1.393(6) . ?
C5 H5A 0.9300 . ?
C6 N3 1.387(5) . ?
C6 H6A 0.9300 . ?
C7 C8 1.334(6) . ?
C7 N4 1.381(5) . ?
C7 H7A 0.9300 . ?
C8 N2 1.366(6) . ?
C8 H8A 0.9300 . ?
C9 N2 1.308(6) . ?
C9 N4 1.368(5) . ?
C9 H4A 0.9300 . ?
C10 N1 1.317(6) . ?
C10 N3 1.347(6) . ?
C10 H10A 0.9300 . ?
Co1 O4W 2.060(3) . ?
Co1 O3W 2.071(3) . ?
Co1 O1W 2.120(4) . ?
Co1 N1 2.140(4) . ?
Co1 O2W 2.150(3) . ?
Co1 N2 2.162(4) . ?
O1 S1 1.478(3) . ?
O2 S1 1.470(4) . ?
O3 S1 1.471(4) . ?
O4 S1 1.444(4) . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?
O2W H2WA 0.8499 . ?
O2W H2WB 0.8499 . ?
O3W H3WA 0.8500 . ?
O3W H3WB 0.8500 . ?
O4W H4WA 0.8501 . ?
O4W H4WB 0.8501 . ?

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
C2 C1 C2 118.5(4) . 2_655 ?
C2 C1 H1A 120.7 . . ?
C2 C1 H1A 120.7 2_655 . ?
C1 C2 C1 121.5(4) . 3_665 ?
C1 C2 N3 119.8(4) . . ?
C1 C2 N3 118.7(4) 3_665 . ?
C4 C3 C4 118.1(4) . 3_655 ?
C4 C3 H2A 120.9 . . ?
C4 C3 H2A 120.9 3_655 . ?
C3 C4 C3 121.9(4) . 2_545 ?
C3 C4 N4 118.5(4) . . ?
C3 C4 N4 119.6(4) 2_545 . ?
C6 C5 N1 110.6(4) . . ?
C6 C5 H5A 124.7 . . ?
N1 C5 H5A 124.7 . . ?
C5 C6 N3 106.4(4) . . ?
C5 C6 H6A 126.8 . . ?
N3 C6 H6A 126.8 . . ?
C8 C7 N4 106.3(4) . . ?
C8 C7 H7A 126.9 . . ?
N4 C7 H7A 126.9 . . ?
C7 C8 N2 110.8(4) . . ?
C7 C8 H8A 124.6 . . ?
N2 C8 H8A 124.6 . . ?
N2 C9 N4 111.2(4) . . ?
N2 C9 H4A 124.4 . . ?
N4 C9 H4A 124.4 . . ?
N1 C10 N3 112.4(4) . . ?
N1 C10 H10A 123.8 . . ?
N3 C10 H10A 123.8 . . ?
O4W Co1 O3W 96.59(17) . . ?
O4W Co1 O1W 88.03(15) . . ?
O3W Co1 O1W 174.36(15) . . ?
O4W Co1 N1 94.51(15) . . ?
O3W Co1 N1 87.39(15) . . ?
O1W Co1 N1 95.50(15) . . ?
O4W Co1 O2W 171.00(15) . . ?
O3W Co1 O2W 92.40(14) . . ?
O1W Co1 O2W 82.99(13) . . ?
N1 Co1 O2W 85.82(13) . . ?
O4W Co1 N2 90.71(15) . . ?
O3W Co1 N2 83.72(16) . . ?
O1W Co1 N2 93.02(15) . . ?
N1 Co1 N2 170.15(14) . . ?
O2W Co1 N2 90.32(13) . . ?
C10 N1 C5 104.4(4) . . ?
C10 N1 Co1 133.0(3) . . ?
C5 N1 Co1 122.6(3) . . ?
C9 N2 C8 105.7(4) . . ?
C9 N2 Co1 132.9(3) . . ?
C8 N2 Co1 121.3(3) . . ?
C10 N3 C6 106.3(4) . . ?
C10 N3 C2 128.6(4) . . ?
C6 N3 C2 125.2(4) . . ?
C9 N4 C7 106.0(4) . . ?
C9 N4 C4 126.5(4) . . ?
C7 N4 C4 127.5(4) . . ?
Co1 O1W H1WA 126.2 . . ?
Co1 O1W H1WB 136.6 . . ?
H1WA O1W H1WB 96.7 . . ?
Co1 O2W H2WA 111.7 . . ?
Co1 O2W H2WB 100.8 . . ?
H2WA O2W H2WB 96.7 . . ?
Co1 O3W H3WA 130.0 . . ?
Co1 O3W H3WB 127.6 . . ?
H3WA O3W H3WB 96.7 . . ?
Co1 O4W H4WA 132.2 . . ?
Co1 O4W H4WB 126.2 . . ?
H4WA O4W H4WB 96.7 . . ?
O4 S1 O2 109.7(3) . . ?
O4 S1 O3 109.5(3) . . ?
O2 S1 O3 108.8(2) . . ?
O4 S1 O1 111.4(2) . . ?
O2 S1 O1 108.1(2) . . ?
O3 S1 O1 109.3(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.069
_database_code_depnum_ccdc_archive 'CCDC 923879'
#######################################################################
#
#                 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_global

# Attachment 'Mn.cif'


data_global2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H16 Mn N4 O8 S'
_chemical_formula_weight         407.27

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R3c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'x, x-y, z+1/2'
'-x+y, y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'

_cell_length_a                   23.8731(5)
_cell_length_b                   23.8731(5)
_cell_length_c                   13.8236(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6822.9(3)
_cell_formula_units_Z            18
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3762
_exptl_absorpt_coefficient_mu    1.059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7417
_exptl_absorpt_correction_T_max  0.8161
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4678
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2110
_reflns_number_gt                1957
_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 F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0940P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.35(4)
_refine_ls_number_reflns         2110
_refine_ls_number_parameters     242
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.1282
_refine_ls_wR_factor_gt          0.1226
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.088
_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 1.00100(4) 0.44370(3) 0.35129(8) 0.0200(2) Uani 1 1 d . . .
O1WA O 0.9854(3) 0.3911(3) 0.4865(4) 0.0554(15) Uani 1 1 d . . .
O2WA O 1.0143(2) 0.3704(2) 0.2724(3) 0.0317(9) Uani 1 1 d . . .
O3WA O 1.0099(3) 0.4836(3) 0.2047(3) 0.0378(11) Uani 1 1 d . . .
O4WA O 0.9964(3) 0.5257(3) 0.3994(5) 0.0613(18) Uani 1 1 d . . .
N3 N 0.8929(2) 0.3809(2) 0.3412(4) 0.0249(10) Uani 1 1 d . . .
N1 N 1.1076(2) 0.4896(2) 0.3855(4) 0.0280(11) Uani 1 1 d . . .
C6 C 0.8633(3) 0.3156(3) 0.3290(6) 0.0361(16) Uani 1 1 d . . .
H5 H 0.8846 0.2919 0.3274 0.043 Uiso 1 1 calc R . .
C8 C 0.8462(3) 0.3946(3) 0.3388(4) 0.0238(12) Uani 1 1 d . . .
H7 H 0.8526 0.4362 0.3445 0.029 Uiso 1 1 calc R . .
N4 N 0.7874(2) 0.3411(2) 0.3271(4) 0.0214(10) Uani 1 1 d . . .
C7 C 0.7997(3) 0.2903(3) 0.3197(6) 0.0365(16) Uani 1 1 d . . .
H6 H 0.7693 0.2469 0.3101 0.044 Uiso 1 1 calc R . .
C9 C 0.7255(2) 0.3366(3) 0.3247(4) 0.0188(11) Uani 1 1 d . . .
C10 C 0.6705(3) 0.2772(2) 0.3237(4) 0.0219(12) Uani 1 1 d . . .
H8 H 0.6730 0.2395 0.3223 0.026 Uiso 1 1 calc R . .
C4 C 1.1363(3) 0.4533(3) 0.4118(5) 0.0352(16) Uani 1 1 d . . .
H3 H 1.1144 0.4087 0.4203 0.042 Uiso 1 1 calc R . .
C5 C 1.1548(3) 0.5493(3) 0.3823(4) 0.0243(12) Uani 1 1 d . . .
H4 H 1.1496 0.5845 0.3676 0.029 Uiso 1 1 calc R . .
C3 C 1.1999(3) 0.4924(3) 0.4229(5) 0.0303(14) Uani 1 1 d . . .
H2 H 1.2300 0.4803 0.4406 0.036 Uiso 1 1 calc R . .
C2 C 1.2740(2) 0.6114(2) 0.4045(4) 0.0188(11) Uani 1 1 d . . .
C1 C 1.2765(2) 0.6705(3) 0.4039(4) 0.0221(12) Uani 1 1 d . . .
H1 H 1.2390 0.6731 0.4032 0.027 Uiso 1 1 calc R . .
N2 N 1.2123(2) 0.5540(2) 0.4030(4) 0.0219(10) Uani 1 1 d . . .
H4WA H 0.976(3) 0.545(3) 0.381(4) 0.026 Uiso 1 1 d D . .
H1WA H 0.959(3) 0.395(3) 0.528(5) 0.026 Uiso 1 1 d D . .
H3WA H 0.982(3) 0.494(3) 0.203(5) 0.026 Uiso 1 1 d D . .
H2WA H 1.022(3) 0.356(3) 0.307(4) 0.026 Uiso 1 1 d D . .
H2WB H 1.052(3) 0.393(3) 0.237(4) 0.026 Uiso 1 1 d D . .
H1WB H 1.006(3) 0.384(3) 0.524(5) 0.026 Uiso 1 1 d D . .
H4WB H 1.021(3) 0.551(3) 0.438(4) 0.026 Uiso 1 1 d D . .
H3WB H 1.021(3) 0.478(4) 0.165(5) 0.026 Uiso 1 1 d D . .
S1 S 0.56507(6) 0.89191(6) 0.55388(11) 0.0218(3) Uani 1 1 d . . .
O1 O 0.5759(2) 0.9581(2) 0.5403(3) 0.0380(10) Uani 1 1 d . . .
O2 O 0.5030(3) 0.8428(3) 0.5190(6) 0.0779(19) Uani 1 1 d . . .
O3 O 0.5705(3) 0.8811(2) 0.6575(4) 0.0548(14) Uani 1 1 d . . .
O4 O 0.6150(3) 0.8858(3) 0.5039(5) 0.075(2) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0153(3) 0.0181(4) 0.0276(4) -0.0016(3) -0.0016(3) 0.0091(3)
O1WA 0.052(3) 0.086(4) 0.039(3) 0.030(3) 0.007(2) 0.042(3)
O2WA 0.036(2) 0.028(2) 0.036(2) 0.0065(18) 0.005(2) 0.0190(19)
O3WA 0.049(3) 0.045(3) 0.032(2) 0.004(2) 0.006(2) 0.033(2)
O4WA 0.080(4) 0.063(3) 0.075(4) -0.048(3) -0.048(3) 0.062(3)
N3 0.015(2) 0.027(2) 0.035(3) -0.001(2) -0.0005(19) 0.012(2)
N1 0.023(2) 0.020(2) 0.041(3) -0.001(2) -0.008(2) 0.011(2)
C6 0.021(3) 0.023(3) 0.068(5) -0.003(3) 0.003(3) 0.014(3)
C8 0.019(3) 0.014(3) 0.032(3) -0.002(2) -0.002(2) 0.004(2)
N4 0.012(2) 0.018(2) 0.034(3) 0.0001(19) 0.0012(19) 0.0074(18)
C7 0.024(3) 0.013(3) 0.072(5) 0.001(3) 0.004(3) 0.008(2)
C9 0.012(2) 0.025(3) 0.018(2) -0.001(2) 0.0012(19) 0.008(2)
C10 0.021(3) 0.016(2) 0.031(3) -0.001(2) 0.000(2) 0.011(2)
C4 0.023(3) 0.021(3) 0.060(4) 0.008(3) -0.007(3) 0.009(2)
C5 0.020(3) 0.020(3) 0.033(3) 0.005(2) 0.001(2) 0.010(2)
C3 0.023(3) 0.021(3) 0.048(4) 0.001(3) -0.007(3) 0.012(2)
C2 0.016(3) 0.022(3) 0.020(2) 0.001(2) 0.001(2) 0.010(2)
C1 0.020(3) 0.020(3) 0.028(3) 0.004(2) 0.002(2) 0.010(2)
N2 0.017(2) 0.014(2) 0.034(3) 0.0057(19) -0.0009(19) 0.0074(19)
S1 0.0219(6) 0.0188(6) 0.0258(7) 0.0002(5) -0.0009(5) 0.0109(5)
O1 0.054(3) 0.028(2) 0.038(2) 0.003(2) -0.003(2) 0.025(2)
O2 0.074(4) 0.043(3) 0.091(4) -0.010(3) -0.047(4) 0.009(3)
O3 0.092(4) 0.033(3) 0.038(3) 0.008(2) 0.005(3) 0.030(3)
O4 0.062(4) 0.089(5) 0.101(6) 0.031(4) 0.037(4) 0.057(4)

_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 O4WA 2.121(4) . ?
Mn1 O1WA 2.177(5) . ?
Mn1 O3WA 2.204(5) . ?
Mn1 O2WA 2.215(4) . ?
Mn1 N3 2.248(5) . ?
Mn1 N1 2.261(5) . ?
O1WA H1WA 0.89(6) . ?
O1WA H1WB 0.79(6) . ?
O2WA H2WA 0.66(6) . ?
O2WA H2WB 0.93(6) . ?
O3WA H3WA 0.82(6) . ?
O3WA H3WB 0.64(6) . ?
O4WA H4WA 0.85(6) . ?
O4WA H4WB 0.79(6) . ?
N3 C8 1.310(7) . ?
N3 C6 1.364(8) . ?
N1 C5 1.303(8) . ?
N1 C4 1.394(7) . ?
C6 C7 1.330(8) . ?
C6 H5 0.9300 . ?
C8 N4 1.354(6) . ?
C8 H7 0.9300 . ?
N4 C7 1.386(7) . ?
N4 C9 1.428(7) . ?
C7 H6 0.9300 . ?
C9 C10 1.369(7) . ?
C9 C10 1.389(7) 2_655 ?
C10 C9 1.389(7) 3_665 ?
C10 H8 0.9300 . ?
C4 C3 1.336(8) . ?
C4 H3 0.9300 . ?
C5 N2 1.350(7) . ?
C5 H4 0.9300 . ?
C3 N2 1.376(7) . ?
C3 H2 0.9300 . ?
C2 C1 1.381(7) . ?
C2 C1 1.393(7) 2_755 ?
C2 N2 1.425(6) . ?
C1 C2 1.393(7) 3_775 ?
C1 H1 0.9300 . ?
S1 O2 1.437(5) . ?
S1 O4 1.446(6) . ?
S1 O3 1.473(5) . ?
S1 O1 1.481(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
O4WA Mn1 O1WA 100.9(3) . . ?
O4WA Mn1 O3WA 85.8(2) . . ?
O1WA Mn1 O3WA 172.0(2) . . ?
O4WA Mn1 O2WA 167.7(2) . . ?
O1WA Mn1 O2WA 91.0(2) . . ?
O3WA Mn1 O2WA 82.41(18) . . ?
O4WA Mn1 N3 93.6(2) . . ?
O1WA Mn1 N3 82.0(2) . . ?
O3WA Mn1 N3 93.50(19) . . ?
O2WA Mn1 N3 90.75(18) . . ?
O4WA Mn1 N1 93.0(2) . . ?
O1WA Mn1 N1 85.8(2) . . ?
O3WA Mn1 N1 98.1(2) . . ?
O2WA Mn1 N1 85.11(17) . . ?
N3 Mn1 N1 167.01(17) . . ?
Mn1 O1WA H1WA 115(4) . . ?
Mn1 O1WA H1WB 139(5) . . ?
H1WA O1WA H1WB 98(5) . . ?
Mn1 O2WA H2WA 103(6) . . ?
Mn1 O2WA H2WB 106(4) . . ?
H2WA O2WA H2WB 105(6) . . ?
Mn1 O3WA H3WA 104(5) . . ?
Mn1 O3WA H3WB 131(6) . . ?
H3WA O3WA H3WB 120(7) . . ?
Mn1 O4WA H4WA 135(4) . . ?
Mn1 O4WA H4WB 124(4) . . ?
H4WA O4WA H4WB 101(5) . . ?
C8 N3 C6 105.2(5) . . ?
C8 N3 Mn1 132.2(4) . . ?
C6 N3 Mn1 122.4(4) . . ?
C5 N1 C4 105.3(5) . . ?
C5 N1 Mn1 132.2(4) . . ?
C4 N1 Mn1 122.5(4) . . ?
C7 C6 N3 110.6(5) . . ?
C7 C6 H5 124.7 . . ?
N3 C6 H5 124.7 . . ?
N3 C8 N4 112.2(5) . . ?
N3 C8 H7 123.9 . . ?
N4 C8 H7 123.9 . . ?
C8 N4 C7 105.2(5) . . ?
C8 N4 C9 128.2(5) . . ?
C7 N4 C9 126.6(4) . . ?
C6 C7 N4 106.8(5) . . ?
C6 C7 H6 126.6 . . ?
N4 C7 H6 126.6 . . ?
C10 C9 C10 121.5(5) . 2_655 ?
C10 C9 N4 119.9(5) . . ?
C10 C9 N4 118.6(5) 2_655 . ?
C9 C10 C9 118.5(5) . 3_665 ?
C9 C10 H8 120.8 . . ?
C9 C10 H8 120.8 3_665 . ?
C3 C4 N1 109.7(5) . . ?
C3 C4 H3 125.2 . . ?
N1 C4 H3 125.2 . . ?
N1 C5 N2 111.8(5) . . ?
N1 C5 H4 124.1 . . ?
N2 C5 H4 124.1 . . ?
C4 C3 N2 106.5(5) . . ?
C4 C3 H2 126.7 . . ?
N2 C3 H2 126.7 . . ?
C1 C2 C1 122.4(5) . 2_755 ?
C1 C2 N2 118.5(5) . . ?
C1 C2 N2 119.0(5) 2_755 . ?
C2 C1 C2 117.6(5) . 3_775 ?
C2 C1 H1 121.2 . . ?
C2 C1 H1 121.2 3_775 . ?
C5 N2 C3 106.7(5) . . ?
C5 N2 C2 127.0(4) . . ?
C3 N2 C2 126.2(5) . . ?
O2 S1 O4 108.8(5) . . ?
O2 S1 O3 109.2(4) . . ?
O4 S1 O3 107.4(4) . . ?
O2 S1 O1 112.8(4) . . ?
O4 S1 O1 109.5(3) . . ?
O3 S1 O1 109.1(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4WA Mn1 N3 C8 16.8(6) . . . . ?
O1WA Mn1 N3 C8 117.4(6) . . . . ?
O3WA Mn1 N3 C8 -69.2(6) . . . . ?
O2WA Mn1 N3 C8 -151.6(6) . . . . ?
N1 Mn1 N3 C8 137.2(8) . . . . ?
O4WA Mn1 N3 C6 -168.0(6) . . . . ?
O1WA Mn1 N3 C6 -67.5(6) . . . . ?
O3WA Mn1 N3 C6 105.9(5) . . . . ?
O2WA Mn1 N3 C6 23.5(6) . . . . ?
N1 Mn1 N3 C6 -47.7(12) . . . . ?
O4WA Mn1 N1 C5 -33.3(6) . . . . ?
O1WA Mn1 N1 C5 -134.1(6) . . . . ?
O3WA Mn1 N1 C5 52.9(6) . . . . ?
O2WA Mn1 N1 C5 134.5(6) . . . . ?
N3 Mn1 N1 C5 -153.7(7) . . . . ?
O4WA Mn1 N1 C4 150.3(5) . . . . ?
O1WA Mn1 N1 C4 49.5(5) . . . . ?
O3WA Mn1 N1 C4 -123.5(5) . . . . ?
O2WA Mn1 N1 C4 -41.9(5) . . . . ?
N3 Mn1 N1 C4 29.9(12) . . . . ?
C8 N3 C6 C7 -0.2(8) . . . . ?
Mn1 N3 C6 C7 -176.4(5) . . . . ?
C6 N3 C8 N4 0.9(7) . . . . ?
Mn1 N3 C8 N4 176.7(4) . . . . ?
N3 C8 N4 C7 -1.3(7) . . . . ?
N3 C8 N4 C9 177.5(5) . . . . ?
N3 C6 C7 N4 -0.6(9) . . . . ?
C8 N4 C7 C6 1.1(7) . . . . ?
C9 N4 C7 C6 -177.7(6) . . . . ?
C8 N4 C9 C10 -172.2(5) . . . . ?
C7 N4 C9 C10 6.4(9) . . . . ?
C8 N4 C9 C10 7.6(9) . . . 2_655 ?
C7 N4 C9 C10 -173.8(6) . . . 2_655 ?
C10 C9 C10 C9 -2.0(12) 2_655 . . 3_665 ?
N4 C9 C10 C9 177.8(3) . . . 3_665 ?
C5 N1 C4 C3 -0.4(8) . . . . ?
Mn1 N1 C4 C3 176.8(5) . . . . ?
C4 N1 C5 N2 1.2(7) . . . . ?
Mn1 N1 C5 N2 -175.7(4) . . . . ?
N1 C4 C3 N2 -0.4(8) . . . . ?
C1 C2 C1 C2 -1.1(12) 2_755 . . 3_775 ?
N2 C2 C1 C2 -179.4(3) . . . 3_775 ?
N1 C5 N2 C3 -1.4(7) . . . . ?
N1 C5 N2 C2 178.8(5) . . . . ?
C4 C3 N2 C5 1.1(7) . . . . ?
C4 C3 N2 C2 -179.1(5) . . . . ?
C1 C2 N2 C5 13.9(8) . . . . ?
C1 C2 N2 C5 -164.5(6) 2_755 . . . ?
C1 C2 N2 C3 -165.8(6) . . . . ?
C1 C2 N2 C3 15.8(8) 2_755 . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.084



_database_code_depnum_ccdc_archive 'CCDC 923880'