# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
_publ_author_address
'Keith Murray'
;School of Chemistry
Monash University
Clayton
VIC 3800
Australia
;
'Stuart R. Batten'
;School of Chemistry
Monash University
Clayton
VIC 3800
Australia
;
'Paul Jensen'
;School of Chemistry
Monash University
Clayton
VIC 3800
Australia
;
'Boujemaa Moubaraki'
;School of Chemistry
Monash University
Clayton
VIC 3800
Australia
;
'David Turner'
;School of Chemistry
Monash University
Clayton
VIC 3800
Australia
;

_publ_contact_author_name        'Keith Murray'
_publ_contact_author_email       KEITH.MURRAY@SCI.MONASH.EDU.AU

_publ_section_title              
;
Coordination Polymers of Nitrocyanamide, O2NNCN-.
Synthesis, Structure and Magnetism
;
_publ_contact_author_address     
;School of Chemistry
Monash University
Clayton
VIC 3800
Australia
;
_publ_requested_journal          CrystEngComm

# Attachment 'AnnaCh6_CIF.CIF'

data_1
_database_code_depnum_ccdc_archive 'CCDC 725137'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
catena[bis(nitrocyanamide)(pyrazine)Copper(II)]
;
_chemical_name_common            '[Cu(CAN)2(pyz)]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H4 Cu N8 O4'
_chemical_formula_sum            'C6 H4 Cu N8 O4'
_chemical_formula_weight         315.71

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           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   6.3272(2)
_cell_length_b                   6.8535(2)
_cell_length_c                   6.9057(2)
_cell_angle_alpha                112.863(2)
_cell_angle_beta                 102.779(2)
_cell_angle_gamma                103.167(2)
_cell_volume                     252.161(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    123(1)
_cell_measurement_reflns_used    2087
_cell_measurement_theta_min      3.41
_cell_measurement_theta_max      27.49

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.079
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             157
_exptl_absorpt_coefficient_mu    2.196
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.3983
_exptl_absorpt_correction_T_max  0.7194
_exptl_absorpt_process_details   SORTAV

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(1)
_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  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2087
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.41
_diffrn_reflns_theta_max         27.49
_reflns_number_total             1096
_reflns_number_gt                1038
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Hooft, 1999)'
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression ?
_refine_ls_number_reflns         1096
_refine_ls_number_parameters     88
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0886
_refine_ls_wR_factor_gt          0.0863
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_restrained_S_all      1.136
_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 0.5000 0.5000 0.5000 0.00683(18) Uani 1 2 d S . .
O1 O -0.0990(3) 0.6651(3) 0.7333(3) 0.0120(4) Uani 1 1 d . . .
N1 N 0.4981(4) 0.7984(3) 0.5021(3) 0.0067(4) Uani 1 1 d . . .
N2 N 0.3719(4) 0.5658(4) 0.7437(4) 0.0098(5) Uani 1 1 d . . .
O2 O -0.1091(3) 0.8100(3) 1.0735(3) 0.0160(4) Uani 1 1 d . . .
C1 C 0.3298(5) 0.8802(4) 0.5377(4) 0.0082(5) Uani 1 1 d . . .
H1 H 0.2066 0.7988 0.5650 0.010 Uiso 1 1 calc R . .
N4 N -0.0125(4) 0.7334(4) 0.9412(4) 0.0101(5) Uani 1 1 d . . .
N3 N 0.1968(4) 0.7228(4) 1.0266(4) 0.0124(5) Uani 1 1 d . . .
C2 C 0.6677(5) 0.9183(4) 0.4647(4) 0.0080(5) Uani 1 1 d . . .
H2 H 0.7896 0.8642 0.4392 0.010 Uiso 1 1 calc R . .
C3 C 0.2808(4) 0.6372(4) 0.8679(4) 0.0088(5) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0089(3) 0.0077(2) 0.0092(3) 0.00560(19) 0.00637(18) 0.00596(18)
O1 0.0089(10) 0.0180(10) 0.0088(9) 0.0062(8) 0.0024(8) 0.0049(8)
N1 0.0076(11) 0.0075(10) 0.0049(10) 0.0028(8) 0.0013(8) 0.0037(8)
N2 0.0103(12) 0.0117(11) 0.0101(11) 0.0061(9) 0.0042(9) 0.0057(9)
O2 0.0136(11) 0.0219(11) 0.0163(10) 0.0062(8) 0.0117(8) 0.0111(9)
C1 0.0081(13) 0.0105(12) 0.0075(12) 0.0045(10) 0.0032(10) 0.0048(10)
N4 0.0083(11) 0.0111(10) 0.0109(11) 0.0050(9) 0.0037(9) 0.0029(9)
N3 0.0103(12) 0.0210(12) 0.0082(11) 0.0060(10) 0.0048(9) 0.0093(10)
C2 0.0070(13) 0.0100(12) 0.0082(12) 0.0039(10) 0.0037(10) 0.0047(10)
C3 0.0082(13) 0.0102(12) 0.0084(12) 0.0057(10) 0.0015(10) 0.0027(10)

_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 N2 1.968(2) 2_666 ?
Cu1 N2 1.968(2) . ?
Cu1 N1 2.042(2) . ?
Cu1 N1 2.042(2) 2_666 ?
Cu1 O1 2.4043(19) 1_655 ?
Cu1 O1 2.4043(19) 2_566 ?
O1 N4 1.262(3) . ?
O1 Cu1 2.4043(19) 1_455 ?
N1 C2 1.334(3) . ?
N1 C1 1.338(3) . ?
N2 C3 1.152(3) . ?
O2 N4 1.226(3) . ?
C1 C2 1.384(4) 2_676 ?
N4 N3 1.356(3) . ?
N3 C3 1.315(3) . ?
C2 C1 1.384(3) 2_676 ?

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
N2 Cu1 N2 180.000(1) 2_666 . ?
N2 Cu1 N1 90.04(9) 2_666 . ?
N2 Cu1 N1 89.96(9) . . ?
N2 Cu1 N1 89.96(9) 2_666 2_666 ?
N2 Cu1 N1 90.04(9) . 2_666 ?
N1 Cu1 N1 180.0 . 2_666 ?
N2 Cu1 O1 83.17(8) 2_666 1_655 ?
N2 Cu1 O1 96.83(8) . 1_655 ?
N1 Cu1 O1 91.89(8) . 1_655 ?
N1 Cu1 O1 88.11(8) 2_666 1_655 ?
N2 Cu1 O1 96.83(8) 2_666 2_566 ?
N2 Cu1 O1 83.17(8) . 2_566 ?
N1 Cu1 O1 88.11(8) . 2_566 ?
N1 Cu1 O1 91.89(8) 2_666 2_566 ?
O1 Cu1 O1 180.0 1_655 2_566 ?
N4 O1 Cu1 128.64(16) . 1_455 ?
C2 N1 C1 117.5(2) . . ?
C2 N1 Cu1 120.03(17) . . ?
C1 N1 Cu1 122.47(17) . . ?
C3 N2 Cu1 163.9(2) . . ?
N1 C1 C2 121.0(2) . 2_676 ?
O2 N4 O1 123.1(2) . . ?
O2 N4 N3 117.2(2) . . ?
O1 N4 N3 119.7(2) . . ?
C3 N3 N4 111.1(2) . . ?
N1 C2 C1 121.5(2) . 2_676 ?
N2 C3 N3 173.9(3) . . ?

_diffrn_measured_fraction_theta_max 0.954
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.954
_refine_diff_density_max         0.512
_refine_diff_density_min         -1.436
_refine_diff_density_rms         0.200

data_2Co
_database_code_depnum_ccdc_archive 'CCDC 725138'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
catena[bis(aqua)bis(nitrocyanamide)(pyrazine)copper(II)] dihydrate
;
_chemical_name_common            {[Cu(CAN)2(pyz)(H2O)2].2H2O}
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H8 Co N8 O6, 2(H2 O)'
_chemical_formula_sum            'C6 H12 Co N8 O8'
_chemical_formula_weight         383.17

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

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

_cell_length_a                   6.7301(1)
_cell_length_b                   7.0910(1)
_cell_length_c                   8.6218(2)
_cell_angle_alpha                109.184(1)
_cell_angle_beta                 90.647(1)
_cell_angle_gamma                107.858(1)
_cell_volume                     367.001(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    123(1)
_cell_measurement_reflns_used    6753
_cell_measurement_theta_min      3.33
_cell_measurement_theta_max      27.50

_exptl_crystal_description       needle
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             195
_exptl_absorpt_coefficient_mu    1.227
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6396
_exptl_absorpt_correction_T_max  0.8568
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(1)
_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 X8 Apex II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6753
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.33
_diffrn_reflns_theta_max         27.50
_reflns_number_total             1680
_reflns_number_gt                1497
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker)'
_computing_cell_refinement       'Bruker SMART (Bruker)'
_computing_data_reduction        'Bruker SAINT (Bruker)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1680
_refine_ls_number_parameters     122
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0250
_refine_ls_wR_factor_ref         0.0565
_refine_ls_wR_factor_gt          0.0548
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_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
Co1 Co 0.5000 0.5000 0.5000 0.01063(10) Uani 1 2 d S . .
O1 O 0.18205(18) 0.41596(18) 0.51128(17) 0.0155(2) Uani 1 1 d . . .
N1 N 0.5038(2) 0.80471(18) 0.50002(16) 0.0116(3) Uani 1 1 d . . .
N2 N 0.4320(2) 0.37233(19) 0.23977(16) 0.0147(3) Uani 1 1 d . . .
O3 O 0.1924(2) -0.09267(17) -0.03427(15) 0.0251(3) Uani 1 1 d . . .
N4 N 0.2032(2) 0.0174(2) -0.12194(16) 0.0181(3) Uani 1 1 d . . .
N3 N 0.2971(2) 0.2300(2) -0.05824(16) 0.0183(3) Uani 1 1 d . . .
C11 C 0.6329(2) 0.9869(2) 0.60885(19) 0.0134(3) Uani 1 1 d . . .
H11 H 0.7296 0.9829 0.6878 0.016 Uiso 1 1 calc R . .
O4 O 0.1293(2) -0.05600(19) -0.26952(15) 0.0281(3) Uani 1 1 d . . .
C10 C 0.3718(2) 0.8199(2) 0.39145(19) 0.0132(3) Uani 1 1 d . . .
H10 H 0.2786 0.6942 0.3121 0.016 Uiso 1 1 calc R . .
C12 C 0.3653(2) 0.2940(2) 0.10178(19) 0.0137(3) Uani 1 1 d . . .
O2 O 0.07090(19) 0.4553(2) 0.81246(15) 0.0202(3) Uani 1 1 d . . .
H3 H 0.140(4) 0.428(4) 0.601(3) 0.041(7) Uiso 1 1 d . . .
H4 H 0.097(4) 0.329(4) 0.441(3) 0.041(7) Uiso 1 1 d . . .
H5 H 0.143(4) 0.404(4) 0.856(3) 0.047(7) Uiso 1 1 d . . .
H6 H 0.107(4) 0.574(4) 0.865(3) 0.055(8) 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 0.01269(17) 0.00774(15) 0.01087(17) 0.00249(11) -0.00135(11) 0.00347(11)
O1 0.0132(6) 0.0164(6) 0.0132(7) 0.0020(5) -0.0008(5) 0.0034(5)
N1 0.0126(6) 0.0093(6) 0.0129(7) 0.0036(5) 0.0006(5) 0.0040(5)
N2 0.0190(7) 0.0112(6) 0.0135(7) 0.0043(5) 0.0005(6) 0.0046(5)
O3 0.0359(7) 0.0150(6) 0.0209(7) 0.0047(5) 0.0023(5) 0.0056(5)
N4 0.0182(7) 0.0165(7) 0.0138(7) 0.0010(6) 0.0024(6) 0.0021(5)
N3 0.0249(8) 0.0137(6) 0.0104(7) 0.0022(5) -0.0024(6) 0.0005(5)
C11 0.0134(8) 0.0121(7) 0.0134(8) 0.0031(6) -0.0032(6) 0.0038(6)
O4 0.0297(7) 0.0284(7) 0.0114(6) -0.0022(5) -0.0037(5) -0.0008(5)
C10 0.0129(8) 0.0117(7) 0.0132(8) 0.0032(6) -0.0019(6) 0.0028(6)
C12 0.0152(8) 0.0108(7) 0.0161(9) 0.0063(6) 0.0026(6) 0.0039(6)
O2 0.0191(6) 0.0198(6) 0.0175(6) 0.0035(5) -0.0011(5) 0.0040(5)

_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 O1 2.0504(11) . ?
Co1 O1 2.0504(11) 2_666 ?
Co1 N2 2.1097(13) 2_666 ?
Co1 N2 2.1097(13) . ?
Co1 N1 2.1530(12) . ?
Co1 N1 2.1530(12) 2_666 ?
O1 H3 0.81(3) . ?
O1 H4 0.78(2) . ?
N1 C10 1.3352(19) . ?
N1 C11 1.3420(19) . ?
N2 C12 1.1516(19) . ?
O3 N4 1.2409(18) . ?
N4 O4 1.2364(17) . ?
N4 N3 1.3556(18) . ?
N3 C12 1.329(2) . ?
C11 C10 1.381(2) 2_676 ?
C11 H11 0.9500 . ?
C10 C11 1.381(2) 2_676 ?
C10 H10 0.9500 . ?
O2 H5 0.84(3) . ?
O2 H6 0.77(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 Co1 O1 180.00(8) . 2_666 ?
O1 Co1 N2 92.11(5) . 2_666 ?
O1 Co1 N2 87.89(5) 2_666 2_666 ?
O1 Co1 N2 87.89(5) . . ?
O1 Co1 N2 92.11(5) 2_666 . ?
N2 Co1 N2 180.0 2_666 . ?
O1 Co1 N1 89.85(4) . . ?
O1 Co1 N1 90.15(4) 2_666 . ?
N2 Co1 N1 89.19(5) 2_666 . ?
N2 Co1 N1 90.81(5) . . ?
O1 Co1 N1 90.15(4) . 2_666 ?
O1 Co1 N1 89.85(4) 2_666 2_666 ?
N2 Co1 N1 90.81(5) 2_666 2_666 ?
N2 Co1 N1 89.19(5) . 2_666 ?
N1 Co1 N1 180.0 . 2_666 ?
Co1 O1 H3 119.0(16) . . ?
Co1 O1 H4 124.6(17) . . ?
H3 O1 H4 110(2) . . ?
C10 N1 C11 116.69(12) . . ?
C10 N1 Co1 120.58(9) . . ?
C11 N1 Co1 122.72(10) . . ?
C12 N2 Co1 170.20(12) . . ?
O4 N4 O3 123.37(13) . . ?
O4 N4 N3 115.83(13) . . ?
O3 N4 N3 120.80(13) . . ?
C12 N3 N4 111.27(13) . . ?
N1 C11 C10 121.45(14) . 2_676 ?
N1 C11 H11 119.3 . . ?
C10 C11 H11 119.3 2_676 . ?
N1 C10 C11 121.87(13) . 2_676 ?
N1 C10 H10 119.1 . . ?
C11 C10 H10 119.1 2_676 . ?
N2 C12 N3 172.21(15) . . ?
H5 O2 H6 105(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H3 O2 0.81(3) 1.85(3) 2.6601(18) 174(2) .
O1 H4 O4 0.78(2) 2.12(3) 2.8941(17) 170(2) 2
O2 H5 N3 0.84(3) 2.13(3) 2.9556(19) 172(2) 1_556
O2 H6 O3 0.77(3) 2.11(3) 2.8763(17) 169(3) 1_566

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.061

data_2Fe
_database_code_depnum_ccdc_archive 'CCDC 725139'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
catena[bis(aqua)bis(nitrocyanamide)(pyrazine)iron(II)] dihydrate
;
_chemical_name_common            {[Fe(CAN)2(pyz)(H2O)2].2H2O}
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H8 Fe N8 O6, 2 (H2 O)'
_chemical_formula_sum            'C6 H12 Fe N8 O8'
_chemical_formula_weight         380.09

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'
Fe Fe 0.3463 0.8444 '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

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

_cell_length_a                   6.7652(1)
_cell_length_b                   7.1822(1)
_cell_length_c                   8.6218(2)
_cell_angle_alpha                109.404(1)
_cell_angle_beta                 90.408(1)
_cell_angle_gamma                108.002(1)
_cell_volume                     372.961(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    123(1)
_cell_measurement_reflns_used    6688
_cell_measurement_theta_min      3.69
_cell_measurement_theta_max      27.49

_exptl_crystal_description       rods
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             194
_exptl_absorpt_coefficient_mu    1.068
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.5912
_exptl_absorpt_correction_T_max  0.8736
_exptl_absorpt_process_details   SORTAV

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(1)
_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  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6688
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.69
_diffrn_reflns_theta_max         27.49
_reflns_number_total             1706
_reflns_number_gt                1552
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Hooft, 1999)'
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression ?
_refine_ls_number_reflns         1706
_refine_ls_number_parameters     122
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0244
_refine_ls_wR_factor_ref         0.0579
_refine_ls_wR_factor_gt          0.0561
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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
Fe1 Fe 0.5000 0.5000 0.5000 0.01175(10) Uani 1 2 d S . .
O1 O 0.17946(16) 0.41483(17) 0.51096(15) 0.0175(2) Uani 1 1 d . . .
O2 O 0.06931(17) 0.45923(19) 0.81240(14) 0.0226(2) Uani 1 1 d . . .
N1 N 0.50397(18) 0.80725(17) 0.50045(14) 0.0138(2) Uani 1 1 d . . .
O3 O 0.19300(19) -0.09039(16) -0.03919(14) 0.0277(3) Uani 1 1 d . . .
N2 N 0.43115(19) 0.37130(17) 0.23587(15) 0.0173(3) Uani 1 1 d . . .
N4 N 0.19846(19) 0.01923(19) -0.12542(15) 0.0203(3) Uani 1 1 d . . .
N3 N 0.2883(2) 0.22991(19) -0.06024(15) 0.0210(3) Uani 1 1 d . . .
O4 O 0.12285(19) -0.05288(18) -0.27225(14) 0.0320(3) Uani 1 1 d . . .
C11 C 0.6301(2) 0.9874(2) 0.60980(17) 0.0158(3) Uani 1 1 d . . .
H11 H 0.7250 0.9839 0.6897 0.019 Uiso 1 1 calc R . .
C10 C 0.3739(2) 0.8214(2) 0.39024(17) 0.0154(3) Uani 1 1 d . . .
H10 H 0.2821 0.6969 0.3101 0.018 Uiso 1 1 calc R . .
C12 C 0.3611(2) 0.2933(2) 0.09853(18) 0.0156(3) Uani 1 1 d . . .
H3 H 0.134(3) 0.424(3) 0.603(3) 0.041(6) Uiso 1 1 d . . .
H4 H 0.095(4) 0.331(4) 0.442(3) 0.042(6) Uiso 1 1 d . . .
H5 H 0.132(4) 0.407(4) 0.851(3) 0.049(7) Uiso 1 1 d . . .
H6 H 0.115(4) 0.587(4) 0.864(3) 0.054(7) 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
Fe1 0.01463(16) 0.00899(14) 0.01053(16) 0.00233(11) -0.00207(10) 0.00367(10)
O1 0.0157(5) 0.0186(5) 0.0138(6) 0.0022(4) -0.0020(5) 0.0038(4)
O2 0.0221(6) 0.0226(6) 0.0180(6) 0.0040(5) -0.0017(4) 0.0037(5)
N1 0.0166(6) 0.0107(5) 0.0140(6) 0.0043(5) -0.0007(5) 0.0046(4)
O3 0.0395(7) 0.0156(5) 0.0238(6) 0.0046(5) 0.0014(5) 0.0059(5)
N2 0.0238(7) 0.0126(5) 0.0138(6) 0.0036(5) -0.0011(5) 0.0052(5)
N4 0.0204(6) 0.0190(6) 0.0131(7) -0.0004(5) 0.0015(5) 0.0017(5)
N3 0.0280(7) 0.0167(6) 0.0112(6) 0.0028(5) -0.0043(5) -0.0001(5)
O4 0.0342(7) 0.0319(6) 0.0122(6) -0.0028(5) -0.0046(5) -0.0014(5)
C11 0.0179(7) 0.0133(6) 0.0146(7) 0.0036(5) -0.0048(5) 0.0045(5)
C10 0.0176(7) 0.0112(6) 0.0143(7) 0.0021(5) -0.0037(5) 0.0031(5)
C12 0.0172(7) 0.0124(6) 0.0170(8) 0.0057(6) 0.0022(6) 0.0040(5)

_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
Fe1 O1 2.0753(10) 2_666 ?
Fe1 O1 2.0753(10) . ?
Fe1 N2 2.1395(12) . ?
Fe1 N2 2.1395(12) 2_666 ?
Fe1 N1 2.1973(10) 2_666 ?
Fe1 N1 2.1973(11) . ?
O1 H3 0.84(2) . ?
O1 H4 0.77(2) . ?
O2 H5 0.78(2) . ?
O2 H6 0.83(3) . ?
N1 C11 1.3367(18) . ?
N1 C10 1.3400(17) . ?
O3 N4 1.2431(17) . ?
N2 C12 1.1522(18) . ?
N4 O4 1.2344(16) . ?
N4 N3 1.3552(17) . ?
N3 C12 1.3272(19) . ?
C11 C10 1.3815(18) 2_676 ?
C11 H11 0.9500 . ?
C10 C11 1.3815(18) 2_676 ?
C10 H10 0.9500 . ?

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 Fe1 O1 180.0 2_666 . ?
O1 Fe1 N2 92.38(5) 2_666 . ?
O1 Fe1 N2 87.62(5) . . ?
O1 Fe1 N2 87.62(5) 2_666 2_666 ?
O1 Fe1 N2 92.38(5) . 2_666 ?
N2 Fe1 N2 180.0 . 2_666 ?
O1 Fe1 N1 89.90(4) 2_666 2_666 ?
O1 Fe1 N1 90.10(4) . 2_666 ?
N2 Fe1 N1 89.21(4) . 2_666 ?
N2 Fe1 N1 90.79(4) 2_666 2_666 ?
O1 Fe1 N1 90.10(4) 2_666 . ?
O1 Fe1 N1 89.90(4) . . ?
N2 Fe1 N1 90.79(4) . . ?
N2 Fe1 N1 89.21(4) 2_666 . ?
N1 Fe1 N1 180.0 2_666 . ?
Fe1 O1 H3 119.4(15) . . ?
Fe1 O1 H4 125.8(17) . . ?
H3 O1 H4 109(2) . . ?
H5 O2 H6 108(2) . . ?
C11 N1 C10 116.59(11) . . ?
C11 N1 Fe1 122.92(9) . . ?
C10 N1 Fe1 120.48(9) . . ?
C12 N2 Fe1 169.02(11) . . ?
O4 N4 O3 123.45(12) . . ?
O4 N4 N3 115.83(12) . . ?
O3 N4 N3 120.72(12) . . ?
C12 N3 N4 111.55(11) . . ?
N1 C11 C10 121.77(12) . 2_676 ?
N1 C11 H11 119.1 . . ?
C10 C11 H11 119.1 2_676 . ?
N1 C10 C11 121.65(12) . 2_676 ?
N1 C10 H10 119.2 . . ?
C11 C10 H10 119.2 2_676 . ?
N2 C12 N3 172.11(14) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H3 O2 0.84(2) 1.81(2) 2.6523(16) 173(2) .
O1 H4 O4 0.77(2) 2.12(2) 2.8767(16) 168(2) 2
O2 H5 N3 0.78(2) 2.19(3) 2.9667(18) 174(2) 1_556
O2 H6 O3 0.83(3) 2.07(3) 2.8918(16) 170(2) 1_566

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.084

data_3Co
_database_code_depnum_ccdc_archive 'CCDC 725140'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
[Co(CAN)2(4,4'-bipy)(H2O)2].4,4'-bipy
;
_chemical_name_common            "[Co(CAN)2(4,4'-bipy)(H2O)2].4,4'-bipy"
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H12 Co N8 O6, C10 H8 N2'
_chemical_formula_sum            'C22 H20 Co N10 O6'
_chemical_formula_weight         579.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   P2/c

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

_cell_length_a                   7.2816(2)
_cell_length_b                   11.3892(2)
_cell_length_c                   15.2587(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.407(1)
_cell_angle_gamma                90.00
_cell_volume                     1235.88(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(1)
_cell_measurement_reflns_used    14072
_cell_measurement_theta_min      3.83
_cell_measurement_theta_max      27.50

_exptl_crystal_description       rods
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             594
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.8337
_exptl_absorpt_correction_T_max  0.9455
_exptl_absorpt_process_details   SORTAV

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(1)
_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  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14072
_diffrn_reflns_av_R_equivalents  0.0879
_diffrn_reflns_av_sigmaI/netI    0.0824
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.83
_diffrn_reflns_theta_max         27.50
_reflns_number_total             2826
_reflns_number_gt                2021
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Hooft, 1999)'
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression ?
_refine_ls_number_reflns         2826
_refine_ls_number_parameters     187
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0594
_refine_ls_wR_factor_ref         0.0899
_refine_ls_wR_factor_gt          0.0801
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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
Co1 Co 0.5000 0.34170(5) 0.2500 0.00869(15) Uani 1 2 d S . .
O10 O 0.9892(3) 0.08870(19) 0.38836(16) 0.0320(6) Uani 1 1 d . . .
N10 N 0.7951(3) 0.3347(2) 0.30641(15) 0.0144(5) Uani 1 1 d . . .
O11 O 1.2700(3) 0.12619(19) 0.46649(15) 0.0285(6) Uani 1 1 d . . .
N11 N 1.0994(3) 0.2752(2) 0.40291(16) 0.0164(6) Uani 1 1 d . . .
C11 C 0.9329(4) 0.3011(2) 0.35085(19) 0.0122(6) Uani 1 1 d . . .
N12 N 1.1173(4) 0.1571(2) 0.41882(16) 0.0207(6) Uani 1 1 d . . .
O20 O 0.4559(3) 0.35011(17) 0.37988(13) 0.0119(4) Uani 1 1 d . . .
N20 N 0.5000 0.5294(3) 0.2500 0.0115(7) Uani 1 2 d S . .
N21 N 0.5000 1.1526(3) 0.2500 0.0120(7) Uani 1 2 d S . .
C21 C 0.5942(4) 0.5906(2) 0.32073(19) 0.0115(6) Uani 1 1 d . . .
H21 H 0.6621 0.5486 0.3711 0.014 Uiso 1 1 calc R . .
C22 C 0.5970(4) 0.7112(2) 0.32376(19) 0.0117(6) Uani 1 1 d . . .
H22 H 0.6645 0.7507 0.3756 0.014 Uiso 1 1 calc R . .
C23 C 0.5000 0.7755(3) 0.2500 0.0109(9) Uani 1 2 d S . .
C24 C 0.5000 0.9058(3) 0.2500 0.0101(9) Uani 1 2 d S . .
C25 C 0.5461(4) 0.9703(2) 0.32923(19) 0.0158(7) Uani 1 1 d . . .
H25 H 0.5775 0.9309 0.3854 0.019 Uiso 1 1 calc R . .
C26 C 0.5460(4) 1.0907(2) 0.32615(19) 0.0163(7) Uani 1 1 d . . .
H26 H 0.5805 1.1324 0.3811 0.020 Uiso 1 1 calc R . .
N30 N 0.2709(3) 0.7086(2) 0.47389(16) 0.0170(6) Uani 1 1 d . . .
C31 C 0.1937(4) 0.8065(3) 0.4345(2) 0.0190(7) Uani 1 1 d . . .
H31 H 0.2133 0.8777 0.4677 0.023 Uiso 1 1 calc R . .
C32 C 0.0861(4) 0.8100(2) 0.3478(2) 0.0163(7) Uani 1 1 d . . .
H32 H 0.0336 0.8822 0.3230 0.020 Uiso 1 1 calc R . .
C33 C 0.0553(4) 0.7076(2) 0.29722(19) 0.0129(6) Uani 1 1 d . . .
C34 C 0.1323(4) 0.6047(3) 0.33875(19) 0.0146(6) Uani 1 1 d . . .
H34 H 0.1128 0.5319 0.3078 0.018 Uiso 1 1 calc R . .
C35 C 0.2378(4) 0.6097(3) 0.4258(2) 0.0174(7) Uani 1 1 d . . .
H35 H 0.2898 0.5387 0.4530 0.021 Uiso 1 1 calc R . .
H2A H 0.537(5) 0.318(3) 0.424(2) 0.031(10) Uiso 1 1 d . . .
H2B H 0.350(6) 0.327(3) 0.391(2) 0.044(12) 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 0.0092(3) 0.0066(3) 0.0091(3) 0.000 -0.0006(2) 0.000
O10 0.0237(14) 0.0172(13) 0.0500(17) 0.0007(11) -0.0033(12) -0.0015(10)
N10 0.0107(12) 0.0139(13) 0.0166(13) 0.0001(11) -0.0012(10) -0.0005(11)
O11 0.0218(13) 0.0370(14) 0.0238(13) 0.0128(10) -0.0015(10) 0.0118(10)
N11 0.0100(13) 0.0171(15) 0.0203(15) 0.0057(10) -0.0009(11) 0.0012(10)
C11 0.0154(16) 0.0100(15) 0.0124(16) -0.0016(11) 0.0052(13) -0.0046(12)
N12 0.0177(14) 0.0255(15) 0.0187(14) 0.0061(12) 0.0034(11) 0.0074(13)
O20 0.0119(11) 0.0141(11) 0.0090(11) 0.0009(8) 0.0008(9) 0.0007(9)
N20 0.0114(19) 0.0103(18) 0.012(2) 0.000 0.0013(15) 0.000
N21 0.0105(17) 0.0120(17) 0.0118(18) 0.000 -0.0013(14) 0.000
C21 0.0117(16) 0.0106(16) 0.0115(16) 0.0015(11) 0.0008(12) -0.0013(11)
C22 0.0090(15) 0.0122(16) 0.0130(16) -0.0025(11) 0.0000(12) -0.0020(11)
C23 0.012(2) 0.007(2) 0.016(2) 0.000 0.0060(18) 0.000
C24 0.008(2) 0.005(2) 0.017(2) 0.000 0.0026(17) 0.000
C25 0.0270(18) 0.0095(16) 0.0099(16) 0.0035(11) 0.0012(13) -0.0002(13)
C26 0.0219(17) 0.0125(16) 0.0114(16) -0.0008(12) -0.0032(13) 0.0011(13)
N30 0.0148(14) 0.0226(14) 0.0124(14) 0.0002(11) 0.0002(11) 0.0015(11)
C31 0.0188(17) 0.0194(17) 0.0177(17) -0.0046(12) 0.0014(13) -0.0011(13)
C32 0.0151(16) 0.0153(17) 0.0164(17) 0.0010(12) -0.0011(13) 0.0012(12)
C33 0.0075(15) 0.0174(15) 0.0141(16) 0.0007(12) 0.0030(12) -0.0008(12)
C34 0.0131(16) 0.0163(16) 0.0139(16) -0.0005(12) 0.0019(13) -0.0010(12)
C35 0.0194(17) 0.0164(16) 0.0154(17) 0.0038(13) 0.0019(13) 0.0032(13)

_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 O20 2.0770(19) . ?
Co1 O20 2.0770(19) 2_655 ?
Co1 N20 2.137(3) . ?
Co1 N10 2.138(2) . ?
Co1 N10 2.138(2) 2_655 ?
Co1 N21 2.154(3) 1_545 ?
O10 N12 1.228(3) . ?
N10 C11 1.149(3) . ?
O11 N12 1.242(3) . ?
N11 C11 1.332(4) . ?
N11 N12 1.367(3) . ?
O20 H2A 0.87(4) . ?
O20 H2B 0.87(4) . ?
N20 C21 1.343(3) . ?
N20 C21 1.343(3) 2_655 ?
N21 C26 1.339(3) 2_655 ?
N21 C26 1.339(3) . ?
N21 Co1 2.154(3) 1_565 ?
C21 C22 1.374(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.400(3) . ?
C22 H22 0.9500 . ?
C23 C22 1.400(3) 2_655 ?
C23 C24 1.484(5) . ?
C24 C25 1.392(3) . ?
C24 C25 1.392(3) 2_655 ?
C25 C26 1.372(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
N30 C31 1.333(4) . ?
N30 C35 1.337(4) . ?
C31 C32 1.386(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.390(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.392(4) . ?
C33 C33 1.492(6) 2 ?
C34 C35 1.386(4) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?

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
O20 Co1 O20 174.71(11) . 2_655 ?
O20 Co1 N20 87.35(6) . . ?
O20 Co1 N20 87.35(6) 2_655 . ?
O20 Co1 N10 88.04(9) . . ?
O20 Co1 N10 92.16(9) 2_655 . ?
N20 Co1 N10 92.14(7) . . ?
O20 Co1 N10 92.16(9) . 2_655 ?
O20 Co1 N10 88.04(9) 2_655 2_655 ?
N20 Co1 N10 92.14(6) . 2_655 ?
N10 Co1 N10 175.72(13) . 2_655 ?
O20 Co1 N21 92.65(6) . 1_545 ?
O20 Co1 N21 92.65(6) 2_655 1_545 ?
N20 Co1 N21 180.000(1) . 1_545 ?
N10 Co1 N21 87.86(6) . 1_545 ?
N10 Co1 N21 87.86(6) 2_655 1_545 ?
C11 N10 Co1 157.7(2) . . ?
C11 N11 N12 111.3(2) . . ?
N10 C11 N11 173.3(3) . . ?
O10 N12 O11 123.6(3) . . ?
O10 N12 N11 121.4(2) . . ?
O11 N12 N11 115.0(3) . . ?
Co1 O20 H2A 120(2) . . ?
Co1 O20 H2B 120(2) . . ?
H2A O20 H2B 101(3) . . ?
C21 N20 C21 117.4(3) . 2_655 ?
C21 N20 Co1 121.31(17) . . ?
C21 N20 Co1 121.31(17) 2_655 . ?
C26 N21 C26 116.4(4) 2_655 . ?
C26 N21 Co1 121.79(18) 2_655 1_565 ?
C26 N21 Co1 121.79(18) . 1_565 ?
N20 C21 C22 123.2(3) . . ?
N20 C21 H21 118.4 . . ?
C22 C21 H21 118.4 . . ?
C21 C22 C23 119.6(3) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C22 C23 C22 116.9(3) 2_655 . ?
C22 C23 C24 121.55(17) 2_655 . ?
C22 C23 C24 121.55(17) . . ?
C25 C24 C25 116.4(4) . 2_655 ?
C25 C24 C23 121.81(18) . . ?
C25 C24 C23 121.81(18) 2_655 . ?
C26 C25 C24 119.9(3) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
N21 C26 C25 123.7(3) . . ?
N21 C26 H26 118.2 . . ?
C25 C26 H26 118.2 . . ?
C31 N30 C35 116.7(2) . . ?
N30 C31 C32 123.5(3) . . ?
N30 C31 H31 118.3 . . ?
C32 C31 H31 118.3 . . ?
C31 C32 C33 119.8(3) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C32 C33 C34 116.9(3) . . ?
C32 C33 C33 121.70(17) . 2 ?
C34 C33 C33 121.38(17) . 2 ?
C35 C34 C33 119.2(3) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
N30 C35 C34 123.9(3) . . ?
N30 C35 H35 118.0 . . ?
C34 C35 H35 118.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O20 H2A N30 0.87(4) 1.88(4) 2.734(3) 164(3) 3_666
O20 H2B N11 0.87(4) 1.96(4) 2.825(3) 174(4) 1_455

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.098

data_3Fe
_database_code_depnum_ccdc_archive 'CCDC 725141'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
{[Fe(CAN)2(4,4'-bipy)(H2O)2].4,4'-bipy}
;
_chemical_name_common            {[Fe(CAN)2(4,4'-bipy)(H2O)2].4,4'-bipy}
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H12 Fe N8 O6, C10 H8 N2'
_chemical_formula_sum            'C22 H20 Fe N10 O6'
_chemical_formula_weight         576.33

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2/c

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

_cell_length_a                   7.2742(1)
_cell_length_b                   11.4850(2)
_cell_length_c                   15.2616(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.364(1)
_cell_angle_gamma                90.00
_cell_volume                     1245.45(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(1)
_cell_measurement_reflns_used    14407
_cell_measurement_theta_min      3.80
_cell_measurement_theta_max      27.50

_exptl_crystal_description       rods
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             592
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.8783
_exptl_absorpt_correction_T_max  0.9364
_exptl_absorpt_process_details   SORTAV

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(1)
_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  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14407
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.80
_diffrn_reflns_theta_max         27.50
_reflns_number_total             2848
_reflns_number_gt                2425
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Hooft, 1999)'
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression ?
_refine_ls_number_reflns         2848
_refine_ls_number_parameters     187
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.0733
_refine_ls_wR_factor_gt          0.0698
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_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
Fe1 Fe 0.5000 0.34115(3) 0.2500 0.00958(10) Uani 1 2 d S . .
N20 N 0.5000 0.53080(18) 0.2500 0.0123(4) Uani 1 2 d S . .
C21 C 0.5936(2) 0.59217(15) 0.32059(12) 0.0127(4) Uani 1 1 d . . .
H21 H 0.6615 0.5506 0.3711 0.015 Uiso 1 1 calc R . .
N21 N 0.5000 1.14965(18) 0.2500 0.0131(4) Uani 1 2 d S . .
C23 C 0.5000 0.7758(2) 0.2500 0.0122(5) Uani 1 2 d S . .
C24 C 0.5000 0.9049(2) 0.2500 0.0120(5) Uani 1 2 d S . .
C25 C 0.5435(3) 0.96831(16) 0.32954(12) 0.0180(4) Uani 1 1 d . . .
H25 H 0.5732 0.9292 0.3857 0.022 Uiso 1 1 calc R . .
C22 C 0.5965(2) 0.71227(15) 0.32371(12) 0.0129(4) Uani 1 1 d . . .
H22 H 0.6637 0.7515 0.3756 0.016 Uiso 1 1 calc R . .
C26 C 0.5433(3) 1.08817(16) 0.32612(12) 0.0174(4) Uani 1 1 d . . .
H26 H 0.5757 1.1297 0.3811 0.021 Uiso 1 1 calc R . .
O20 O 0.4567(2) 0.34898(11) 0.38116(8) 0.0133(3) Uani 1 1 d . . .
H2B H 0.358(4) 0.328(2) 0.3881(16) 0.030(7) Uiso 1 1 d . . .
H2A H 0.546(4) 0.322(2) 0.4281(19) 0.048(8) Uiso 1 1 d . . .
N10 N 0.7985(2) 0.33329(13) 0.30644(10) 0.0161(3) Uani 1 1 d . . .
N11 N 1.1011(2) 0.27256(14) 0.40378(11) 0.0184(4) Uani 1 1 d . . .
C11 C 0.9360(2) 0.29901(15) 0.35122(12) 0.0141(4) Uani 1 1 d . . .
N12 N 1.1186(2) 0.15490(15) 0.41925(11) 0.0202(4) Uani 1 1 d . . .
O11 O 1.2705(2) 0.12380(13) 0.46653(10) 0.0303(4) Uani 1 1 d . . .
O10 O 0.9898(2) 0.08791(12) 0.38776(11) 0.0331(4) Uani 1 1 d . . .
C34 C 0.1324(2) 0.60528(16) 0.33850(12) 0.0155(4) Uani 1 1 d . . .
H34 H 0.1133 0.5332 0.3073 0.019 Uiso 1 1 calc R . .
C35 C 0.2375(3) 0.60991(17) 0.42535(12) 0.0179(4) Uani 1 1 d . . .
H35 H 0.2892 0.5394 0.4524 0.021 Uiso 1 1 calc R . .
N30 N 0.2707(2) 0.70806(14) 0.47363(10) 0.0174(3) Uani 1 1 d . . .
C32 C 0.0854(3) 0.80936(16) 0.34769(12) 0.0168(4) Uani 1 1 d . . .
H32 H 0.0327 0.8809 0.3230 0.020 Uiso 1 1 calc R . .
C33 C 0.0548(2) 0.70763(16) 0.29708(12) 0.0133(4) Uani 1 1 d . . .
C31 C 0.1933(3) 0.80584(17) 0.43440(13) 0.0196(4) Uani 1 1 d . . .
H31 H 0.2132 0.8764 0.4676 0.023 Uiso 1 1 calc R . .

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
Fe1 0.00994(18) 0.00674(18) 0.01107(18) 0.000 0.00006(13) 0.000
N20 0.0121(10) 0.0101(11) 0.0146(11) 0.000 0.0026(8) 0.000
C21 0.0130(9) 0.0110(9) 0.0134(9) 0.0015(7) 0.0016(7) 0.0008(6)
N21 0.0115(10) 0.0101(11) 0.0167(11) 0.000 0.0009(8) 0.000
C23 0.0121(12) 0.0095(13) 0.0164(13) 0.000 0.0061(10) 0.000
C24 0.0106(12) 0.0082(13) 0.0170(13) 0.000 0.0024(10) 0.000
C25 0.0280(10) 0.0120(10) 0.0125(9) 0.0020(7) 0.0008(8) 0.0014(8)
C22 0.0126(9) 0.0125(9) 0.0135(9) -0.0021(7) 0.0022(7) -0.0010(7)
C26 0.0246(10) 0.0122(10) 0.0133(9) -0.0020(7) -0.0007(7) 0.0010(7)
O20 0.0124(7) 0.0140(7) 0.0129(6) 0.0004(5) 0.0014(5) -0.0010(5)
N10 0.0139(8) 0.0132(8) 0.0202(8) 0.0005(6) 0.0015(6) -0.0008(6)
N11 0.0133(8) 0.0193(9) 0.0208(9) 0.0045(7) -0.0007(6) 0.0010(6)
C11 0.0139(9) 0.0134(9) 0.0158(9) -0.0007(7) 0.0045(7) -0.0031(7)
N12 0.0174(8) 0.0243(9) 0.0196(8) 0.0058(7) 0.0052(7) 0.0056(7)
O11 0.0216(8) 0.0401(9) 0.0268(8) 0.0143(7) 0.0002(6) 0.0133(6)
O10 0.0251(8) 0.0180(8) 0.0522(11) 0.0006(7) -0.0007(7) -0.0011(6)
C34 0.0141(9) 0.0162(10) 0.0159(9) -0.0002(7) 0.0025(7) -0.0008(7)
C35 0.0176(10) 0.0195(10) 0.0161(9) 0.0042(8) 0.0025(7) 0.0033(8)
N30 0.0154(8) 0.0230(9) 0.0131(8) -0.0009(6) 0.0014(6) 0.0005(6)
C32 0.0179(9) 0.0156(10) 0.0160(10) 0.0009(7) 0.0015(7) 0.0019(7)
C33 0.0089(8) 0.0174(9) 0.0136(9) 0.0004(7) 0.0024(7) -0.0012(7)
C31 0.0205(10) 0.0202(10) 0.0169(10) -0.0039(8) 0.0014(8) -0.0009(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
Fe1 O20 2.0938(13) . ?
Fe1 O20 2.0938(13) 2_655 ?
Fe1 N10 2.1593(15) 2_655 ?
Fe1 N10 2.1593(15) . ?
Fe1 N20 2.178(2) . ?
Fe1 N21 2.199(2) 1_545 ?
N20 C21 1.344(2) . ?
N20 C21 1.344(2) 2_655 ?
C21 C22 1.380(3) . ?
C21 H21 0.9500 . ?
N21 C26 1.338(2) 2_655 ?
N21 C26 1.338(2) . ?
N21 Fe1 2.199(2) 1_565 ?
C23 C22 1.398(2) 2_655 ?
C23 C22 1.398(2) . ?
C23 C24 1.482(3) . ?
C24 C25 1.393(2) . ?
C24 C25 1.393(2) 2_655 ?
C25 C26 1.378(3) . ?
C25 H25 0.9500 . ?
C22 H22 0.9500 . ?
C26 H26 0.9500 . ?
O20 H2B 0.79(3) . ?
O20 H2A 0.91(3) . ?
N10 C11 1.154(2) . ?
N11 C11 1.328(2) . ?
N11 N12 1.373(2) . ?
N12 O10 1.228(2) . ?
N12 O11 1.236(2) . ?
C34 C35 1.382(2) . ?
C34 C33 1.396(3) . ?
C34 H34 0.9500 . ?
C35 N30 1.340(2) . ?
C35 H35 0.9500 . ?
N30 C31 1.339(3) . ?
C32 C31 1.387(3) . ?
C32 C33 1.392(3) . ?
C32 H32 0.9500 . ?
C33 C33 1.487(3) 2 ?
C31 H31 0.9500 . ?

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
O20 Fe1 O20 175.08(7) . 2_655 ?
O20 Fe1 N10 92.23(6) . 2_655 ?
O20 Fe1 N10 87.97(6) 2_655 2_655 ?
O20 Fe1 N10 87.97(6) . . ?
O20 Fe1 N10 92.23(6) 2_655 . ?
N10 Fe1 N10 175.21(8) 2_655 . ?
O20 Fe1 N20 87.54(4) . . ?
O20 Fe1 N20 87.54(4) 2_655 . ?
N10 Fe1 N20 92.40(4) 2_655 . ?
N10 Fe1 N20 92.40(4) . . ?
O20 Fe1 N21 92.46(4) . 1_545 ?
O20 Fe1 N21 92.46(4) 2_655 1_545 ?
N10 Fe1 N21 87.60(4) 2_655 1_545 ?
N10 Fe1 N21 87.60(4) . 1_545 ?
N20 Fe1 N21 180.0 . 1_545 ?
C21 N20 C21 116.8(2) . 2_655 ?
C21 N20 Fe1 121.62(11) . . ?
C21 N20 Fe1 121.62(11) 2_655 . ?
N20 C21 C22 123.57(17) . . ?
N20 C21 H21 118.2 . . ?
C22 C21 H21 118.2 . . ?
C26 N21 C26 116.3(2) 2_655 . ?
C26 N21 Fe1 121.85(11) 2_655 1_565 ?
C26 N21 Fe1 121.85(11) . 1_565 ?
C22 C23 C22 117.0(2) 2_655 . ?
C22 C23 C24 121.49(11) 2_655 . ?
C22 C23 C24 121.49(11) . . ?
C25 C24 C25 117.0(2) . 2_655 ?
C25 C24 C23 121.52(11) . . ?
C25 C24 C23 121.52(11) 2_655 . ?
C26 C25 C24 119.42(18) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C21 C22 C23 119.54(17) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
N21 C26 C25 123.94(18) . . ?
N21 C26 H26 118.0 . . ?
C25 C26 H26 118.0 . . ?
Fe1 O20 H2B 116.3(17) . . ?
Fe1 O20 H2A 120.7(17) . . ?
H2B O20 H2A 108(2) . . ?
C11 N10 Fe1 157.10(14) . . ?
C11 N11 N12 111.56(15) . . ?
N10 C11 N11 173.23(19) . . ?
O10 N12 O11 123.99(17) . . ?
O10 N12 N11 120.98(15) . . ?
O11 N12 N11 115.03(16) . . ?
C35 C34 C33 119.28(17) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
N30 C35 C34 123.87(17) . . ?
N30 C35 H35 118.1 . . ?
C34 C35 H35 118.1 . . ?
C31 N30 C35 116.79(16) . . ?
C31 C32 C33 119.71(17) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C32 C33 C34 117.03(16) . . ?
C32 C33 C33 121.70(11) . 2 ?
C34 C33 C33 121.27(11) . 2 ?
N30 C31 C32 123.30(18) . . ?
N30 C31 H31 118.4 . . ?
C32 C31 H31 118.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O20 H2B N11 0.79(3) 2.03(3) 2.822(2) 179(3) 1_455
O20 H2A N30 0.91(3) 1.82(3) 2.718(2) 171(2) 3_666

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.060

data_3Mn
_database_code_depnum_ccdc_archive 'CCDC 725142'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
{[Mn(CAN)2(4,4'-bipy)(H2O)2].4,4'-bipy}
;
_chemical_name_common            {[Mn(CAN)2(4,4'-bipy)(H2O)2].4,4'-bipy}
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H12 Mn N8 O6, (C10 H8 N2)'
_chemical_formula_sum            'C22 H20 Mn N10 O6'
_chemical_formula_weight         575.42

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   P2/c

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

_cell_length_a                   7.3102(1)
_cell_length_b                   11.5900(2)
_cell_length_c                   15.2784(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.865(1)
_cell_angle_gamma                90.00
_cell_volume                     1266.81(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(1)
_cell_measurement_reflns_used    14237
_cell_measurement_theta_min      3.77
_cell_measurement_theta_max      27.50

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             590
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.8451
_exptl_absorpt_correction_T_max  0.9442
_exptl_absorpt_process_details   SORTAV

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(1)
_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  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14237
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.77
_diffrn_reflns_theta_max         27.50
_reflns_number_total             2899
_reflns_number_gt                2125
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Hooft, 1999)'
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression ?
_refine_ls_number_reflns         2899
_refine_ls_number_parameters     187
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.1013
_refine_ls_wR_factor_gt          0.0893
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.5000 0.34288(3) 0.2500 0.01332(14) Uani 1 2 d S . .
N20 N 0.5000 0.53633(18) 0.2500 0.0154(5) Uani 1 2 d S . .
C21 C 0.5915(2) 0.59692(16) 0.32069(12) 0.0161(4) Uani 1 1 d . . .
H21 H 0.6571 0.5557 0.3712 0.019 Uiso 1 1 calc R . .
N21 N 0.5000 1.14855(17) 0.2500 0.0152(5) Uani 1 2 d S . .
C23 C 0.5000 0.7785(2) 0.2500 0.0133(5) Uani 1 2 d S . .
C24 C 0.5000 0.9068(2) 0.2500 0.0149(5) Uani 1 2 d S . .
C25 C 0.5385(3) 0.96904(16) 0.32917(12) 0.0204(4) Uani 1 1 d . . .
H25 H 0.5650 0.9300 0.3850 0.025 Uiso 1 1 calc R . .
C22 C 0.5948(2) 0.71575(15) 0.32355(12) 0.0153(4) Uani 1 1 d . . .
H22 H 0.6610 0.7547 0.3751 0.018 Uiso 1 1 calc R . .
C26 C 0.5382(3) 1.08817(16) 0.32633(12) 0.0211(4) Uani 1 1 d . . .
H26 H 0.5666 1.1293 0.3812 0.025 Uiso 1 1 calc R . .
O20 O 0.4553(2) 0.35111(11) 0.38644(9) 0.0169(3) Uani 1 1 d . . .
H2B H 0.353(4) 0.3288(19) 0.4002(16) 0.038(7) Uiso 1 1 d . . .
H2A H 0.550(3) 0.321(2) 0.4300(17) 0.045(7) Uiso 1 1 d . . .
N10 N 0.8058(2) 0.33806(13) 0.30806(11) 0.0208(4) Uani 1 1 d . . .
N11 N 1.1000(2) 0.27189(14) 0.40653(11) 0.0223(4) Uani 1 1 d . . .
C11 C 0.9389(3) 0.30091(17) 0.35320(13) 0.0180(4) Uani 1 1 d . . .
N12 N 1.1141(2) 0.15491(14) 0.41973(11) 0.0236(4) Uani 1 1 d . . .
O11 O 1.2621(2) 0.12197(14) 0.46767(10) 0.0350(4) Uani 1 1 d . . .
O10 O 0.9856(2) 0.09028(13) 0.38576(11) 0.0376(4) Uani 1 1 d . . .
C34 C 0.1309(2) 0.60987(17) 0.33786(12) 0.0184(4) Uani 1 1 d . . .
H34 H 0.1117 0.5385 0.3068 0.022 Uiso 1 1 calc R . .
C35 C 0.2348(3) 0.61456(17) 0.42412(13) 0.0206(4) Uani 1 1 d . . .
H35 H 0.2861 0.5446 0.4510 0.025 Uiso 1 1 calc R . .
N30 N 0.2677(2) 0.71159(14) 0.47225(10) 0.0215(4) Uani 1 1 d . . .
C32 C 0.0846(3) 0.81215(17) 0.34767(13) 0.0208(4) Uani 1 1 d . . .
H32 H 0.0323 0.8831 0.3233 0.025 Uiso 1 1 calc R . .
C33 C 0.0544(2) 0.71146(16) 0.29692(12) 0.0158(4) Uani 1 1 d . . .
C31 C 0.1910(3) 0.80843(18) 0.43360(13) 0.0221(4) Uani 1 1 d . . .
H31 H 0.2106 0.8782 0.4669 0.027 Uiso 1 1 calc R . .

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 0.0158(2) 0.0081(2) 0.0147(2) 0.000 -0.00004(16) 0.000
N20 0.0202(11) 0.0102(11) 0.0162(11) 0.000 0.0049(9) 0.000
C21 0.0196(9) 0.0129(10) 0.0151(10) -0.0001(7) 0.0017(8) -0.0007(7)
N21 0.0180(11) 0.0098(11) 0.0167(11) 0.000 0.0009(9) 0.000
C23 0.0152(12) 0.0102(13) 0.0154(13) 0.000 0.0051(10) 0.000
C24 0.0137(12) 0.0131(13) 0.0174(14) 0.000 0.0022(10) 0.000
C25 0.0322(10) 0.0132(10) 0.0139(10) 0.0017(8) 0.0001(8) 0.0003(8)
C22 0.0169(9) 0.0133(10) 0.0148(10) -0.0012(7) 0.0008(8) -0.0017(7)
C26 0.0333(11) 0.0133(10) 0.0146(10) -0.0022(8) 0.0001(8) 0.0003(8)
O20 0.0168(7) 0.0175(7) 0.0152(7) 0.0011(6) 0.0004(6) -0.0003(6)
N10 0.0166(8) 0.0193(9) 0.0250(9) 0.0011(7) 0.0007(7) -0.0014(7)
N11 0.0172(8) 0.0224(9) 0.0251(9) 0.0041(7) -0.0009(7) 0.0008(7)
C11 0.0195(10) 0.0164(10) 0.0189(10) -0.0003(8) 0.0059(8) -0.0041(8)
N12 0.0231(9) 0.0252(10) 0.0227(9) 0.0050(8) 0.0050(8) 0.0040(7)
O11 0.0285(8) 0.0438(10) 0.0303(9) 0.0158(7) 0.0002(7) 0.0157(7)
O10 0.0333(9) 0.0214(8) 0.0538(11) 0.0000(8) -0.0011(8) 0.0002(7)
C34 0.0187(10) 0.0161(10) 0.0193(10) -0.0003(8) 0.0011(8) -0.0001(8)
C35 0.0210(10) 0.0209(10) 0.0182(10) 0.0039(8) 0.0002(8) 0.0033(8)
N30 0.0207(8) 0.0252(10) 0.0173(9) 0.0006(7) 0.0008(7) 0.0004(7)
C32 0.0224(10) 0.0181(10) 0.0206(11) -0.0001(8) 0.0010(8) 0.0013(8)
C33 0.0143(9) 0.0185(10) 0.0147(10) -0.0001(8) 0.0035(8) -0.0023(8)
C31 0.0231(10) 0.0228(10) 0.0195(10) -0.0048(9) 0.0021(8) -0.0009(9)

_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 O20 2.1775(13) 2_655 ?
Mn1 O20 2.1775(13) . ?
Mn1 N10 2.2298(15) . ?
Mn1 N10 2.2298(15) 2_655 ?
Mn1 N20 2.242(2) . ?
Mn1 N21 2.252(2) 1_545 ?
N20 C21 1.345(2) . ?
N20 C21 1.345(2) 2_655 ?
C21 C22 1.378(3) . ?
C21 H21 0.9500 . ?
N21 C26 1.339(2) 2_655 ?
N21 C26 1.339(2) . ?
N21 Mn1 2.252(2) 1_565 ?
C23 C22 1.397(2) 2_655 ?
C23 C22 1.397(2) . ?
C23 C24 1.487(4) . ?
C24 C25 1.387(2) . ?
C24 C25 1.387(2) 2_655 ?
C25 C26 1.381(3) . ?
C25 H25 0.9500 . ?
C22 H22 0.9500 . ?
C26 H26 0.9500 . ?
O20 H2B 0.86(3) . ?
O20 H2A 0.92(2) . ?
N10 C11 1.154(2) . ?
N11 C11 1.330(2) . ?
N11 N12 1.371(2) . ?
N12 O10 1.230(2) . ?
N12 O11 1.236(2) . ?
C34 C35 1.380(3) . ?
C34 C33 1.395(3) . ?
C34 H34 0.9500 . ?
C35 N30 1.338(3) . ?
C35 H35 0.9500 . ?
N30 C31 1.337(2) . ?
C32 C31 1.382(3) . ?
C32 C33 1.393(3) . ?
C32 H32 0.9500 . ?
C33 C33 1.490(4) 2 ?
C31 H31 0.9500 . ?

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
O20 Mn1 O20 174.98(7) 2_655 . ?
O20 Mn1 N10 92.66(6) 2_655 . ?
O20 Mn1 N10 87.47(6) . . ?
O20 Mn1 N10 87.47(6) 2_655 2_655 ?
O20 Mn1 N10 92.66(6) . 2_655 ?
N10 Mn1 N10 177.13(8) . 2_655 ?
O20 Mn1 N20 87.49(3) 2_655 . ?
O20 Mn1 N20 87.49(3) . . ?
N10 Mn1 N20 91.43(4) . . ?
N10 Mn1 N20 91.43(4) 2_655 . ?
O20 Mn1 N21 92.51(3) 2_655 1_545 ?
O20 Mn1 N21 92.51(3) . 1_545 ?
N10 Mn1 N21 88.57(4) . 1_545 ?
N10 Mn1 N21 88.57(4) 2_655 1_545 ?
N20 Mn1 N21 180.0 . 1_545 ?
C21 N20 C21 117.1(2) . 2_655 ?
C21 N20 Mn1 121.47(11) . . ?
C21 N20 Mn1 121.47(11) 2_655 . ?
N20 C21 C22 123.35(17) . . ?
N20 C21 H21 118.3 . . ?
C22 C21 H21 118.3 . . ?
C26 N21 C26 117.0(2) 2_655 . ?
C26 N21 Mn1 121.50(11) 2_655 1_565 ?
C26 N21 Mn1 121.50(11) . 1_565 ?
C22 C23 C22 117.3(2) 2_655 . ?
C22 C23 C24 121.37(11) 2_655 . ?
C22 C23 C24 121.37(11) . . ?
C25 C24 C25 117.3(2) . 2_655 ?
C25 C24 C23 121.35(12) . . ?
C25 C24 C23 121.35(12) 2_655 . ?
C26 C25 C24 119.60(18) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C21 C22 C23 119.48(17) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
N21 C26 C25 123.24(18) . . ?
N21 C26 H26 118.4 . . ?
C25 C26 H26 118.4 . . ?
Mn1 O20 H2B 122.1(16) . . ?
Mn1 O20 H2A 115.9(15) . . ?
H2B O20 H2A 106(2) . . ?
C11 N10 Mn1 154.17(15) . . ?
C11 N11 N12 111.74(16) . . ?
N10 C11 N11 172.7(2) . . ?
O10 N12 O11 124.16(18) . . ?
O10 N12 N11 120.82(16) . . ?
O11 N12 N11 115.02(16) . . ?
C35 C34 C33 119.08(18) . . ?
C35 C34 H34 120.5 . . ?
C33 C34 H34 120.5 . . ?
N30 C35 C34 124.00(18) . . ?
N30 C35 H35 118.0 . . ?
C34 C35 H35 118.0 . . ?
C31 N30 C35 116.83(17) . . ?
C31 C32 C33 119.76(18) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C34 C33 C32 117.02(17) . . ?
C34 C33 C33 121.13(11) . 2 ?
C32 C33 C33 121.86(11) . 2 ?
N30 C31 C32 123.28(19) . . ?
N30 C31 H31 118.4 . . ?
C32 C31 H31 118.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O20 H2B N11 0.86(3) 1.98(3) 2.830(2) 169(2) 1_455
O20 H2A N30 0.92(2) 1.83(3) 2.737(2) 169(2) 3_666

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.105


