# Supplementary Material (ESI) for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2011

data_global
_journal_name_full               CrystEngComm
_journal_coden_cambridge         1350
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_address     
;
Center of Applied Solid State Chemistry Research
Ningbo University
Ningbo 315211
P. R. China

;
_publ_contact_author_email       zhengyueqing@nbu.edu.cn
_publ_contact_author_fax         '86 574 87600747'
_publ_contact_author_phone       '86 574 87600747'
_publ_contact_author_name        'Yue-Qing Zheng'
_publ_author_name                'Xu Wei'

data_shx97_1
_database_code_depnum_ccdc_archive 'CCDC 740623'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H22 Mn3 N2 O21'
_chemical_formula_sum            'C16 H22 Mn3 N2 O21'
_chemical_formula_weight         743.18

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           Monoclinic
_symmetry_space_group_name_H-M   'C c'
_symmetry_space_group_name_Hall  C-2yc

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

_cell_length_a                   19.824(4)
_cell_length_b                   6.8479(14)
_cell_length_c                   19.765(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 117.16(3)
_cell_angle_gamma                90.00
_cell_volume                     2387.3(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    10063
_cell_measurement_theta_min      3.2
_cell_measurement_theta_max      27.4

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1500
_exptl_absorpt_coefficient_mu    1.672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(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  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         0
_diffrn_standards_interval_count image
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            11244
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.19
_diffrn_reflns_theta_max         27.43
_reflns_number_total             5318
_reflns_number_gt                4808
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        RAPID-AUTO
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    XP
_computing_publication_material  SHELXL-97

_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^)+(0.0278P)^2^+1.5311P] 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    constr
_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   -0.003(13)
_refine_ls_number_reflns         5318
_refine_ls_number_parameters     379
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0270
_refine_ls_wR_factor_ref         0.0685
_refine_ls_wR_factor_gt          0.0578
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.110
_refine_ls_shift/su_max          0.004
_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 0.82821(2) 0.24006(7) 0.90210(3) 0.02189(11) Uani 1 1 d . . .
Mn2 Mn 0.59382(3) 0.21191(7) 0.57817(3) 0.02470(12) Uani 1 1 d . . .
Mn3 Mn 0.36469(3) 0.14914(7) 0.69368(3) 0.02287(11) Uani 1 1 d . . .
N1 N 0.71151(13) 0.2478(4) 0.88987(15) 0.0175(5) Uani 1 1 d . . .
C1 C 0.65220(16) 0.2063(4) 0.82295(17) 0.0169(6) Uani 1 1 d . . .
C2 C 0.57880(16) 0.1983(4) 0.81443(17) 0.0186(6) Uani 1 1 d . . .
H2 H 0.5383 0.1701 0.7674 0.022 Uiso 1 1 calc R . .
C3 C 0.56677(17) 0.2335(4) 0.87782(17) 0.0169(6) Uani 1 1 d . . .
C4 C 0.62864(16) 0.2781(4) 0.94654(17) 0.0174(6) Uani 1 1 d . . .
H4 H 0.6224 0.3012 0.9897 0.021 Uiso 1 1 calc R . .
C5 C 0.70068(17) 0.2879(4) 0.94999(17) 0.0171(6) Uani 1 1 d . . .
C6 C 0.67425(18) 0.1639(5) 0.76043(18) 0.0213(6) Uani 1 1 d . . .
O1 O 0.74408(13) 0.1422(4) 0.78203(14) 0.0348(6) Uani 1 1 d . . .
O2 O 0.62166(14) 0.1543(4) 0.69441(13) 0.0309(5) Uani 1 1 d . . .
C7 C 0.48835(16) 0.2200(4) 0.87365(17) 0.0176(6) Uani 1 1 d . . .
O3 O 0.43525(12) 0.1529(4) 0.81297(13) 0.0278(5) Uani 1 1 d . . .
O4 O 0.48123(12) 0.2693(4) 0.93056(13) 0.0270(5) Uani 1 1 d . . .
C8 C 0.77268(17) 0.3369(4) 1.02027(17) 0.0176(6) Uani 1 1 d . . .
O5 O 0.76852(11) 0.3751(4) 1.08019(12) 0.0245(5) Uani 1 1 d . . .
O6 O 0.83293(12) 0.3375(4) 1.01334(13) 0.0271(5) Uani 1 1 d . . .
N2 N 0.59854(15) 0.2315(4) 0.46429(15) 0.0191(5) Uani 1 1 d . . .
C9 C 0.66594(17) 0.2153(4) 0.46357(17) 0.0182(6) Uani 1 1 d . . .
C10 C 0.67296(16) 0.2454(4) 0.39730(17) 0.0182(6) Uani 1 1 d . . .
H10 H 0.7203 0.2379 0.3984 0.022 Uiso 1 1 calc R . .
C11 C 0.60892(16) 0.2865(4) 0.32977(17) 0.0177(6) Uani 1 1 d . . .
C12 C 0.53905(18) 0.2974(5) 0.33098(18) 0.0199(6) Uani 1 1 d . . .
H12 H 0.4948 0.3223 0.2866 0.024 Uiso 1 1 calc R . .
C13 C 0.53685(16) 0.2706(4) 0.39897(18) 0.0181(6) Uani 1 1 d . . .
C14 C 0.73087(18) 0.1550(5) 0.53914(17) 0.0219(6) Uani 1 1 d . . .
O7 O 0.71414(13) 0.1321(4) 0.59311(13) 0.0299(5) Uani 1 1 d . . .
O8 O 0.79424(13) 0.1294(4) 0.54289(13) 0.0315(6) Uani 1 1 d . . .
C15 C 0.61233(17) 0.3170(5) 0.25576(17) 0.0201(6) Uani 1 1 d . . .
O9 O 0.67325(13) 0.3738(4) 0.25847(14) 0.0307(5) Uani 1 1 d . . .
O10 O 0.55224(13) 0.2862(4) 0.19506(13) 0.0303(5) Uani 1 1 d . . .
C16 C 0.46408(19) 0.2726(5) 0.4054(2) 0.0247(7) Uani 1 1 d . . .
O11 O 0.40372(13) 0.3195(4) 0.34862(14) 0.0326(6) Uani 1 1 d . . .
O12 O 0.46691(15) 0.2249(4) 0.46691(17) 0.0397(7) Uani 1 1 d . . .
O13 O 0.86371(15) -0.0505(4) 0.95614(16) 0.0389(6) Uani 1 1 d . . .
H13A H 0.8392 -0.1091 0.9756 0.047 Uiso 1 1 d . . .
H13B H 0.8849 -0.1162 0.9427 0.047 Uiso 1 1 d . . .
O14 O 0.82025(13) 0.5462(4) 0.86417(14) 0.0318(5) Uani 1 1 d . . .
H14A H 0.7786 0.5810 0.8317 0.038 Uiso 1 1 d . . .
H14B H 0.8420 0.5797 0.8428 0.038 Uiso 1 1 d . . .
O15 O 0.64981(13) 0.5015(4) 0.61465(13) 0.0323(5) Uani 1 1 d . . .
H15A H 0.6610 0.5514 0.6557 0.039 Uiso 1 1 d . . .
H15B H 0.6713 0.5534 0.5896 0.039 Uiso 1 1 d . . .
O16 O 0.50339(17) 0.4042(5) 0.59515(17) 0.0516(8) Uani 1 1 d . . .
H16A H 0.4775 0.4383 0.5507 0.062 Uiso 1 1 d . . .
H16B H 0.5118 0.5093 0.6202 0.062 Uiso 1 1 d . . .
O17 O 0.55587(18) -0.0844(4) 0.56895(14) 0.0469(7) Uani 1 1 d . . .
H17A H 0.5702 -0.1555 0.6093 0.056 Uiso 1 1 d . . .
H17B H 0.5289 -0.1637 0.5374 0.056 Uiso 1 1 d . . .
O18 O 0.28185(15) 0.3402(4) 0.70663(15) 0.0369(6) Uani 1 1 d . . .
H18A H 0.2769 0.3932 0.7384 0.044 Uiso 1 1 d . . .
H18B H 0.2645 0.4063 0.6688 0.044 Uiso 1 1 d . . .
O19 O 0.32834(15) -0.1318(4) 0.71174(14) 0.0410(7) Uani 1 1 d . . .
H19A H 0.3432 -0.1925 0.7496 0.049 Uiso 1 1 d . . .
H19B H 0.2905 -0.1977 0.6801 0.049 Uiso 1 1 d . . .
O20 O 0.43951(13) 0.0090(4) 0.65365(14) 0.0369(6) Uani 1 1 d . . .
H20A H 0.4252 0.0127 0.6104 0.044 Uiso 1 1 d . . .
H20B H 0.4677 -0.0788 0.6696 0.044 Uiso 1 1 d . . .
O21 O 0.40611(13) 0.4220(4) 0.66773(14) 0.0357(6) Uani 1 1 d . . .
H21A H 0.4320 0.4388 0.6477 0.043 Uiso 1 1 d . . .
H21B H 0.3690 0.4540 0.6355 0.043 Uiso 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 0.0164(2) 0.0322(3) 0.0202(2) -0.0027(2) 0.01105(18) -0.0010(2)
Mn2 0.0310(3) 0.0306(3) 0.0147(2) -0.0010(2) 0.0122(2) -0.0044(2)
Mn3 0.0196(2) 0.0313(3) 0.0150(2) 0.0010(2) 0.00560(17) 0.0000(2)
N1 0.0130(12) 0.0237(13) 0.0141(12) -0.0009(10) 0.0049(10) -0.0010(10)
C1 0.0166(14) 0.0191(14) 0.0141(14) -0.0004(11) 0.0062(12) 0.0001(12)
C2 0.0155(14) 0.0222(15) 0.0164(15) -0.0008(13) 0.0059(11) -0.0018(13)
C3 0.0186(14) 0.0196(15) 0.0145(14) 0.0008(12) 0.0094(12) 0.0013(12)
C4 0.0159(14) 0.0217(14) 0.0147(15) -0.0004(12) 0.0071(12) 0.0010(12)
C5 0.0165(14) 0.0212(14) 0.0150(15) -0.0003(12) 0.0084(12) 0.0010(12)
C6 0.0245(16) 0.0260(16) 0.0172(16) -0.0035(13) 0.0128(13) -0.0049(14)
O1 0.0223(12) 0.0586(18) 0.0278(14) -0.0157(12) 0.0152(10) -0.0050(12)
O2 0.0330(12) 0.0471(15) 0.0128(11) -0.0043(10) 0.0106(10) -0.0107(12)
C7 0.0140(13) 0.0215(15) 0.0150(14) 0.0051(12) 0.0046(11) 0.0006(12)
O3 0.0177(11) 0.0442(14) 0.0166(12) -0.0020(10) 0.0034(9) -0.0058(11)
O4 0.0208(11) 0.0432(14) 0.0207(12) 0.0002(10) 0.0127(10) 0.0033(10)
C8 0.0169(14) 0.0217(15) 0.0153(15) 0.0009(12) 0.0082(12) 0.0006(13)
O5 0.0174(10) 0.0409(13) 0.0145(11) -0.0053(10) 0.0067(9) -0.0023(10)
O6 0.0184(11) 0.0455(14) 0.0204(12) -0.0073(11) 0.0114(9) -0.0027(11)
N2 0.0199(12) 0.0216(13) 0.0184(13) -0.0024(11) 0.0109(11) -0.0044(11)
C9 0.0208(15) 0.0188(14) 0.0163(15) -0.0009(12) 0.0096(12) -0.0014(13)
C10 0.0144(14) 0.0259(16) 0.0150(15) -0.0006(12) 0.0074(12) -0.0031(12)
C11 0.0165(14) 0.0226(15) 0.0160(14) -0.0008(12) 0.0091(12) -0.0024(12)
C12 0.0199(15) 0.0227(15) 0.0182(15) -0.0010(12) 0.0096(12) -0.0010(13)
C13 0.0145(14) 0.0234(15) 0.0188(15) -0.0024(12) 0.0096(12) -0.0024(12)
C14 0.0224(15) 0.0269(16) 0.0151(15) -0.0019(13) 0.0075(12) 0.0007(14)
O7 0.0289(12) 0.0445(15) 0.0183(11) 0.0064(11) 0.0125(10) 0.0089(11)
O8 0.0256(12) 0.0476(15) 0.0211(12) 0.0029(11) 0.0106(10) 0.0079(11)
C15 0.0205(15) 0.0230(16) 0.0185(16) 0.0032(13) 0.0104(13) 0.0007(13)
O9 0.0225(11) 0.0511(15) 0.0239(13) 0.0004(11) 0.0153(10) -0.0076(11)
O10 0.0282(12) 0.0466(15) 0.0153(12) 0.0019(10) 0.0093(10) -0.0060(11)
C16 0.0273(17) 0.0220(17) 0.0350(19) -0.0067(14) 0.0230(15) -0.0038(14)
O11 0.0195(11) 0.0469(15) 0.0317(14) -0.0115(12) 0.0120(10) -0.0021(11)
O12 0.0412(15) 0.0466(16) 0.0491(17) 0.0143(13) 0.0359(13) 0.0121(13)
O13 0.0489(16) 0.0310(14) 0.0550(17) 0.0048(12) 0.0393(14) 0.0059(12)
O14 0.0280(12) 0.0388(14) 0.0316(13) 0.0037(11) 0.0163(10) 0.0009(11)
O15 0.0389(13) 0.0373(14) 0.0294(13) -0.0053(11) 0.0232(11) -0.0057(12)
O16 0.0477(16) 0.0565(18) 0.0432(17) -0.0079(15) 0.0142(14) -0.0024(15)
O17 0.080(2) 0.0321(13) 0.0185(13) -0.0031(11) 0.0139(13) -0.0175(14)
O18 0.0437(15) 0.0406(15) 0.0317(14) 0.0001(12) 0.0219(12) 0.0120(12)
O19 0.0478(16) 0.0377(14) 0.0225(13) 0.0047(11) 0.0031(11) -0.0158(13)
O20 0.0325(13) 0.0531(16) 0.0242(13) 0.0020(12) 0.0121(10) 0.0139(12)
O21 0.0262(12) 0.0449(15) 0.0348(14) 0.0070(12) 0.0127(11) -0.0027(12)

_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 O14 2.208(3) . ?
Mn1 N1 2.214(2) . ?
Mn1 O13 2.215(3) . ?
Mn1 O11 2.229(3) 4 ?
Mn1 O6 2.258(2) . ?
Mn1 O1 2.291(3) . ?
Mn1 O12 2.458(3) 4 ?
Mn2 O2 2.140(2) . ?
Mn2 O17 2.143(3) . ?
Mn2 O15 2.226(2) . ?
Mn2 N2 2.299(3) . ?
Mn2 O7 2.331(2) . ?
Mn2 O16 2.369(3) . ?
Mn2 O12 2.474(3) . ?
Mn3 O3 2.123(2) . ?
Mn3 O19 2.140(3) . ?
Mn3 O5 2.188(2) 4_454 ?
Mn3 O21 2.194(3) . ?
Mn3 O20 2.195(2) . ?
Mn3 O18 2.204(2) . ?
N1 C5 1.329(4) . ?
N1 C1 1.339(4) . ?
C1 C2 1.387(4) . ?
C1 C6 1.515(4) . ?
C2 C3 1.399(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.386(4) . ?
C3 C7 1.521(4) . ?
C4 C5 1.400(4) . ?
C4 H4 0.9300 . ?
C5 C8 1.506(4) . ?
C6 O2 1.246(4) . ?
C6 O1 1.257(4) . ?
C7 O4 1.243(4) . ?
C7 O3 1.267(4) . ?
C8 O5 1.252(4) . ?
C8 O6 1.263(4) . ?
O5 Mn3 2.188(2) 4 ?
N2 C13 1.339(4) . ?
N2 C9 1.347(4) . ?
C9 C10 1.394(4) . ?
C9 C14 1.517(4) . ?
C10 C11 1.388(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.398(4) . ?
C11 C15 1.509(4) . ?
C12 C13 1.376(4) . ?
C12 H12 0.9300 . ?
C13 C16 1.505(4) . ?
C14 O8 1.237(4) . ?
C14 O7 1.263(4) . ?
C15 O9 1.246(4) . ?
C15 O10 1.264(4) . ?
C16 O12 1.236(4) . ?
C16 O11 1.252(4) . ?
O11 Mn1 2.229(3) 4_454 ?
O12 Mn1 2.458(3) 4_454 ?
O13 H13A 0.8472 . ?
O13 H13B 0.7430 . ?
O14 H14A 0.8162 . ?
O14 H14B 0.7637 . ?
O15 H15A 0.8117 . ?
O15 H15B 0.8633 . ?
O16 H16A 0.8237 . ?
O16 H16B 0.8458 . ?
O17 H17A 0.8644 . ?
O17 H17B 0.8151 . ?
O18 H18A 0.7703 . ?
O18 H18B 0.8046 . ?
O19 H19A 0.7866 . ?
O19 H19B 0.8541 . ?
O20 H20A 0.7685 . ?
O20 H20B 0.7823 . ?
O21 H21A 0.7865 . ?
O21 H21B 0.7530 . ?

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
O14 Mn1 N1 91.78(9) . . ?
O14 Mn1 O13 166.96(10) . . ?
N1 Mn1 O13 99.21(9) . . ?
O14 Mn1 O11 88.40(9) . 4 ?
N1 Mn1 O11 147.89(10) . 4 ?
O13 Mn1 O11 85.99(9) . 4 ?
O14 Mn1 O6 90.84(9) . . ?
N1 Mn1 O6 71.10(9) . . ?
O13 Mn1 O6 86.17(10) . . ?
O11 Mn1 O6 141.02(9) 4 . ?
O14 Mn1 O1 91.19(10) . . ?
N1 Mn1 O1 70.35(9) . . ?
O13 Mn1 O1 99.06(11) . . ?
O11 Mn1 O1 77.54(9) 4 . ?
O6 Mn1 O1 141.44(8) . . ?
O14 Mn1 O12 88.50(9) . 4 ?
N1 Mn1 O12 156.77(9) . 4 ?
O13 Mn1 O12 78.63(10) . 4 ?
O11 Mn1 O12 55.35(9) 4 4 ?
O6 Mn1 O12 85.67(9) . 4 ?
O1 Mn1 O12 132.88(9) . 4 ?
O2 Mn2 O17 79.93(10) . . ?
O2 Mn2 O15 88.31(9) . . ?
O17 Mn2 O15 167.19(10) . . ?
O2 Mn2 N2 162.92(10) . . ?
O17 Mn2 N2 98.14(10) . . ?
O15 Mn2 N2 91.60(9) . . ?
O2 Mn2 O7 94.21(10) . . ?
O17 Mn2 O7 95.05(11) . . ?
O15 Mn2 O7 80.66(9) . . ?
N2 Mn2 O7 68.96(9) . . ?
O2 Mn2 O16 77.95(11) . . ?
O17 Mn2 O16 106.23(12) . . ?
O15 Mn2 O16 75.91(10) . . ?
N2 Mn2 O16 118.56(11) . . ?
O7 Mn2 O16 155.43(10) . . ?
O2 Mn2 O12 128.31(9) . . ?
O17 Mn2 O12 77.49(10) . . ?
O15 Mn2 O12 114.22(9) . . ?
N2 Mn2 O12 66.86(9) . . ?
O7 Mn2 O12 133.44(8) . . ?
O16 Mn2 O12 65.02(10) . . ?
O3 Mn3 O19 85.81(10) . . ?
O3 Mn3 O5 164.46(8) . 4_454 ?
O19 Mn3 O5 84.30(9) . 4_454 ?
O3 Mn3 O21 97.02(10) . . ?
O19 Mn3 O21 174.15(11) . . ?
O5 Mn3 O21 93.96(9) 4_454 . ?
O3 Mn3 O20 101.22(9) . . ?
O19 Mn3 O20 90.08(12) . . ?
O5 Mn3 O20 90.76(9) 4_454 . ?
O21 Mn3 O20 84.35(10) . . ?
O3 Mn3 O18 90.68(10) . . ?
O19 Mn3 O18 100.87(11) . . ?
O5 Mn3 O18 79.48(9) 4_454 . ?
O21 Mn3 O18 84.25(10) . . ?
O20 Mn3 O18 164.43(10) . . ?
C5 N1 C1 120.0(3) . . ?
C5 N1 Mn1 119.6(2) . . ?
C1 N1 Mn1 120.3(2) . . ?
N1 C1 C2 121.8(3) . . ?
N1 C1 C6 113.3(3) . . ?
C2 C1 C6 124.8(3) . . ?
C1 C2 C3 118.9(3) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C4 C3 C2 118.6(3) . . ?
C4 C3 C7 119.4(3) . . ?
C2 C3 C7 121.9(3) . . ?
C3 C4 C5 119.0(3) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
N1 C5 C4 121.6(3) . . ?
N1 C5 C8 113.5(2) . . ?
C4 C5 C8 124.9(3) . . ?
O2 C6 O1 127.9(3) . . ?
O2 C6 C1 116.7(3) . . ?
O1 C6 C1 115.4(3) . . ?
C6 O1 Mn1 119.0(2) . . ?
C6 O2 Mn2 142.9(2) . . ?
O4 C7 O3 124.5(3) . . ?
O4 C7 C3 118.0(3) . . ?
O3 C7 C3 117.4(3) . . ?
C7 O3 Mn3 153.8(2) . . ?
O5 C8 O6 125.2(3) . . ?
O5 C8 C5 118.4(3) . . ?
O6 C8 C5 116.5(3) . . ?
C8 O5 Mn3 123.44(19) . 4 ?
C8 O6 Mn1 118.9(2) . . ?
C13 N2 C9 118.7(3) . . ?
C13 N2 Mn2 121.9(2) . . ?
C9 N2 Mn2 119.3(2) . . ?
N2 C9 C10 121.5(3) . . ?
N2 C9 C14 114.3(3) . . ?
C10 C9 C14 124.1(3) . . ?
C11 C10 C9 119.6(3) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C12 118.2(3) . . ?
C10 C11 C15 122.3(3) . . ?
C12 C11 C15 119.5(3) . . ?
C13 C12 C11 118.9(3) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
N2 C13 C12 123.1(3) . . ?
N2 C13 C16 114.2(3) . . ?
C12 C13 C16 122.7(3) . . ?
O8 C14 O7 125.7(3) . . ?
O8 C14 C9 118.7(3) . . ?
O7 C14 C9 115.7(3) . . ?
C14 O7 Mn2 120.8(2) . . ?
O9 C15 O10 124.6(3) . . ?
O9 C15 C11 118.2(3) . . ?
O10 C15 C11 117.2(3) . . ?
O12 C16 O11 123.0(3) . . ?
O12 C16 C13 117.8(3) . . ?
O11 C16 C13 119.2(3) . . ?
C16 O11 Mn1 95.9(2) . 4_454 ?
C16 O12 Mn1 85.6(2) . 4_454 ?
C16 O12 Mn2 117.1(2) . . ?
Mn1 O12 Mn2 155.26(12) 4_454 . ?
Mn1 O13 H13A 121.5 . . ?
Mn1 O13 H13B 118.6 . . ?
H13A O13 H13B 114.3 . . ?
Mn1 O14 H14A 115.7 . . ?
Mn1 O14 H14B 120.1 . . ?
H14A O14 H14B 95.8 . . ?
Mn2 O15 H15A 124.6 . . ?
Mn2 O15 H15B 119.0 . . ?
H15A O15 H15B 114.7 . . ?
Mn2 O16 H16A 98.6 . . ?
Mn2 O16 H16B 126.6 . . ?
H16A O16 H16B 104.1 . . ?
Mn2 O17 H17A 120.0 . . ?
Mn2 O17 H17B 141.1 . . ?
H17A O17 H17B 98.9 . . ?
Mn3 O18 H18A 139.0 . . ?
Mn3 O18 H18B 104.6 . . ?
H18A O18 H18B 109.5 . . ?
Mn3 O19 H19A 128.8 . . ?
Mn3 O19 H19B 127.1 . . ?
H19A O19 H19B 103.8 . . ?
Mn3 O20 H20A 114.8 . . ?
Mn3 O20 H20B 131.8 . . ?
H20A O20 H20B 107.9 . . ?
Mn3 O21 H21A 129.9 . . ?
Mn3 O21 H21B 96.9 . . ?
H21A O21 H21B 98.1 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.43
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.095

# Attachment '2.cif'

data_shx97_2
_database_code_depnum_ccdc_archive 'CCDC 740624'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H16 Co6 N4 O28'
_chemical_formula_sum            'C16 H8 Co3 N2 O14'
_chemical_formula_weight         629.03

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P b c n'
_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                   15.9192(6)
_cell_length_b                   5.9225(3)
_cell_length_c                   18.5992(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1753.56(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    12634
_cell_measurement_theta_min      3.2
_cell_measurement_theta_max      27.5

_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1244
_exptl_absorpt_coefficient_mu    2.900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.417
_exptl_absorpt_correction_T_max  0.503
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(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  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         0
_diffrn_standards_interval_count imagen
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            9413
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         28.05
_reflns_number_total             2109
_reflns_number_gt                1466
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        RAPID-AUTO
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    XP
_computing_publication_material  SHELXL-97

_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^)+(0.0273P)^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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2109
_refine_ls_number_parameters     159
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0259
_refine_ls_wR_factor_ref         0.0589
_refine_ls_wR_factor_gt          0.0573
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_restrained_S_all      0.886
_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
Co1 Co 0.0000 0.40570(8) 0.7500 0.01510(12) Uani 1 2 d S . .
Co2 Co -0.175677(18) 1.08603(6) 0.852580(16) 0.01611(10) Uani 1 1 d . . .
N N 0.05509(11) 0.4366(3) 0.84715(10) 0.0164(5) Uani 1 1 d . . .
C1 C 0.11886(13) 0.3012(4) 0.86593(11) 0.0153(5) Uani 1 1 d . . .
C2 C 0.15946(13) 0.3265(5) 0.93093(11) 0.0187(6) Uani 1 1 d . . .
H2 H 0.2025 0.2287 0.9441 0.022 Uiso 1 1 calc R . .
C3 C 0.13499(14) 0.5003(4) 0.97647(11) 0.0166(5) Uani 1 1 d . . .
C4 C 0.07016(13) 0.6451(4) 0.95538(12) 0.0183(6) Uani 1 1 d . . .
H4 H 0.0535 0.7642 0.9847 0.022 Uiso 1 1 calc R . .
C5 C 0.03126(13) 0.6074(4) 0.88994(12) 0.0170(5) Uani 1 1 d . . .
C6 C 0.14344(14) 0.1385(4) 0.80756(12) 0.0192(6) Uani 1 1 d . . .
O1 O 0.10719(9) 0.1700(3) 0.74570(8) 0.0195(4) Uani 1 1 d . . .
O2 O 0.19824(11) -0.0034(3) 0.82043(9) 0.0289(4) Uani 1 1 d . . .
C7 C 0.17690(14) 0.5358(4) 1.04833(12) 0.0165(5) Uani 1 1 d . . .
O3 O 0.24979(10) 0.4604(3) 1.05657(8) 0.0214(4) Uani 1 1 d . . .
O4 O 0.13387(9) 0.6402(3) 1.09435(8) 0.0207(4) Uani 1 1 d . . .
C8 C -0.04206(13) 0.7379(5) 0.85928(12) 0.0174(5) Uani 1 1 d . . .
O5 O -0.07287(10) 0.8982(3) 0.89413(8) 0.0226(4) Uani 1 1 d . . .
O6 O -0.06826(9) 0.6678(3) 0.79900(8) 0.0202(4) Uani 1 1 d . . .
O7 O -0.22407(9) 0.7841(3) 0.80255(8) 0.0186(4) Uani 1 1 d . . .
H7A H -0.2227 0.8179 0.7611 0.022 Uiso 1 1 d . . .
H7B H -0.1822 0.7026 0.7997 0.022 Uiso 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
Co1 0.0128(2) 0.0199(3) 0.0126(2) 0.000 -0.00202(17) 0.000
Co2 0.01420(15) 0.0179(2) 0.01626(17) 0.00010(14) -0.00019(12) -0.00024(14)
N 0.0151(9) 0.0181(14) 0.0160(10) -0.0011(9) -0.0007(7) 0.0036(8)
C1 0.0150(10) 0.0151(15) 0.0157(12) 0.0011(10) 0.0001(9) 0.0017(10)
C2 0.0177(11) 0.0205(16) 0.0180(12) 0.0014(10) -0.0037(9) 0.0056(10)
C3 0.0158(11) 0.0189(15) 0.0151(11) -0.0003(10) -0.0001(9) -0.0012(10)
C4 0.0167(10) 0.0202(16) 0.0179(12) -0.0030(11) 0.0017(10) 0.0027(10)
C5 0.0157(11) 0.0197(16) 0.0157(12) 0.0029(11) 0.0009(9) 0.0010(10)
C6 0.0176(11) 0.0221(17) 0.0180(12) 0.0000(11) -0.0012(10) -0.0015(11)
O1 0.0180(8) 0.0253(11) 0.0152(8) -0.0019(8) -0.0023(7) 0.0055(7)
O2 0.0342(10) 0.0313(12) 0.0213(9) -0.0049(9) -0.0062(8) 0.0181(9)
C7 0.0202(11) 0.0147(15) 0.0147(11) 0.0015(10) -0.0014(10) -0.0028(10)
O3 0.0204(8) 0.0233(12) 0.0203(9) -0.0013(8) -0.0064(8) 0.0047(8)
O4 0.0192(8) 0.0262(12) 0.0167(8) -0.0049(8) 0.0015(7) -0.0030(7)
C8 0.0154(11) 0.0177(16) 0.0190(12) 0.0039(12) 0.0031(9) 0.0008(10)
O5 0.0221(8) 0.0228(12) 0.0228(9) -0.0030(8) -0.0040(7) 0.0088(8)
O6 0.0173(8) 0.0277(12) 0.0157(8) -0.0032(7) -0.0031(7) 0.0071(7)
O7 0.0154(8) 0.0231(12) 0.0174(8) 0.0001(8) 0.0014(6) 0.0000(7)

_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
Co1 N 2.0168(18) 3_556 ?
Co1 N 2.0168(18) . ?
Co1 O6 2.1027(17) 3_556 ?
Co1 O6 2.1027(17) . ?
Co1 O1 2.2059(16) 3_556 ?
Co1 O1 2.2059(16) . ?
Co2 O4 2.0117(17) 5_577 ?
Co2 O3 2.0830(15) 4_467 ?
Co2 O5 2.1243(16) . ?
Co2 O7 2.1581(18) . ?
Co2 O1 2.1857(15) 3_566 ?
Co2 O7 2.1883(16) 8_565 ?
N C1 1.340(3) . ?
N C5 1.342(3) . ?
C1 C2 1.379(3) . ?
C1 C6 1.504(3) . ?
C2 C3 1.389(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.398(3) . ?
C3 C7 1.509(3) . ?
C4 C5 1.384(3) . ?
C4 H4 0.9300 . ?
C5 C8 1.512(3) . ?
C6 O2 1.235(3) . ?
C6 O1 1.301(3) . ?
O1 Co2 2.1857(15) 3_546 ?
C7 O3 1.253(3) . ?
C7 O4 1.258(3) . ?
O3 Co2 2.0830(15) 4_567 ?
O4 Co2 2.0117(17) 5_577 ?
C8 O5 1.250(3) . ?
C8 O6 1.266(3) . ?
O7 Co2 2.1883(15) 8 ?
O7 H7A 0.7973 . ?
O7 H7B 0.8251 . ?

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
N Co1 N 169.59(12) 3_556 . ?
N Co1 O6 76.67(7) 3_556 3_556 ?
N Co1 O6 95.54(7) . 3_556 ?
N Co1 O6 95.54(7) 3_556 . ?
N Co1 O6 76.67(7) . . ?
O6 Co1 O6 84.82(10) 3_556 . ?
N Co1 O1 75.73(7) 3_556 3_556 ?
N Co1 O1 111.18(7) . 3_556 ?
O6 Co1 O1 151.96(6) 3_556 3_556 ?
O6 Co1 O1 92.96(6) . 3_556 ?
N Co1 O1 111.18(7) 3_556 . ?
N Co1 O1 75.73(7) . . ?
O6 Co1 O1 92.96(6) 3_556 . ?
O6 Co1 O1 151.96(6) . . ?
O1 Co1 O1 101.50(9) 3_556 . ?
O4 Co2 O3 84.09(6) 5_577 4_467 ?
O4 Co2 O5 89.35(7) 5_577 . ?
O3 Co2 O5 94.28(6) 4_467 . ?
O4 Co2 O7 176.06(6) 5_577 . ?
O3 Co2 O7 92.12(6) 4_467 . ?
O5 Co2 O7 89.89(6) . . ?
O4 Co2 O1 93.54(6) 5_577 3_566 ?
O3 Co2 O1 173.03(7) 4_467 3_566 ?
O5 Co2 O1 92.24(6) . 3_566 ?
O7 Co2 O1 90.35(6) . 3_566 ?
O4 Co2 O7 91.02(7) 5_577 8_565 ?
O3 Co2 O7 90.02(6) 4_467 8_565 ?
O5 Co2 O7 175.70(6) . 8_565 ?
O7 Co2 O7 90.03(4) . 8_565 ?
O1 Co2 O7 83.46(6) 3_566 8_565 ?
C1 N C5 120.71(19) . . ?
C1 N Co1 120.58(16) . . ?
C5 N Co1 118.48(15) . . ?
N C1 C2 121.3(2) . . ?
N C1 C6 113.11(19) . . ?
C2 C1 C6 125.5(2) . . ?
C1 C2 C3 118.9(2) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C2 C3 C4 119.4(2) . . ?
C2 C3 C7 121.3(2) . . ?
C4 C3 C7 119.3(2) . . ?
C5 C4 C3 118.6(2) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
N C5 C4 121.1(2) . . ?
N C5 C8 112.33(19) . . ?
C4 C5 C8 126.5(2) . . ?
O2 C6 O1 125.6(2) . . ?
O2 C6 C1 118.7(2) . . ?
O1 C6 C1 115.5(2) . . ?
C6 O1 Co2 119.06(14) . 3_546 ?
C6 O1 Co1 113.71(14) . . ?
Co2 O1 Co1 124.07(7) 3_546 . ?
O3 C7 O4 126.6(2) . . ?
O3 C7 C3 117.9(2) . . ?
O4 C7 C3 115.5(2) . . ?
C7 O3 Co2 132.37(15) . 4_567 ?
C7 O4 Co2 123.32(15) . 5_577 ?
O5 C8 O6 125.4(2) . . ?
O5 C8 C5 119.7(2) . . ?
O6 C8 C5 114.9(2) . . ?
C8 O5 Co2 120.75(14) . . ?
C8 O6 Co1 117.10(14) . . ?
Co2 O7 Co2 121.41(7) . 8 ?
Co2 O7 H7A 101.5 . . ?
Co2 O7 H7A 124.4 8 . ?
Co2 O7 H7B 102.9 . . ?
Co2 O7 H7B 107.6 8 . ?
H7A O7 H7B 93.7 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        28.05
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.091

# Attachment '3.cif'

data_shx97_3
_database_code_depnum_ccdc_archive 'CCDC 740625'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C8 H4 Co N O7), C10 H16 Co N2 O4'
_chemical_formula_sum            'C26 H24 Co3 N4 O18'
_chemical_formula_weight         857.28

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'
Co Co 0.3494 0.9721 '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                   8.0920(16)
_cell_length_b                   8.9980(18)
_cell_length_c                   10.884(2)
_cell_angle_alpha                81.53(3)
_cell_angle_beta                 71.23(3)
_cell_angle_gamma                82.80(3)
_cell_volume                     739.6(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    15368
_cell_measurement_theta_min      3.2
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             433
_exptl_absorpt_coefficient_mu    1.759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.592
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(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  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         0
_diffrn_standards_interval_count image
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            4118
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3396
_reflns_number_gt                2943
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        RAPID-AUTO
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    XP
_computing_publication_material  SHELXL-97

_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^)+(0.0782P)^2^+0.3339P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3396
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.1224
_refine_ls_wR_factor_gt          0.1120
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_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
Co1 Co 0.87098(5) 0.90174(4) 0.95017(3) 0.01799(13) Uani 1 1 d . . .
Co2 Co 0.5000 0.0000 0.5000 0.01609(15) Uani 1 2 d S . .
N1 N 0.8321(3) 0.6801(2) 0.9544(2) 0.0166(4) Uani 1 1 d . . .
C1 C 0.9387(3) 0.6001(3) 0.8617(2) 0.0160(5) Uani 1 1 d . . .
C2 C 0.92617(16) 0.44702(12) 0.86631(11) 0.0182(5) Uani 1 1 d . . .
H2A H 1.0038 0.3910 0.8033 0.022 Uiso 1 1 calc R . .
C3 C 0.79433(16) 0.37962(12) 0.96779(11) 0.0168(5) Uani 1 1 d R . .
C4 C 0.67931(16) 0.46626(12) 1.06073(11) 0.0184(5) Uani 1 1 d R . .
H4A H 0.5868 0.4239 1.1266 0.022 Uiso 1 1 calc R . .
C5 C 0.70585(16) 0.61651(12) 1.05278(11) 0.0179(5) Uani 1 1 d R . .
C6 C 1.07679(16) 0.69325(12) 0.76254(11) 0.0179(5) Uani 1 1 d R . .
O1 O 1.0730(3) 0.8279(2) 0.7887(2) 0.0230(4) Uani 1 1 d . . .
O2 O 1.1815(2) 0.63597(18) 0.66923(16) 0.0301(5) Uani 1 1 d . . .
C7 C 0.7694(2) 0.21344(18) 0.98083(16) 0.0180(5) Uani 1 1 d R . .
O3 O 0.9091(3) 0.1220(2) 0.9514(2) 0.0214(4) Uani 1 1 d . . .
O4 O 0.6197(2) 0.17689(18) 1.01790(18) 0.0316(5) Uani 1 1 d . . .
C8 C 0.6113(2) 0.72438(18) 1.15268(18) 0.0218(6) Uani 1 1 d R . .
O5 O 0.4859(4) 0.6859(3) 1.2453(2) 0.0422(7) Uani 1 1 d . . .
O6 O 0.6778(3) 0.8502(2) 1.1310(2) 0.0270(5) Uani 1 1 d . . .
N2 N 0.30388(16) 0.17878(13) 0.49025(12) 0.0246(5) Uani 1 1 d . . .
C9 C 0.35175(16) 0.31157(13) 0.42242(12) 0.0327(7) Uani 1 1 d R . .
H9A H 0.4684 0.3182 0.3723 0.039 Uiso 1 1 calc R . .
C10 C 0.23756(16) 0.43907(13) 0.42277(12) 0.0309(7) Uani 1 1 d R . .
H10A H 0.2771 0.5287 0.3738 0.037 Uiso 1 1 calc R . .
C11 C 0.06260(16) 0.43208(13) 0.49726(12) 0.0201(5) Uani 1 1 d R . .
C12 C 0.01225(16) 0.29352(13) 0.56523(12) 0.0261(6) Uani 1 1 d R . .
H12A H -0.1039 0.2829 0.6149 0.031 Uiso 1 1 calc R . .
C13 C 0.13587(16) 0.17126(13) 0.55866(12) 0.0285(7) Uani 1 1 d R . .
H13A H 0.0994 0.0793 0.6044 0.034 Uiso 1 1 calc R . .
O7 O 0.6980(3) 0.9567(3) 0.8328(2) 0.0339(5) Uani 1 1 d . . .
H7A H 0.5975 0.9321 0.8807 0.041 Uiso 1 1 d . . .
H7B H 0.7491 1.0173 0.8602 0.041 Uiso 1 1 d . . .
O8 O 0.3811(3) -0.0498(2) 0.69754(19) 0.0237(4) Uani 1 1 d . . .
H8A H 0.3671 0.0197 0.7459 0.028 Uiso 1 1 d . . .
H8B H 0.2919 -0.0997 0.7215 0.028 Uiso 1 1 d . . .
O9 O 0.3485(3) -0.1562(2) 0.4620(2) 0.0273(5) Uani 1 1 d . . .
H9C H 0.3815 -0.2041 0.3955 0.033 Uiso 1 1 d . . .
H9B H 0.2888 -0.2169 0.5229 0.033 Uiso 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
Co1 0.0191(2) 0.00850(19) 0.0240(2) -0.00333(13) -0.00295(15) -0.00056(13)
Co2 0.0138(3) 0.0117(2) 0.0199(3) -0.00140(17) -0.00324(19) 0.00385(18)
N1 0.0172(11) 0.0094(9) 0.0217(11) -0.0017(8) -0.0047(9) 0.0011(8)
C1 0.0165(12) 0.0126(11) 0.0186(11) -0.0020(9) -0.0055(10) 0.0009(9)
C2 0.0205(13) 0.0115(11) 0.0219(12) -0.0043(9) -0.0065(10) 0.0035(9)
C3 0.0190(12) 0.0082(11) 0.0244(12) -0.0008(9) -0.0096(10) 0.0013(9)
C4 0.0175(12) 0.0126(11) 0.0222(12) -0.0003(9) -0.0034(10) -0.0005(9)
C5 0.0164(12) 0.0131(12) 0.0223(12) -0.0025(9) -0.0043(10) 0.0022(9)
C6 0.0172(12) 0.0141(12) 0.0212(12) 0.0002(9) -0.0054(10) -0.0011(9)
O1 0.0211(10) 0.0139(9) 0.0291(10) -0.0041(7) 0.0005(8) -0.0037(7)
O2 0.0313(12) 0.0230(10) 0.0276(10) -0.0078(8) 0.0056(9) -0.0047(9)
C7 0.0219(13) 0.0088(11) 0.0232(12) -0.0003(9) -0.0089(10) 0.0019(9)
O3 0.0214(10) 0.0092(8) 0.0343(11) -0.0044(7) -0.0105(8) 0.0032(7)
O4 0.0234(11) 0.0155(10) 0.0542(14) -0.0052(9) -0.0089(10) -0.0027(8)
C8 0.0239(14) 0.0143(12) 0.0239(13) -0.0032(10) -0.0026(11) -0.0011(10)
O5 0.0449(15) 0.0303(12) 0.0356(12) -0.0135(10) 0.0183(11) -0.0161(11)
O6 0.0312(11) 0.0147(9) 0.0292(10) -0.0080(8) 0.0023(9) -0.0046(8)
N2 0.0190(12) 0.0152(11) 0.0346(13) -0.0009(9) -0.0058(10) 0.0083(9)
C9 0.0189(14) 0.0220(14) 0.0426(17) 0.0051(12) 0.0033(13) 0.0081(12)
C10 0.0221(15) 0.0180(13) 0.0426(17) 0.0053(12) -0.0026(13) 0.0059(11)
C11 0.0196(13) 0.0144(12) 0.0264(13) -0.0008(10) -0.0100(11) 0.0043(10)
C12 0.0152(13) 0.0191(13) 0.0398(16) 0.0029(11) -0.0079(12) 0.0047(10)
C13 0.0202(14) 0.0162(13) 0.0451(17) 0.0044(12) -0.0094(13) 0.0023(11)
O7 0.0263(12) 0.0328(12) 0.0447(13) -0.0054(10) -0.0147(10) 0.0011(9)
O8 0.0226(10) 0.0221(10) 0.0225(9) -0.0060(7) 0.0006(8) -0.0042(8)
O9 0.0279(11) 0.0236(10) 0.0280(10) -0.0061(8) -0.0024(9) -0.0058(8)

_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
Co1 O3 2.0461(19) 1_565 ?
Co1 N1 2.049(2) . ?
Co1 O1 2.104(2) . ?
Co1 O6 2.113(2) . ?
Co1 O7 2.151(2) . ?
Co1 O3 2.329(2) 2_767 ?
Co1 H7B 1.7544 . ?
Co2 O8 2.060(2) 2_656 ?
Co2 O8 2.060(2) . ?
Co2 N2 2.1298(13) . ?
Co2 N2 2.1298(13) 2_656 ?
Co2 O9 2.140(2) 2_656 ?
Co2 O9 2.140(2) . ?
N1 C1 1.333(3) . ?
N1 C5 1.33405 . ?
C1 C2 1.386(3) . ?
C1 C6 1.51926 . ?
C2 C3 1.3901 . ?
C2 H2A 0.9300 . ?
C3 C4 1.3936 . ?
C3 C7 1.51374 . ?
C4 C5 1.3812 . ?
C4 H4A 0.9300 . ?
C5 C8 1.51628 . ?
C6 O2 1.22717 . ?
C6 O1 1.27931 . ?
C7 O4 1.21845 . ?
C7 O3 1.29188 . ?
O3 Co1 2.0461(19) 1_545 ?
O3 Co1 2.329(2) 2_767 ?
C8 O5 1.22178 . ?
C8 O6 1.27250 . ?
N2 C13 1.3282 . ?
N2 C9 1.3397 . ?
C9 C10 1.3796 . ?
C9 H9A 0.9300 . ?
C10 C11 1.3908 . ?
C10 H10A 0.9300 . ?
C11 C12 1.3890 . ?
C11 C11 1.48194 2_566 ?
C12 C13 1.3847 . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
O7 H7A 0.8489 . ?
O7 H7B 0.8604 . ?
O8 H8A 0.8499 . ?
O8 H8B 0.8461 . ?
O9 H9C 0.8485 . ?
O9 H9B 0.8507 . ?

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
O3 Co1 N1 178.42(8) 1_565 . ?
O3 Co1 O1 105.32(9) 1_565 . ?
N1 Co1 O1 75.74(9) . . ?
O3 Co1 O6 103.64(8) 1_565 . ?
N1 Co1 O6 75.12(9) . . ?
O1 Co1 O6 149.36(8) . . ?
O3 Co1 O7 93.93(9) 1_565 . ?
N1 Co1 O7 87.22(10) . . ?
O1 Co1 O7 90.47(9) . . ?
O6 Co1 O7 97.38(10) . . ?
O3 Co1 O3 77.89(8) 1_565 2_767 ?
N1 Co1 O3 101.12(8) . 2_767 ?
O1 Co1 O3 84.35(8) . 2_767 ?
O6 Co1 O3 92.13(9) . 2_767 ?
O7 Co1 O3 168.73(8) . 2_767 ?
O3 Co1 H7B 71.3 1_565 . ?
N1 Co1 H7B 109.9 . . ?
O1 Co1 H7B 96.5 . . ?
O6 Co1 H7B 102.1 . . ?
O7 Co1 H7B 22.7 . . ?
O3 Co1 H7B 148.2 2_767 . ?
O8 Co2 O8 180.0 2_656 . ?
O8 Co2 N2 89.01(8) 2_656 . ?
O8 Co2 N2 90.99(8) . . ?
O8 Co2 N2 90.99(8) 2_656 2_656 ?
O8 Co2 N2 89.01(8) . 2_656 ?
N2 Co2 N2 180.0 . 2_656 ?
O8 Co2 O9 89.72(8) 2_656 2_656 ?
O8 Co2 O9 90.28(8) . 2_656 ?
N2 Co2 O9 89.22(7) . 2_656 ?
N2 Co2 O9 90.78(7) 2_656 2_656 ?
O8 Co2 O9 90.28(8) 2_656 . ?
O8 Co2 O9 89.72(8) . . ?
N2 Co2 O9 90.78(7) . . ?
N2 Co2 O9 89.22(7) 2_656 . ?
O9 Co2 O9 180.00(7) 2_656 . ?
C1 N1 C5 121.10 . . ?
C1 N1 Co1 119.30(17) . . ?
C5 N1 Co1 119.54 . . ?
N1 C1 C2 121.3(2) . . ?
N1 C1 C6 112.24 . . ?
C2 C1 C6 126.31 . . ?
C1 C2 C3 118.15 . . ?
C1 C2 H2A 120.9 . . ?
C3 C2 H2A 120.9 . . ?
C2 C3 C4 119.8 . . ?
C2 C3 C7 122.08 . . ?
C4 C3 C7 118.12 . . ?
C5 C4 C3 118.5 . . ?
C5 C4 H4A 120.8 . . ?
C3 C4 H4A 120.8 . . ?
N1 C5 C4 121.08 . . ?
N1 C5 C8 112.12 . . ?
C4 C5 C8 126.68 . . ?
O2 C6 O1 126.06 . . ?
O2 C6 C1 119.74 . . ?
O1 C6 C1 114.18 . . ?
C6 O1 Co1 118.38 . . ?
O4 C7 O3 125.38 . . ?
O4 C7 C3 117.49 . . ?
O3 C7 C3 117.12 . . ?
C7 O3 Co1 116.02(15) . 1_545 ?
C7 O3 Co1 124.76(15) . 2_767 ?
Co1 O3 Co1 102.11(8) 1_545 2_767 ?
O5 C8 O6 125.89 . . ?
O5 C8 C5 120.19 . . ?
O6 C8 C5 113.89 . . ?
C8 O6 Co1 118.42 . . ?
C13 N2 C9 117.1 . . ?
C13 N2 Co2 123.29 . . ?
C9 N2 Co2 119.30 . . ?
N2 C9 C10 123.6 . . ?
N2 C9 H9A 118.2 . . ?
C10 C9 H9A 118.2 . . ?
C9 C10 C11 119.2 . . ?
C9 C10 H10A 120.4 . . ?
C11 C10 H10A 120.4 . . ?
C12 C11 C10 117.1 . . ?
C12 C11 C11 122.23(9) . 2_566 ?
C10 C11 C11 120.66(10) . 2_566 ?
C13 C12 C11 119.7 . . ?
C13 C12 H12A 120.2 . . ?
C11 C12 H12A 120.2 . . ?
N2 C13 C12 123.3 . . ?
N2 C13 H13A 118.4 . . ?
C12 C13 H13A 118.4 . . ?
Co1 O7 H7A 106.9 . . ?
Co1 O7 H7B 51.8 . . ?
H7A O7 H7B 118.2 . . ?
Co2 O8 H8A 117.7 . . ?
Co2 O8 H8B 117.7 . . ?
H8A O8 H8B 110.7 . . ?
Co2 O9 H9C 124.3 . . ?
Co2 O9 H9B 121.6 . . ?
H9C O9 H9B 104.4 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.831
_refine_diff_density_min         -1.306
_refine_diff_density_rms         0.163