# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Wen Dong'
_publ_contact_author_email       DW320@YAHOO.COM.CN

_publ_section_title              
;
Syntheses, Structures and Properties of Seven H2BTA
Coordinating 3d Metallic Complexes Containing Zero-, One-, Two-, and
Three-Dimensional Frameworks (H2BTA = Bis(tetrazoly)amine )
;
loop_
_publ_author_name
'Wen Dong'
'Yang-Fan Guan'
'Bei-Shu Huang'
'Jiao-Min Lin'
;
Zhao-Qing Liu
;
'Dong-Yao Wang'

data_mn2
_database_code_depnum_ccdc_archive 'CCDC 659743'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C2 H7 Mn N9 O3), H2 O'
_chemical_formula_sum            'C4 H16 Mn2 N18 O7'
_chemical_formula_weight         538.23

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           orthorhombic
_symmetry_space_group_name_H-M   P21212

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

_cell_length_a                   23.9993(19)
_cell_length_b                   10.2755(8)
_cell_length_c                   7.4265(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1831.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2453
_cell_measurement_theta_min      1.70
_cell_measurement_theta_max      27.580

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.113
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.952
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1088
_exptl_absorpt_coefficient_mu    1.458
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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  'Bruker APEX-II area-detector diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            28926
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         27.58
_reflns_number_total             4245
_reflns_number_gt                4141
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2004)'
_computing_cell_refinement       'SMART (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2002)'
_computing_publication_material  SHELXL-97

_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)+(0.0415P)²+0.4997P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_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   0.035(11)
_refine_ls_number_reflns         4245
_refine_ls_number_parameters     345
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0211
_refine_ls_wR_factor_ref         0.0605
_refine_ls_wR_factor_gt          0.0601
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.002
_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 0.162849(10) 1.00311(2) 0.02610(4) 0.01666(7) Uani 1 1 d . . .
Mn2 Mn 0.063794(10) 0.36427(2) 0.52345(4) 0.01951(7) Uani 1 1 d . . .
N1 N 0.11741(6) 0.81589(14) 0.0653(2) 0.0206(3) Uani 1 1 d . . .
N2 N 0.06243(7) 0.80545(16) 0.1040(3) 0.0260(3) Uani 1 1 d . . .
N3 N 0.04781(7) 0.68485(16) 0.0901(3) 0.0293(4) Uani 1 1 d . . .
N4 N 0.09192(6) 0.60958(14) 0.0444(3) 0.0278(4) Uani 1 1 d . . .
N5 N 0.18684(6) 0.65619(14) -0.0101(3) 0.0286(4) Uani 1 1 d . . .
N6 N 0.28443(6) 0.68321(13) 0.0254(3) 0.0221(3) Uani 1 1 d . . .
N7 N 0.31713(6) 0.78887(14) 0.0518(3) 0.0313(4) Uani 1 1 d . . .
N8 N 0.28650(6) 0.89235(15) 0.0589(3) 0.0304(4) Uani 1 1 d . . .
N9 N 0.23245(6) 0.86017(13) 0.0347(2) 0.0228(3) Uani 1 1 d . . .
N10 N -0.15426(6) 0.61003(14) 0.4721(3) 0.0236(3) Uani 1 1 d . . .
N11 N -0.18903(6) 0.71164(16) 0.4412(3) 0.0300(4) Uani 1 1 d . . .
N12 N -0.23983(6) 0.67104(16) 0.4380(3) 0.0313(4) Uani 1 1 d . . .
N13 N -0.24107(6) 0.54077(15) 0.4654(3) 0.0290(4) Uani 1 1 d . . .
N14 N -0.17074(6) 0.38285(15) 0.5173(3) 0.0290(4) Uani 1 1 d . . .
N15 N -0.10427(6) 0.22379(15) 0.5991(3) 0.0237(3) Uani 1 1 d . . .
N16 N -0.04846(6) 0.22175(16) 0.6095(2) 0.0246(3) Uani 1 1 d . . .
N17 N -0.02874(6) 0.33549(14) 0.5669(2) 0.0216(3) Uani 1 1 d . . .
N18 N -0.07121(6) 0.41738(13) 0.5254(2) 0.0196(3) Uani 1 1 d . . .
O1 O 0.05423(6) 0.36132(17) 0.2294(2) 0.0295(3) Uani 1 1 d . . .
H3 H 0.0228(11) 0.360(3) 0.177(4) 0.037(7) Uiso 1 1 d . . .
H4 H 0.070(2) 0.441(5) 0.190(7) 0.116(18) Uiso 1 1 d . . .
O2 O 0.07797(7) 0.37339(17) 0.8142(2) 0.0334(3) Uani 1 1 d . . .
H5 H 0.0786(18) 0.461(5) 0.859(6) 0.100(15) Uiso 1 1 d . . .
O3 O 0.07291(6) 0.15482(13) 0.5296(3) 0.0327(3) Uani 1 1 d . . .
H7 H 0.0966(12) 0.113(3) 0.592(4) 0.043(8) Uiso 1 1 d . . .
H8 H 0.0536(11) 0.111(3) 0.472(4) 0.036(7) Uiso 1 1 d . . .
O4 O 0.17026(7) 1.04096(16) 0.3083(2) 0.0293(3) Uani 1 1 d . . .
H10 H 0.1697(12) 1.114(3) 0.340(4) 0.046(8) Uiso 1 1 d . . .
O5 O 0.15417(6) 0.99550(15) -0.27095(18) 0.0235(3) Uani 1 1 d . . .
H11 H 0.1863(13) 1.006(3) -0.311(4) 0.046(8) Uiso 1 1 d . . .
H12 H 0.1437(13) 0.928(3) -0.320(5) 0.056(9) Uiso 1 1 d . . .
O6 O 0.08380(6) 1.10697(15) 0.0273(3) 0.0313(3) Uani 1 1 d . . .
H13 H 0.0759(14) 1.169(4) 0.072(5) 0.063(11) Uiso 1 1 d . . .
H14 H 0.0589(12) 1.071(3) -0.025(4) 0.045(8) Uiso 1 1 d . . .
O7 O 0.0000 0.0000 0.8174(3) 0.0297(4) Uani 1 2 d S . .
H15 H -0.0126(12) 0.049(3) 0.751(4) 0.036(8) Uiso 1 1 d . . .
H16 H 0.0139(11) -0.048(3) 0.272(4) 0.029(7) Uiso 1 1 d . . .
O8 O 0.0000 0.0000 0.3269(3) 0.0331(5) Uani 1 2 d S . .
C1 C 0.13369(7) 0.69428(15) 0.0320(3) 0.0197(3) Uani 1 1 d . . .
C2 C 0.23280(7) 0.73142(15) 0.0170(3) 0.0185(3) Uani 1 1 d . . .
C3 C -0.18775(7) 0.50784(17) 0.4852(2) 0.0205(3) Uani 1 1 d . . .
C4 C -0.11671(7) 0.34509(16) 0.5461(3) 0.0187(3) Uani 1 1 d . . .
H1 H 0.1901(10) 0.577(3) -0.026(4) 0.037(7) Uiso 1 1 d . . .
H2 H -0.1904(10) 0.340(2) 0.529(3) 0.022(6) Uiso 1 1 d . . .
H9 H 0.1952(13) 1.009(4) 0.349(4) 0.049(9) Uiso 1 1 d . . .
H6 H 0.1111(19) 0.352(5) 0.862(7) 0.110(16) Uiso 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
Mn1 O4 2.1387(16) . ?
Mn1 O6 2.1767(14) . ?
Mn1 O5 2.2172(14) . ?
Mn1 N9 2.2251(14) . ?
Mn1 N1 2.2304(14) . ?
Mn1 N6 2.2743(14) 4 ?
Mn2 O3 2.1637(14) . ?
Mn2 O2 2.1881(16) . ?
Mn2 O1 2.1957(15) . ?
Mn2 N10 2.2202(14) 2_565 ?
Mn2 N18 2.2508(14) 2_565 ?
Mn2 N17 2.2634(15) . ?
N1 C1 1.332(2) . ?
N1 N2 1.355(2) . ?
N2 N3 1.292(2) . ?
N3 N4 1.354(2) . ?
N4 C1 1.331(2) . ?
N5 C2 1.362(2) . ?
N5 C1 1.370(2) . ?
N5 H1 0.82(3) . ?
N6 C2 1.336(2) . ?
N6 N7 1.354(2) . ?
N6 Mn1 2.2743(14) 4_545 ?
N7 N8 1.294(2) . ?
N8 N9 1.351(2) . ?
N9 C2 1.330(2) . ?
N10 C3 1.326(2) . ?
N10 N11 1.356(2) . ?
N10 Mn2 2.2202(14) 2_565 ?
N11 N12 1.289(2) . ?
N12 N13 1.354(2) . ?
N13 C3 1.332(2) . ?
N14 C3 1.369(2) . ?
N14 C4 1.370(2) . ?
N14 H2 0.65(2) . ?
N15 C4 1.341(2) . ?
N15 N16 1.342(2) . ?
N16 N17 1.300(2) . ?
N17 N18 1.3572(19) . ?
N18 C4 1.329(2) . ?
N18 Mn2 2.2508(14) 2_565 ?
O1 H3 0.85(3) . ?
O1 H4 0.94(5) . ?
O2 H5 0.96(5) . ?
O2 H6 0.90(5) . ?
O3 H7 0.85(3) . ?
O3 H8 0.77(3) . ?
O4 H10 0.79(3) . ?
O4 H9 0.75(3) . ?
O5 H11 0.83(3) . ?
O5 H12 0.82(4) . ?
O6 H13 0.75(4) . ?
O6 H14 0.80(3) . ?
O7 H15 0.77(3) . ?
O8 H16 0.72(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Mn1 O6 88.82(7) . . ?
O4 Mn1 O5 171.52(6) . . ?
O6 Mn1 O5 86.53(6) . . ?
O4 Mn1 N9 91.69(7) . . ?
O6 Mn1 N9 167.89(6) . . ?
O5 Mn1 N9 94.35(6) . . ?
O4 Mn1 N1 93.99(6) . . ?
O6 Mn1 N1 89.79(5) . . ?
O5 Mn1 N1 93.07(6) . . ?
N9 Mn1 N1 78.11(5) . . ?
O4 Mn1 N6 88.32(7) . 4 ?
O6 Mn1 N6 94.96(6) . 4 ?
O5 Mn1 N6 85.04(6) . 4 ?
N9 Mn1 N6 97.14(5) . 4 ?
N1 Mn1 N6 174.76(5) . 4 ?
O3 Mn2 O2 90.35(7) . . ?
O3 Mn2 O1 91.02(7) . . ?
O2 Mn2 O1 176.61(7) . . ?
O3 Mn2 N10 91.32(5) . 2_565 ?
O2 Mn2 N10 90.71(7) . 2_565 ?
O1 Mn2 N10 86.16(6) . 2_565 ?
O3 Mn2 N18 169.54(5) . 2_565 ?
O2 Mn2 N18 86.49(7) . 2_565 ?
O1 Mn2 N18 91.62(6) . 2_565 ?
N10 Mn2 N18 78.77(5) 2_565 2_565 ?
O3 Mn2 N17 88.07(5) . . ?
O2 Mn2 N17 91.01(6) . . ?
O1 Mn2 N17 92.13(6) . . ?
N10 Mn2 N17 178.18(7) 2_565 . ?
N18 Mn2 N17 101.94(5) 2_565 . ?
C1 N1 N2 104.53(14) . . ?
C1 N1 Mn1 129.88(12) . . ?
N2 N1 Mn1 124.90(11) . . ?
N3 N2 N1 108.87(15) . . ?
N2 N3 N4 110.82(15) . . ?
C1 N4 N3 103.46(14) . . ?
C2 N5 C1 123.91(14) . . ?
C2 N5 H1 120.3(17) . . ?
C1 N5 H1 113.7(17) . . ?
C2 N6 N7 104.30(13) . . ?
C2 N6 Mn1 144.08(12) . 4_545 ?
N7 N6 Mn1 110.76(10) . 4_545 ?
N8 N7 N6 109.62(14) . . ?
N7 N8 N9 109.81(14) . . ?
C2 N9 N8 104.52(13) . . ?
C2 N9 Mn1 131.20(11) . . ?
N8 N9 Mn1 124.28(11) . . ?
C3 N10 N11 104.44(13) . . ?
C3 N10 Mn2 132.40(11) . 2_565 ?
N11 N10 Mn2 122.63(11) . 2_565 ?
N12 N11 N10 109.63(15) . . ?
N11 N12 N13 109.75(15) . . ?
C3 N13 N12 104.27(14) . . ?
C3 N14 C4 125.11(15) . . ?
C3 N14 H2 116(2) . . ?
C4 N14 H2 119(2) . . ?
C4 N15 N16 104.69(14) . . ?
N17 N16 N15 109.59(14) . . ?
N16 N17 N18 109.83(14) . . ?
N16 N17 Mn2 120.62(11) . . ?
N18 N17 Mn2 128.57(11) . . ?
C4 N18 N17 104.13(13) . . ?
C4 N18 Mn2 128.51(11) . 2_565 ?
N17 N18 Mn2 124.06(10) . 2_565 ?
Mn2 O1 H3 123.4(18) . . ?
Mn2 O1 H4 105(3) . . ?
H3 O1 H4 103(3) . . ?
Mn2 O2 H5 113(3) . . ?
Mn2 O2 H6 121(3) . . ?
H5 O2 H6 94(4) . . ?
Mn2 O3 H7 125.6(19) . . ?
Mn2 O3 H8 120(2) . . ?
H7 O3 H8 114(3) . . ?
Mn1 O4 H10 118(2) . . ?
Mn1 O4 H9 113(2) . . ?
H10 O4 H9 108(3) . . ?
Mn1 O5 H11 105(2) . . ?
Mn1 O5 H12 120(2) . . ?
H11 O5 H12 104(3) . . ?
Mn1 O6 H13 130(3) . . ?
Mn1 O6 H14 115(2) . . ?
H13 O6 H14 115(3) . . ?
N4 C1 N1 112.30(15) . . ?
N4 C1 N5 122.02(15) . . ?
N1 C1 N5 125.68(15) . . ?
N9 C2 N6 111.73(15) . . ?
N9 C2 N5 125.06(15) . . ?
N6 C2 N5 123.20(14) . . ?
N10 C3 N13 111.90(15) . . ?
N10 C3 N14 125.12(15) . . ?
N13 C3 N14 122.98(16) . . ?
N18 C4 N15 111.75(14) . . ?
N18 C4 N14 126.93(15) . . ?
N15 C4 N14 121.31(15) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.58
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.073

data_co5
_database_code_depnum_ccdc_archive 'CCDC 660797'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H6 Co N18 Na2 O2'
_chemical_formula_sum            'C4 H6 Co N18 Na2 O2'
_chemical_formula_weight         443.18

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   p21/c
_symmetry_space_group_name_Hall  -p2ybc

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                   9.4760(12)
_cell_length_b                   9.4375(11)
_cell_length_c                   8.2912(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.035(7)
_cell_angle_gamma                90.00
_cell_volume                     700.94(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1624
_cell_measurement_theta_min      2.274
_cell_measurement_theta_max      27.539

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.043
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.1
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             442
_exptl_absorpt_coefficient_mu    1.344
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            5593
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.27
_diffrn_reflns_theta_max         27.53
_reflns_number_total             1586
_reflns_number_gt                1436
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001-2005) '
_computing_cell_refinement       'SAINT (Bruker, 2001-2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001-2005)'
_computing_publication_material  SHELXTL

_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)+(0.0317P)²+0.3461P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0038(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1586
_refine_ls_number_parameters     137
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0245
_refine_ls_wR_factor_ref         0.0644
_refine_ls_wR_factor_gt          0.0621
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_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 0.5000 0.0000 0.01200(12) Uani 1 2 d S . .
Na1 Na 0.38788(8) 0.30333(8) 0.05602(10) 0.0274(2) Uani 1 1 d . . .
N2 N 0.34476(16) 0.55692(16) 0.07674(19) 0.0206(3) Uani 1 1 d . . .
N1 N 0.21632(16) 0.59453(15) 0.10541(18) 0.0167(3) Uani 1 1 d . . .
N3 N 0.43696(17) 0.66282(18) 0.1135(2) 0.0267(4) Uani 1 1 d . . .
N4 N 0.37565(18) 0.77366(17) 0.1714(2) 0.0273(4) Uani 1 1 d . . .
C1 C 0.24183(19) 0.72671(18) 0.1646(2) 0.0173(3) Uani 1 1 d . . .
N7 N -0.16651(16) 0.62648(16) 0.23804(18) 0.0187(3) Uani 1 1 d . . .
N9 N -0.05481(16) 0.82528(15) 0.32887(18) 0.0168(3) Uani 1 1 d . . .
N8 N -0.17113(16) 0.74028(16) 0.32411(19) 0.0193(3) Uani 1 1 d . . .
C2 C 0.01766(18) 0.75648(17) 0.23973(19) 0.0148(3) Uani 1 1 d . . .
N6 N -0.04734(16) 0.63348(15) 0.18128(17) 0.0162(3) Uani 1 1 d . . .
N5 N 0.14308(18) 0.80875(16) 0.2128(2) 0.0227(3) Uani 1 1 d . . .
O2 O 0.3546(3) 0.0631(2) -0.0134(3) 0.0496(5) Uani 1 1 d . . .
H1 H 0.169(2) 0.890(3) 0.248(3) 0.030(6) Uiso 1 1 d . . .
H3 H 0.365(7) 0.015(5) 0.046(7) 0.12(2) Uiso 1 1 d . . .
H2 H 0.313(10) 0.037(8) -0.089(12) 0.26(5) Uiso 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
Co1 N6 2.1183(14) . ?
Co1 N6 2.1183(14) 3_565 ?
Co1 N9 2.1263(14) 4_575 ?
Co1 N9 2.1263(14) 2_545 ?
Co1 N1 2.1432(14) . ?
Co1 N1 2.1432(14) 3_565 ?
Na1 O2 2.335(2) . ?
Na1 N2 2.4433(17) . ?
Na1 N3 2.5208(18) 3_665 ?
Na1 N8 2.6253(17) 2_545 ?
Na1 N4 2.6274(19) 2_645 ?
Na1 N7 2.7290(17) 3_565 ?
Na1 N3 3.0092(18) 2_645 ?
N2 N3 1.297(2) . ?
N2 N1 1.361(2) . ?
N1 C1 1.333(2) . ?
N3 N4 1.358(2) . ?
N3 Na1 2.5208(18) 3_665 ?
N3 Na1 3.0092(18) 2_655 ?
N4 C1 1.327(2) . ?
N4 Na1 2.6274(19) 2_655 ?
C1 N5 1.371(2) . ?
N7 N8 1.298(2) . ?
N7 N6 1.359(2) . ?
N7 Na1 2.7290(17) 3_565 ?
N9 C2 1.331(2) . ?
N9 N8 1.353(2) . ?
N9 Co1 2.1263(14) 2 ?
N8 Na1 2.6253(17) 2 ?
C2 N6 1.329(2) . ?
C2 N5 1.371(2) . ?
N5 H1 0.83(2) . ?
O2 H3 0.65(5) . ?
O2 H2 0.67(10) . ?

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
N6 Co1 N6 180.00(5) . 3_565 ?
N6 Co1 N9 87.14(5) . 4_575 ?
N6 Co1 N9 92.86(5) 3_565 4_575 ?
N6 Co1 N9 92.86(5) . 2_545 ?
N6 Co1 N9 87.14(5) 3_565 2_545 ?
N9 Co1 N9 180.00(5) 4_575 2_545 ?
N6 Co1 N1 81.88(5) . . ?
N6 Co1 N1 98.12(5) 3_565 . ?
N9 Co1 N1 86.69(5) 4_575 . ?
N9 Co1 N1 93.31(5) 2_545 . ?
N6 Co1 N1 98.12(5) . 3_565 ?
N6 Co1 N1 81.88(5) 3_565 3_565 ?
N9 Co1 N1 93.31(5) 4_575 3_565 ?
N9 Co1 N1 86.69(5) 2_545 3_565 ?
N1 Co1 N1 180.0 . 3_565 ?
O2 Na1 N2 162.97(8) . . ?
O2 Na1 N3 92.65(7) . 3_665 ?
N2 Na1 N3 94.05(6) . 3_665 ?
O2 Na1 N8 79.27(7) . 2_545 ?
N2 Na1 N8 91.49(5) . 2_545 ?
N3 Na1 N8 168.11(6) 3_665 2_545 ?
O2 Na1 N4 96.73(8) . 2_645 ?
N2 Na1 N4 99.16(6) . 2_645 ?
N3 Na1 N4 87.77(6) 3_665 2_645 ?
N8 Na1 N4 101.73(5) 2_545 2_645 ?
O2 Na1 N7 90.74(8) . 3_565 ?
N2 Na1 N7 74.19(5) . 3_565 ?
N3 Na1 N7 85.71(5) 3_665 3_565 ?
N8 Na1 N7 85.70(5) 2_545 3_565 ?
N4 Na1 N7 170.30(6) 2_645 3_565 ?
O2 Na1 N3 77.68(8) . 2_645 ?
N2 Na1 N3 115.01(6) . 2_645 ?
N3 Na1 N3 107.19(6) 3_665 2_645 ?
N8 Na1 N3 79.79(5) 2_545 2_645 ?
N4 Na1 N3 26.80(5) 2_645 2_645 ?
N7 Na1 N3 162.84(5) 3_565 2_645 ?
N3 N2 N1 109.28(14) . . ?
N3 N2 Na1 131.01(12) . . ?
N1 N2 Na1 116.57(11) . . ?
C1 N1 N2 104.08(14) . . ?
C1 N1 Co1 125.03(11) . . ?
N2 N1 Co1 127.66(11) . . ?
N2 N3 N4 110.10(14) . . ?
N2 N3 Na1 118.84(11) . 3_665 ?
N4 N3 Na1 122.34(12) . 3_665 ?
N2 N3 Na1 133.07(12) . 2_655 ?
N4 N3 Na1 60.73(10) . 2_655 ?
Na1 N3 Na1 100.60(6) 3_665 2_655 ?
C1 N4 N3 103.94(14) . . ?
C1 N4 Na1 127.39(12) . 2_655 ?
N3 N4 Na1 92.47(11) . 2_655 ?
N4 C1 N1 112.58(15) . . ?
N4 C1 N5 122.19(15) . . ?
N1 C1 N5 125.22(15) . . ?
N8 N7 N6 109.32(13) . . ?
N8 N7 Na1 97.84(10) . 3_565 ?
N6 N7 Na1 99.33(10) . 3_565 ?
C2 N9 N8 104.92(13) . . ?
C2 N9 Co1 133.71(11) . 2 ?
N8 N9 Co1 119.90(10) . 2 ?
N7 N8 N9 109.47(13) . . ?
N7 N8 Na1 124.50(11) . 2 ?
N9 N8 Na1 125.79(10) . 2 ?
N6 C2 N9 111.53(14) . . ?
N6 C2 N5 125.33(14) . . ?
N9 C2 N5 123.14(15) . . ?
C2 N6 N7 104.76(13) . . ?
C2 N6 Co1 126.72(11) . . ?
N7 N6 Co1 127.51(11) . . ?
C2 N5 C1 123.69(15) . . ?
C2 N5 H1 117.1(15) . . ?
C1 N5 H1 117.9(15) . . ?
Na1 O2 H3 121(5) . . ?
Na1 O2 H2 126(7) . . ?
H3 O2 H2 110(7) . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.062

data_cu1
_database_code_depnum_ccdc_archive 'CCDC 661222'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H5 Cu N9 O2'
_chemical_formula_sum            'C2 H5 Cu N9 O2'
_chemical_formula_weight         250.70

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   6.39620(10)
_cell_length_b                   9.2177(2)
_cell_length_c                   14.2410(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.8310(10)
_cell_angle_gamma                90.00
_cell_volume                     837.75(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1917
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      27.46

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.143
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.988
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             500.0
_exptl_absorpt_coefficient_mu    2.601
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.550
_exptl_absorpt_correction_T_max  0.689
_exptl_absorpt_process_details   SADABS
_exptl_special_details           
;
?
;

__diffrn_ambient_temperature     296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            12747
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.63
_diffrn_reflns_theta_max         27.46
_reflns_number_total             1917
_reflns_number_gt                1772
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0370P)²+1.1251P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0037(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1917
_refine_ls_number_parameters     148
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0274
_refine_ls_wR_factor_ref         0.0755
_refine_ls_wR_factor_gt          0.0740
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_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
Cu1 Cu 0.06656(4) 0.63014(3) 0.749677(17) 0.02099(12) Uani 1 1 d . . .
N1 N 0.0718(3) 0.6925(2) 0.61707(13) 0.0249(4) Uani 1 1 d . . .
N3 N 0.1594(4) 0.8182(3) 0.49832(16) 0.0417(6) Uani 1 1 d . . .
N2 N 0.2190(3) 0.7817(3) 0.58364(15) 0.0353(5) Uani 1 1 d . . .
C1 C -0.0733(4) 0.6800(3) 0.54640(16) 0.0245(5) Uani 1 1 d . . .
N4 N -0.0264(4) 0.7554(3) 0.47185(15) 0.0374(5) Uani 1 1 d . . .
N5 N -0.2524(4) 0.5989(3) 0.54856(16) 0.0345(5) Uani 1 1 d . . .
O2 O 0.0423(3) 0.5653(2) 0.88331(14) 0.0412(5) Uani 1 1 d . . .
O1 O 0.3742(3) 0.6731(3) 0.77267(16) 0.0481(5) Uani 1 1 d . . .
N8 N -0.4281(3) 0.3521(2) 0.70619(15) 0.0279(4) Uani 1 1 d . . .
N6 N -0.1796(3) 0.5097(2) 0.70498(13) 0.0228(4) Uani 1 1 d . . .
C2 C -0.2924(3) 0.5111(2) 0.62231(15) 0.0231(4) Uani 1 1 d . . .
N9 N -0.4485(3) 0.4163(2) 0.62019(14) 0.0275(4) Uani 1 1 d . . .
N7 N -0.2702(3) 0.4059(2) 0.75675(14) 0.0268(4) Uani 1 1 d . . .
H1 H -0.323(5) 0.602(3) 0.507(2) 0.029(8) Uiso 1 1 d . . .
H3 H 0.177(7) 0.600(4) 0.930(3) 0.064(12) Uiso 1 1 d . . .
H2 H -0.094(6) 0.609(4) 0.907(3) 0.050(10) Uiso 1 1 d . . .
H4 H 0.419(6) 0.722(4) 0.838(3) 0.056(10) Uiso 1 1 d . . .
H5 H 0.487(8) 0.597(6) 0.757(3) 0.085(15) Uiso 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
Cu1 N1 1.9765(19) . ?
Cu1 N6 1.9960(18) . ?
Cu1 O2 2.011(2) . ?
Cu1 O1 2.012(2) . ?
Cu1 N8 2.332(2) 2_456 ?
N1 C1 1.327(3) . ?
N1 N2 1.360(3) . ?
N3 N2 1.293(3) . ?
N3 N4 1.353(3) . ?
C1 N4 1.320(3) . ?
C1 N5 1.370(3) . ?
N5 C2 1.364(3) . ?
N5 H1 0.72(3) . ?
O2 H3 1.10(4) . ?
O2 H2 1.04(4) . ?
O1 H4 1.05(4) . ?
O1 H5 1.04(5) . ?
N8 N7 1.299(3) . ?
N8 N9 1.359(3) . ?
N8 Cu1 2.332(2) 2_446 ?
N6 C2 1.339(3) . ?
N6 N7 1.361(3) . ?
C2 N9 1.326(3) . ?

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
N1 Cu1 N6 85.43(8) . . ?
N1 Cu1 O2 176.53(8) . . ?
N6 Cu1 O2 91.57(8) . . ?
N1 Cu1 O1 91.12(9) . . ?
N6 Cu1 O1 154.61(10) . . ?
O2 Cu1 O1 92.34(9) . . ?
N1 Cu1 N8 91.91(8) . 2_456 ?
N6 Cu1 N8 105.55(8) . 2_456 ?
O2 Cu1 N8 87.19(8) . 2_456 ?
O1 Cu1 N8 99.69(9) . 2_456 ?
C1 N1 N2 104.62(18) . . ?
C1 N1 Cu1 130.05(16) . . ?
N2 N1 Cu1 124.52(15) . . ?
N2 N3 N4 110.4(2) . . ?
N3 N2 N1 108.58(19) . . ?
N4 C1 N1 112.3(2) . . ?
N4 C1 N5 122.7(2) . . ?
N1 C1 N5 125.0(2) . . ?
C1 N4 N3 104.10(19) . . ?
C2 N5 C1 122.8(2) . . ?
C2 N5 H1 121(2) . . ?
C1 N5 H1 116(2) . . ?
Cu1 O2 H3 112(2) . . ?
Cu1 O2 H2 108(2) . . ?
H3 O2 H2 110(3) . . ?
Cu1 O1 H4 116(2) . . ?
Cu1 O1 H5 121(3) . . ?
H4 O1 H5 109(3) . . ?
N7 N8 N9 110.94(19) . . ?
N7 N8 Cu1 118.76(15) . 2_446 ?
N9 N8 Cu1 127.57(15) . 2_446 ?
C2 N6 N7 105.03(17) . . ?
C2 N6 Cu1 129.95(15) . . ?
N7 N6 Cu1 125.01(14) . . ?
N9 C2 N6 112.0(2) . . ?
N9 C2 N5 123.6(2) . . ?
N6 C2 N5 124.4(2) . . ?
C2 N9 N8 103.87(18) . . ?
N8 N7 N6 108.16(18) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.078

# Attachment '1-Co.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 661223'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C6 H6 Co N27), 8(H2 O), O'
_chemical_formula_sum            'C12 H28 Co2 N54 O9'
_chemical_formula_weight         1190.74

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           monoclinic
_symmetry_space_group_name_H-M   P21/c

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                   11.3207(3)
_cell_length_b                   13.0862(4)
_cell_length_c                   15.3142(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.104(2)
_cell_angle_gamma                90.00
_cell_volume                     2218.28(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5156
_cell_measurement_theta_min      1.84
_cell_measurement_theta_max      27.630

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.143
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1208
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_process_details   SADAB

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            33524
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         27.63
_reflns_number_total             5071
_reflns_number_gt                4345
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0619P)²+2.2570P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0000(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5156
_refine_ls_number_parameters     393
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1197
_refine_ls_wR_factor_gt          0.1144
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.040

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 0.81885(3) 0.82690(2) 0.220920(19) 0.02271(12) Uani 1 1 d . . .
N19 N 0.92687(18) 0.75592(14) 0.16132(13) 0.0266(4) Uani 1 1 d . . .
N1 N 0.95501(17) 0.86355(15) 0.31264(13) 0.0262(4) Uani 1 1 d . . .
N6 N 0.71851(18) 0.89905(16) 0.28689(13) 0.0269(4) Uani 1 1 d . . .
N5 N 0.85938(19) 0.93402(18) 0.42403(14) 0.0311(5) Uani 1 1 d . . .
N24 N 0.84368(18) 0.94776(15) 0.15774(13) 0.0252(4) Uani 1 1 d . . .
N15 N 0.68767(19) 0.78777(16) 0.12542(14) 0.0295(4) Uani 1 1 d . . .
N10 N 0.78936(19) 0.70361(16) 0.28111(14) 0.0303(4) Uani 1 1 d . . .
N25 N 0.7816(2) 1.03622(16) 0.15796(15) 0.0344(5) Uani 1 1 d . . .
N7 N 0.5986(2) 0.91798(19) 0.25773(15) 0.0374(5) Uani 1 1 d . . .
N27 N 0.8982(2) 1.05303(17) 0.06270(15) 0.0358(5) Uani 1 1 d . . .
N26 N 0.8148(2) 1.09774(17) 0.10170(16) 0.0376(5) Uani 1 1 d . . .
N20 N 0.9654(2) 0.65761(17) 0.18098(18) 0.0426(6) Uani 1 1 d . . .
N23 N 0.9925(2) 0.89056(16) 0.07793(15) 0.0352(5) Uani 1 1 d . . .
H5 H 1.0404 0.9076 0.0436 0.042 Uiso 1 1 calc R . .
N22 N 1.0732(2) 0.72324(17) 0.09755(16) 0.0369(5) Uani 1 1 d . . .
H6 H 1.1274 0.7295 0.0660 0.044 Uiso 1 1 calc R . .
N11 N 0.8409(3) 0.6810(2) 0.36784(17) 0.0456(6) Uani 1 1 d . . .
N4 N 1.07138(19) 0.92754(18) 0.43253(14) 0.0339(5) Uani 1 1 d . . .
N2 N 1.07191(19) 0.85442(18) 0.30464(15) 0.0345(5) Uani 1 1 d . . .
N9 N 0.6513(2) 0.97855(18) 0.38898(15) 0.0360(5) Uani 1 1 d . . .
H2 H 0.6476 1.0085 0.4383 0.043 Uiso 1 1 calc R . .
N3 N 1.1392(2) 0.89237(19) 0.37639(15) 0.0374(5) Uani 1 1 d . . .
N18 N 0.5682(2) 0.6927(2) 0.02672(19) 0.0496(7) Uani 1 1 d . . .
N8 N 0.5585(2) 0.9660(2) 0.31880(17) 0.0430(6) Uani 1 1 d . . .
N17 N 0.5728(3) 0.7882(2) -0.00566(18) 0.0520(7) Uani 1 1 d . . .
N21 N 1.0524(3) 0.63843(18) 0.14244(19) 0.0487(6) Uani 1 1 d . . .
N12 N 0.8115(3) 0.5892(2) 0.3844(2) 0.0581(8) Uani 1 1 d . . .
N13 N 0.7410(3) 0.5511(2) 0.3089(2) 0.0594(8) Uani 1 1 d . . .
H4 H 0.7106 0.4906 0.3027 0.071 Uiso 1 1 calc R . .
N14 N 0.6622(3) 0.6138(2) 0.1622(2) 0.0546(8) Uani 1 1 d . . .
N16 N 0.6436(2) 0.8454(2) 0.05174(17) 0.0447(6) Uani 1 1 d . . .
C2 C 0.7494(2) 0.93700(18) 0.36928(15) 0.0270(5) Uani 1 1 d . . .
C3 C 0.6394(2) 0.6959(2) 0.1066(2) 0.0375(6) Uani 1 1 d . . .
C1 C 0.9586(2) 0.90885(18) 0.39091(15) 0.0269(5) Uani 1 1 d . . .
C4 C 0.7265(3) 0.6221(2) 0.2465(2) 0.0409(6) Uani 1 1 d . . .
C6 C 0.9137(2) 0.96108(18) 0.09891(16) 0.0279(5) Uani 1 1 d . . .
C5 C 0.9961(2) 0.79495(19) 0.11031(15) 0.0276(5) Uani 1 1 d . . .
O1 O 0.61883(19) 0.05862(15) 0.54291(13) 0.0320(4) Uani 1 1 d . . .
O2 O 0.2667(2) 0.75043(19) 0.0290(2) 0.0493(6) Uani 1 1 d . . .
O3 O 0.4247(6) 0.8144(4) 0.8117(3) 0.1340(18) Uani 1 1 d D . .
O4 O 0.6804(8) 0.3537(5) 0.2916(7) 0.292(6) Uani 1 1 d D . .
O5 O 0.5921(5) 0.4525(5) 0.4261(4) 0.0828(18) Uani 0.50 1 d P . .
H1 H 0.870(3) 0.971(3) 0.465(2) 0.052(10) Uiso 1 1 d . . .
H3 H 0.633(4) 0.568(4) 0.150(3) 0.072(14) Uiso 1 1 d . . .
H7 H 0.302(4) 0.787(4) 0.063(3) 0.069(15) Uiso 1 1 d . . .
H8 H 0.246(4) 0.779(4) -0.013(3) 0.070(16) Uiso 1 1 d . . .
H10 H 0.459(4) 0.869(2) 0.840(3) 0.069(14) Uiso 1 1 d D . .
H9 H 0.352(5) 0.828(18) 0.81(3) 1.0(3) Uiso 1 1 d D . .
H12 H 0.678(3) 0.303(2) 0.258(2) 0.042(10) Uiso 1 1 d D . .
H13 H 0.676(4) 0.091(3) 0.560(2) 0.050(11) Uiso 1 1 d . . .
H14 H 0.564(3) 0.098(3) 0.523(2) 0.052(10) Uiso 1 1 d . . .
H11 H 0.622(2) 0.346(2) 0.3174(19) 0.021(7) Uiso 1 1 d 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
Co1 N24 1.906(2) . ?
Co1 N19 1.9128(19) . ?
Co1 N1 1.916(2) . ?
Co1 N6 1.919(2) . ?
Co1 N10 1.922(2) . ?
Co1 N15 1.922(2) . ?
N19 C5 1.320(3) . ?
N19 N20 1.372(3) . ?
N1 C1 1.330(3) . ?
N1 N2 1.360(3) . ?
N6 C2 1.333(3) . ?
N6 N7 1.360(3) . ?
N5 C2 1.348(3) . ?
N5 C1 1.367(3) . ?
N5 H1 0.78(4) . ?
N24 C6 1.331(3) . ?
N24 N25 1.354(3) . ?
N15 C3 1.326(3) . ?
N15 N16 1.362(3) . ?
N10 C4 1.329(3) . ?
N10 N11 1.366(3) . ?
N25 N26 1.291(3) . ?
N7 N8 1.285(3) . ?
N27 C6 1.321(3) . ?
N27 N26 1.351(3) . ?
N20 N21 1.274(3) . ?
N23 C5 1.343(3) . ?
N23 C6 1.368(3) . ?
N23 H5 0.8600 . ?
N22 C5 1.324(3) . ?
N22 N21 1.352(3) . ?
N22 H6 0.8600 . ?
N11 N12 1.286(4) . ?
N4 C1 1.324(3) . ?
N4 N3 1.348(3) . ?
N2 N3 1.298(3) . ?
N9 C2 1.327(3) . ?
N9 N8 1.346(3) . ?
N9 H2 0.8600 . ?
N18 C3 1.317(4) . ?
N18 N17 1.349(4) . ?
N17 N16 1.296(3) . ?
N12 N13 1.355(4) . ?
N13 C4 1.318(4) . ?
N13 H4 0.8600 . ?
N14 C4 1.346(4) . ?
N14 C3 1.363(4) . ?
N14 H3 0.69(5) . ?
O1 H13 0.77(4) . ?
O1 H14 0.81(4) . ?
O2 H7 0.76(5) . ?
O2 H8 0.74(5) . ?
O3 H10 0.881(10) . ?
O3 H9 0.849(11) . ?
O4 H12 0.840(10) . ?
O4 H11 0.846(10) . ?

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
N24 Co1 N19 89.06(8) . . ?
N24 Co1 N1 89.01(8) . . ?
N19 Co1 N1 88.56(8) . . ?
N24 Co1 N6 91.46(8) . . ?
N19 Co1 N6 176.50(8) . . ?
N1 Co1 N6 87.99(8) . . ?
N24 Co1 N10 177.96(9) . . ?
N19 Co1 N10 90.80(9) . . ?
N1 Co1 N10 93.01(9) . . ?
N6 Co1 N10 88.80(9) . . ?
N24 Co1 N15 90.43(9) . . ?
N19 Co1 N15 88.67(9) . . ?
N1 Co1 N15 177.18(8) . . ?
N6 Co1 N15 94.79(9) . . ?
N10 Co1 N15 87.54(9) . . ?
C5 N19 N20 107.0(2) . . ?
C5 N19 Co1 127.80(17) . . ?
N20 N19 Co1 123.82(16) . . ?
C1 N1 N2 105.88(19) . . ?
C1 N1 Co1 129.81(17) . . ?
N2 N1 Co1 124.10(15) . . ?
C2 N6 N7 106.8(2) . . ?
C2 N6 Co1 127.95(17) . . ?
N7 N6 Co1 125.24(16) . . ?
C2 N5 C1 120.0(2) . . ?
C2 N5 H1 117(3) . . ?
C1 N5 H1 116(3) . . ?
C6 N24 N25 105.83(19) . . ?
C6 N24 Co1 128.67(16) . . ?
N25 N24 Co1 125.20(15) . . ?
C3 N15 N16 105.0(2) . . ?
C3 N15 Co1 128.61(19) . . ?
N16 N15 Co1 124.96(17) . . ?
C4 N10 N11 107.3(2) . . ?
C4 N10 Co1 127.91(19) . . ?
N11 N10 Co1 124.49(18) . . ?
N26 N25 N24 107.92(19) . . ?
N8 N7 N6 109.3(2) . . ?
C6 N27 N26 104.6(2) . . ?
N25 N26 N27 110.7(2) . . ?
N21 N20 N19 108.9(2) . . ?
C5 N23 C6 120.8(2) . . ?
C5 N23 H5 119.6 . . ?
C6 N23 H5 119.6 . . ?
C5 N22 N21 108.4(2) . . ?
C5 N22 H6 125.8 . . ?
N21 N22 H6 125.8 . . ?
N12 N11 N10 108.6(2) . . ?
C1 N4 N3 104.51(19) . . ?
N3 N2 N1 107.5(2) . . ?
C2 N9 N8 108.6(2) . . ?
C2 N9 H2 125.7 . . ?
N8 N9 H2 125.7 . . ?
N2 N3 N4 111.0(2) . . ?
C3 N18 N17 104.4(2) . . ?
N7 N8 N9 107.8(2) . . ?
N16 N17 N18 110.6(2) . . ?
N20 N21 N22 107.9(2) . . ?
N11 N12 N13 107.8(2) . . ?
C4 N13 N12 108.7(3) . . ?
C4 N13 H4 125.6 . . ?
N12 N13 H4 125.6 . . ?
C4 N14 C3 121.9(3) . . ?
C4 N14 H3 118(4) . . ?
C3 N14 H3 119(4) . . ?
N17 N16 N15 108.0(2) . . ?
N9 C2 N6 107.6(2) . . ?
N9 C2 N5 125.3(2) . . ?
N6 C2 N5 127.1(2) . . ?
N18 C3 N15 112.0(3) . . ?
N18 C3 N14 123.6(3) . . ?
N15 C3 N14 124.3(3) . . ?
N4 C1 N1 111.1(2) . . ?
N4 C1 N5 124.1(2) . . ?
N1 C1 N5 124.7(2) . . ?
N13 C4 N10 107.5(3) . . ?
N13 C4 N14 126.7(3) . . ?
N10 C4 N14 125.7(3) . . ?
N27 C6 N24 111.0(2) . . ?
N27 C6 N23 123.5(2) . . ?
N24 C6 N23 125.5(2) . . ?
N19 C5 N22 107.8(2) . . ?
N19 C5 N23 127.1(2) . . ?
N22 C5 N23 125.1(2) . . ?
H13 O1 H14 107(4) . . ?
H7 O2 H8 107(5) . . ?
H10 O3 H9 98(2) . . ?
H12 O4 H11 106(2) . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        27.63
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         1.329
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.073

data_3
_database_code_depnum_ccdc_archive 'CCDC 684778'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H3 Mn N9 O'
_chemical_formula_sum            'C2 H3 Mn N9 O'
_chemical_formula_weight         224.07

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   P21/n

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

_cell_length_a                   6.4026(7)
_cell_length_b                   9.7202(9)
_cell_length_c                   10.5861(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.079(5)
_cell_angle_gamma                90.00
_cell_volume                     656.23(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1521
_cell_measurement_theta_min      2.85
_cell_measurement_theta_max      27.560

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.120
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             444
_exptl_absorpt_coefficient_mu    1.983
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.638
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            5196
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.85
_diffrn_reflns_theta_max         27.56
_reflns_number_total             1521
_reflns_number_gt                1404
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0307P)²+1.0469P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0086(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1521
_refine_ls_number_parameters     131
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0280
_refine_ls_wR_factor_ref         0.0718
_refine_ls_wR_factor_gt          0.0710
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_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 1.53216(5) 0.16384(3) 0.36689(3) 0.01310(14) Uani 1 1 d . . .
N1 N 1.3660(3) 0.16380(18) 0.54761(17) 0.0152(4) Uani 1 1 d . . .
N2 N 1.3519(3) 0.05948(19) 0.63151(17) 0.0167(4) Uani 1 1 d . . .
N3 N 1.2746(3) 0.10407(19) 0.73322(17) 0.0180(4) Uani 1 1 d . . .
N4 N 1.2314(3) 0.23997(19) 0.72012(16) 0.0159(4) Uani 1 1 d . . .
N5 N 1.2819(3) 0.4040(2) 0.56194(17) 0.0172(4) Uani 1 1 d . . .
H1 H 1.256(5) 0.461(3) 0.611(3) 0.027(8) Uiso 1 1 d . . .
N6 N 1.3516(3) 0.36192(19) 0.34574(17) 0.0160(4) Uani 1 1 d . . .
N7 N 1.3103(3) 0.4367(2) 0.23823(17) 0.0189(4) Uani 1 1 d . . .
N8 N 1.2181(3) 0.5507(2) 0.26601(18) 0.0192(4) Uani 1 1 d . . .
N9 N 1.1922(3) 0.55535(19) 0.39162(18) 0.0182(4) Uani 1 1 d . . .
O1 O 1.8188(3) 0.1917(2) 0.49344(17) 0.0224(4) Uani 1 1 d . . .
H2 H 1.825(6) 0.139(4) 0.558(4) 0.042(10) Uiso 1 1 d . . .
H3 H 1.832(6) 0.267(5) 0.526(4) 0.052(11) Uiso 1 1 d . . .
C1 C 1.2927(3) 0.2726(2) 0.60652(19) 0.0132(4) Uani 1 1 d . . .
C2 C 1.2744(3) 0.4376(2) 0.4358(2) 0.0138(4) 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
Mn1 O1 2.1908(18) . ?
Mn1 N6 2.2467(19) . ?
Mn1 N1 2.2699(18) . ?
Mn1 N2 2.2936(19) 3_856 ?
Mn1 N4 2.2949(18) 4_665 ?
Mn1 N8 2.3147(19) 2_745 ?
N1 C1 1.334(3) . ?
N1 N2 1.356(3) . ?
N2 N3 1.299(3) . ?
N2 Mn1 2.2936(19) 3_856 ?
N3 N4 1.354(3) . ?
N4 C1 1.336(3) . ?
N4 Mn1 2.2949(18) 4_566 ?
N5 C1 1.361(3) . ?
N5 C2 1.372(3) . ?
N6 C2 1.333(3) . ?
N6 N7 1.357(3) . ?
N7 N8 1.301(3) . ?
N8 N9 1.355(3) . ?
N8 Mn1 2.3147(19) 2_755 ?
N9 C2 1.327(3) . ?

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 N6 110.54(7) . . ?
O1 Mn1 N1 85.09(7) . . ?
N6 Mn1 N1 78.97(6) . . ?
O1 Mn1 N2 81.91(7) . 3_856 ?
N6 Mn1 N2 167.18(7) . 3_856 ?
N1 Mn1 N2 99.74(6) . 3_856 ?
O1 Mn1 N4 82.99(7) . 4_665 ?
N6 Mn1 N4 83.99(7) . 4_665 ?
N1 Mn1 N4 154.26(7) . 4_665 ?
N2 Mn1 N4 101.05(7) 3_856 4_665 ?
O1 Mn1 N8 158.06(7) . 2_745 ?
N6 Mn1 N8 91.39(7) . 2_745 ?
N1 Mn1 N8 99.28(7) . 2_745 ?
N2 Mn1 N8 76.17(7) 3_856 2_745 ?
N4 Mn1 N8 100.28(7) 4_665 2_745 ?
C1 N1 N2 103.90(17) . . ?
C1 N1 Mn1 127.19(14) . . ?
N2 N1 Mn1 127.97(13) . . ?
N3 N2 N1 110.22(17) . . ?
N3 N2 Mn1 117.17(14) . 3_856 ?
N1 N2 Mn1 132.24(13) . 3_856 ?
N2 N3 N4 109.28(17) . . ?
C1 N4 N3 104.49(17) . . ?
C1 N4 Mn1 137.55(15) . 4_566 ?
N3 N4 Mn1 116.68(13) . 4_566 ?
C1 N5 C2 123.90(19) . . ?
C2 N6 N7 104.28(17) . . ?
C2 N6 Mn1 128.45(14) . . ?
N7 N6 Mn1 127.11(14) . . ?
N8 N7 N6 108.99(17) . . ?
N7 N8 N9 110.34(17) . . ?
N7 N8 Mn1 124.79(14) . 2_755 ?
N9 N8 Mn1 116.25(14) . 2_755 ?
C2 N9 N8 103.75(18) . . ?
N1 C1 N4 112.08(19) . . ?
N1 C1 N5 126.22(19) . . ?
N4 C1 N5 121.68(19) . . ?
N9 C2 N6 112.62(19) . . ?
N9 C2 N5 121.8(2) . . ?
N6 C2 N5 125.53(19) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.083


data_2
_database_code_depnum_ccdc_archive 'CCDC 687023'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H6 Mn N18 Na2 O2'
_chemical_formula_sum            'C4 H6 Mn N18 Na2 O2'
_chemical_formula_weight         439.19

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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                   9.4412(2)
_cell_length_b                   9.6151(2)
_cell_length_c                   8.6398(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.874(2)
_cell_angle_gamma                90.00
_cell_volume                     742.13(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1714
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      27.510

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.063
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             430
_exptl_absorpt_coefficient_mu    1.002
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            6008
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.28
_diffrn_reflns_theta_max         27.51
_reflns_number_total             1614
_reflns_number_gt                1396
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001-2005) '
_computing_cell_refinement       'SAINT (Bruker, 2001-2005)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001-2005)'
_computing_publication_material  SHELXTL

_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)+(0.0317P)²+0.3461P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.022(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1686
_refine_ls_number_parameters     137
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0772
_refine_ls_wR_factor_gt          0.0724
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.141
_refine_ls_shift/su_mean         0.015

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 0.0000 0.5000 0.0000 0.01558(15) Uani 1 2 d S . .
Na1 Na 0.38706(10) 0.30763(10) 0.05534(12) 0.0323(3) Uani 1 1 d . . .
N2 N 0.35178(19) 0.5638(2) 0.0810(2) 0.0253(4) Uani 1 1 d . . .
N1 N 0.22542(18) 0.59707(18) 0.1165(2) 0.0217(4) Uani 1 1 d . . .
N3 N 0.4417(2) 0.6692(2) 0.1144(3) 0.0334(5) Uani 1 1 d . . .
N4 N 0.3810(2) 0.7754(2) 0.1753(3) 0.0355(5) Uani 1 1 d . . .
C1 C 0.2495(2) 0.7257(2) 0.1741(3) 0.0212(5) Uani 1 1 d . . .
N7 N -0.1699(2) 0.6305(2) 0.2340(2) 0.0255(4) Uani 1 1 d . . .
N9 N -0.05238(19) 0.82137(19) 0.3291(2) 0.0228(4) Uani 1 1 d . . .
N8 N -0.17315(19) 0.7413(2) 0.3189(2) 0.0252(4) Uani 1 1 d . . .
C2 C 0.0210(2) 0.7532(2) 0.2452(3) 0.0193(5) Uani 1 1 d . . .
N6 N -0.04705(19) 0.63542(19) 0.1840(2) 0.0212(4) Uani 1 1 d . . .
N5 N 0.1505(2) 0.8033(2) 0.2253(3) 0.0311(5) Uani 1 1 d . . .
O2 O 0.3575(3) 0.0680(3) -0.0034(4) 0.0663(7) Uani 1 1 d . . .
H1 H 0.179(3) 0.882(3) 0.261(3) 0.042(8) Uiso 1 1 d . . .
H3 H 0.353(6) 0.028(6) 0.063(7) 0.11(2) Uiso 1 1 d . . .
H2 H 0.358(16) 0.036(15) -0.06(2) 0.49(11) Uiso 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
Mn1 N1 2.2423(17) . ?
Mn1 N1 2.2423(17) 3_565 ?
Mn1 N6 2.2083(17) . ?
Mn1 N6 2.2083(17) 3_565 ?
Mn1 N9 2.2143(17) 4_575 ?
Mn1 N9 2.2143(17) 2_545 ?
Na1 O2 2.357(3) . ?
Na1 N2 2.505(2) . ?
Na1 N3 2.519(2) 3_665 ?
Na1 N8 2.662(2) 2_545 ?
Na1 N4 2.647(2) 2_645 ?
Na1 N7 2.737(2) 3_565 ?
N2 N3 1.294(3) . ?
N2 N1 1.363(2) . ?
N1 C1 1.325(3) . ?
N3 N4 1.358(3) . ?
N3 Na1 2.519(2) 3_665 ?
N4 C1 1.327(3) . ?
N4 Na1 2.647(2) 2_655 ?
C1 N5 1.377(3) . ?
N7 N8 1.299(3) . ?
N7 N6 1.363(2) . ?
N7 Na1 2.737(2) 3_565 ?
N9 C2 1.327(3) . ?
N9 N8 1.355(2) . ?
N9 Mn1 2.2143(17) 2 ?
N8 Na1 2.662(2) 2 ?
C2 N6 1.325(3) . ?
C2 N5 1.375(3) . ?
N5 H1 0.83(3) . ?
O2 H3 0.70(6) . ?
O2 H2 0.61(15) . ?

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
N1 Mn1 N1 180.0 . 3_565 ?
N1 Mn1 N6 79.29(6) . . ?
N1 Mn1 N6 100.71(6) 3_565 . ?
N1 Mn1 N6 100.71(6) . 3_565 ?
N1 Mn1 N6 79.29(6) 3_565 3_565 ?
N6 Mn1 N6 180.00(6) . 3_565 ?
N1 Mn1 N9 87.21(7) . 4_575 ?
N1 Mn1 N9 92.79(7) 3_565 4_575 ?
N6 Mn1 N9 88.24(7) . 4_575 ?
N6 Mn1 N9 91.76(7) 3_565 4_575 ?
N1 Mn1 N9 92.79(7) . 2_545 ?
N1 Mn1 N9 87.21(7) 3_565 2_545 ?
N6 Mn1 N9 91.76(7) . 2_545 ?
N6 Mn1 N9 88.24(7) 3_565 2_545 ?
N9 Mn1 N9 180.00(6) 4_575 2_545 ?
O2 Na1 N2 166.09(10) . . ?
O2 Na1 N3 90.83(10) . 3_665 ?
N2 Na1 N3 95.35(7) . 3_665 ?
O2 Na1 N8 78.52(9) . 2_545 ?
N2 Na1 N8 93.41(7) . 2_545 ?
N3 Na1 N8 166.70(7) 3_665 2_545 ?
O2 Na1 N4 94.67(10) . 2_645 ?
N2 Na1 N4 97.66(7) . 2_645 ?
N3 Na1 N4 91.02(7) 3_665 2_645 ?
N8 Na1 N4 97.72(7) 2_545 2_645 ?
O2 Na1 N7 90.82(10) . 3_565 ?
N2 Na1 N7 77.60(6) . 3_565 ?
N3 Na1 N7 83.18(7) 3_665 3_565 ?
N8 Na1 N7 88.96(6) 2_545 3_565 ?
N4 Na1 N7 172.08(7) 2_645 3_565 ?
N3 N2 N1 108.95(17) . . ?
N3 N2 Na1 133.94(14) . . ?
N1 N2 Na1 113.71(13) . . ?
C1 N1 N2 104.32(16) . . ?
C1 N1 Mn1 125.44(14) . . ?
N2 N1 Mn1 125.02(13) . . ?
N2 N3 N4 110.30(18) . . ?
N2 N3 Na1 115.97(15) . 3_665 ?
N4 N3 Na1 126.18(15) . 3_665 ?
C1 N4 N3 103.73(18) . . ?
C1 N4 Na1 123.72(16) . 2_655 ?
N3 N4 Na1 95.52(14) . 2_655 ?
N4 C1 N1 112.70(19) . . ?
N4 C1 N5 122.2(2) . . ?
N1 C1 N5 125.07(19) . . ?
N8 N7 N6 109.16(16) . . ?
N8 N7 Na1 100.96(13) . 3_565 ?
N6 N7 Na1 99.54(12) . 3_565 ?
C2 N9 N8 105.13(17) . . ?
C2 N9 Mn1 134.77(14) . 2 ?
N8 N9 Mn1 119.06(13) . 2 ?
N7 N8 N9 109.24(17) . . ?
N7 N8 Na1 125.90(13) . 2 ?
N9 N8 Na1 124.82(13) . 2 ?
N6 C2 N9 111.64(18) . . ?
N6 C2 N5 125.87(19) . . ?
N9 C2 N5 122.48(19) . . ?
C2 N6 N7 104.83(16) . . ?
C2 N6 Mn1 127.35(14) . . ?
N7 N6 Mn1 126.69(13) . . ?
C2 N5 C1 125.0(2) . . ?
C2 N5 H1 118.1(19) . . ?
C1 N5 H1 116.1(19) . . ?
Na1 O2 H3 113(5) . . ?
Na1 O2 H2 130(10) . . ?
H3 O2 H2 117(10) . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.086

data_mn
_database_code_depnum_ccdc_archive 'CCDC 692764'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H32 Mn7 N54 O14'
_chemical_formula_sum            'C12 H32 Mn7 N54 O14'
_chemical_formula_weight         1541.50

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           Hexagonal
_symmetry_space_group_name_H-M   P-3c1

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, -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'

_cell_length_a                   14.3137(3)
_cell_length_b                   14.3137(3)
_cell_length_c                   13.7292(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2436.01(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1878
_cell_measurement_theta_min      1.64
_cell_measurement_theta_max      27.520

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.120
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.102
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1522
_exptl_absorpt_coefficient_mu    1.872
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.654
_exptl_absorpt_correction_T_max  0.799
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            11729
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0128
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         27.48
_reflns_number_total             1870
_reflns_number_gt                1719
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0393P)²+1.6695P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0056(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1870
_refine_ls_number_parameters     149
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0218
_refine_ls_wR_factor_ref         0.0662
_refine_ls_wR_factor_gt          0.0653
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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 0.299792(18) 0.502236(18) 0.149714(17) 0.01712(11) Uani 1 1 d . . .
Mn2 Mn 0.0000 0.0000 0.0000 0.01603(14) Uani 1 6 d S . .
O1 O 0.3333 0.6667 0.18262(14) 0.0167(4) Uani 1 3 d S . .
O2 O 0.31301(12) 0.54142(12) -0.00833(10) 0.0271(3) Uani 1 1 d . . .
O3 O 0.31333(10) 0.48321(10) 0.30737(9) 0.0243(3) Uani 1 1 d . . .
N7 N 0.53194(12) 0.51718(11) 0.12787(11) 0.0249(3) Uani 1 1 d . . .
N3 N 0.22366(11) 0.31830(11) 0.13132(10) 0.0207(3) Uani 1 1 d . . .
N5 N 0.21323(12) 0.16340(11) 0.10606(11) 0.0231(3) Uani 1 1 d . . .
N4 N 0.27865(11) 0.26334(12) 0.12727(11) 0.0244(3) Uani 1 1 d . . .
N8 N 0.63761(11) 0.58764(11) 0.11620(11) 0.0239(3) Uani 1 1 d . . .
N6 N 0.11197(11) 0.14682(11) 0.09382(11) 0.0212(3) Uani 1 1 d . . .
N2 N 0.47980(11) 0.56865(11) 0.13973(10) 0.0209(3) Uani 1 1 d . . .
N1 N 0.12641(10) 0.44999(10) 0.13644(10) 0.0191(3) Uani 1 1 d . . .
C1 C 0.64542(12) 0.68398(13) 0.12147(11) 0.0175(3) Uani 1 1 d . . .
N9 N 0.74261(11) 0.77699(11) 0.11230(12) 0.0245(3) Uani 1 1 d . . .
C2 C 0.75672(12) 0.87871(13) 0.11215(11) 0.0181(3) Uani 1 1 d . . .
H1 H 0.314(2) 0.498(2) -0.043(2) 0.044(7) Uiso 1 1 d . . .
H2 H 0.274(3) 0.554(2) -0.026(2) 0.061(10) Uiso 1 1 d . . .
H3 H 0.286(2) 0.417(2) 0.3262(18) 0.043(7) Uiso 1 1 d . . .
H4 H 0.374(3) 0.508(3) 0.329(2) 0.068(10) Uiso 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
Mn1 O3 2.1999(13) . ?
Mn1 O1 2.2012(5) . ?
Mn1 N1 2.2129(13) . ?
Mn1 O2 2.2231(14) . ?
Mn1 N2 2.2613(13) . ?
Mn1 N3 2.3056(14) . ?
Mn2 N6 2.2965(14) . ?
Mn2 N6 2.2965(14) 7 ?
Mn2 N6 2.2965(14) 2 ?
Mn2 N6 2.2965(14) 3 ?
Mn2 N6 2.2965(14) 9 ?
Mn2 N6 2.2965(14) 8 ?
O1 Mn1 2.2012(5) 3_565 ?
O1 Mn1 2.2012(5) 2_665 ?
N7 N2 1.295(2) . ?
N7 N8 1.3438(19) . ?
N3 C2 1.333(2) 3_565 ?
N3 N4 1.3643(19) . ?
N5 N4 1.292(2) . ?
N5 N6 1.3572(19) . ?
N8 C1 1.329(2) . ?
N6 C2 1.339(2) 3_565 ?
N2 N1 1.3572(18) 2_665 ?
N1 C1 1.331(2) 3_565 ?
N1 N2 1.3572(18) 3_565 ?
C1 N1 1.331(2) 2_665 ?
C1 N9 1.368(2) . ?
N9 C2 1.367(2) . ?
C2 N3 1.333(2) 2_665 ?
C2 N6 1.339(2) 2_665 ?

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 Mn1 O1 86.86(6) . . ?
O3 Mn1 N1 101.09(5) . . ?
O1 Mn1 N1 89.22(3) . . ?
O3 Mn1 O2 171.05(5) . . ?
O1 Mn1 O2 89.11(6) . . ?
N1 Mn1 O2 86.82(5) . . ?
O3 Mn1 N2 87.66(5) . . ?
O1 Mn1 N2 88.25(4) . . ?
N1 Mn1 N2 170.74(5) . . ?
O2 Mn1 N2 84.23(5) . . ?
O3 Mn1 N3 89.24(5) . . ?
O1 Mn1 N3 165.85(4) . . ?
N1 Mn1 N3 78.18(5) . . ?
O2 Mn1 N3 96.52(5) . . ?
N2 Mn1 N3 105.20(5) . . ?
N6 Mn2 N6 180.00(9) . 7 ?
N6 Mn2 N6 91.67(5) . 2 ?
N6 Mn2 N6 88.33(5) 7 2 ?
N6 Mn2 N6 91.67(5) . 3 ?
N6 Mn2 N6 88.33(5) 7 3 ?
N6 Mn2 N6 91.67(5) 2 3 ?
N6 Mn2 N6 88.33(5) . 9 ?
N6 Mn2 N6 91.67(5) 7 9 ?
N6 Mn2 N6 88.33(5) 2 9 ?
N6 Mn2 N6 180.00(8) 3 9 ?
N6 Mn2 N6 88.33(5) . 8 ?
N6 Mn2 N6 91.67(5) 7 8 ?
N6 Mn2 N6 180.00(9) 2 8 ?
N6 Mn2 N6 88.33(5) 3 8 ?
N6 Mn2 N6 91.67(5) 9 8 ?
Mn1 O1 Mn1 115.91(3) 3_565 2_665 ?
Mn1 O1 Mn1 115.91(3) 3_565 . ?
Mn1 O1 Mn1 115.91(3) 2_665 . ?
N2 N7 N8 109.93(13) . . ?
C2 N3 N4 103.87(13) 3_565 . ?
C2 N3 Mn1 130.08(11) 3_565 . ?
N4 N3 Mn1 125.70(10) . . ?
N4 N5 N6 109.94(13) . . ?
N5 N4 N3 109.88(13) . . ?
C1 N8 N7 104.57(13) . . ?
C2 N6 N5 104.01(13) 3_565 . ?
C2 N6 Mn2 135.64(11) 3_565 . ?
N5 N6 Mn2 115.16(10) . . ?
N7 N2 N1 109.43(12) . 2_665 ?
N7 N2 Mn1 128.93(11) . . ?
N1 N2 Mn1 121.37(10) 2_665 . ?
C1 N1 N2 104.13(12) 3_565 3_565 ?
C1 N1 Mn1 133.17(11) 3_565 . ?
N2 N1 Mn1 122.66(10) 3_565 . ?
N8 C1 N1 111.94(14) . 2_665 ?
N8 C1 N9 121.47(14) . . ?
N1 C1 N9 126.59(14) 2_665 . ?
C2 N9 C1 125.02(14) . . ?
N3 C2 N6 112.26(14) 2_665 2_665 ?
N3 C2 N9 126.41(14) 2_665 . ?
N6 C2 N9 121.32(14) 2_665 . ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.063

