# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               Inorg.Chem.

_journal_coden_Cambridge         0009
_journal_year                    2004
_journal_volume                  43
_journal_page_first              4615
_publ_contact_author_name        'Song Gao'
_publ_contact_author_email       gaosong@pku.edu.cn
loop_
_publ_author_name
'Xin-Yi Wang'
'Lin Gan'
'Shi-Wei Zhang'
'Song Gao'

data_Mn(CHOO)3-NH2(CH3)2
_database_code_depnum_ccdc_archive 'CCDC 246991'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         Mn(CHOO)3-NH2(CH3)2
_chemical_formula_sum            'C5 H11 Mn N O6'
_chemical_formula_weight         236.09

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R-3c

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

_cell_length_a                   8.3340(12)
_cell_length_b                   8.3340(12)
_cell_length_c                   22.893(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1377.0(4)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5103
_cell_measurement_theta_min      3.34
_cell_measurement_theta_max      30.45

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             726
_exptl_absorpt_coefficient_mu    1.437
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.484
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
ABSCOR by T.Higashi    8 March, 1995
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaka RAXIS RAPID IP'
_diffrn_measurement_method       OSCILLATIOn
_diffrn_detector_area_resol_mean '100x100 microns'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5103
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         30.45
_reflns_number_total             467
_reflns_number_gt                383
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
Molecular Structure Corporation (1994) MSC/AFC Diffractometer
Control Software MSC, 3200 Research Forest Drive, The Woodlands,
TX 77381, USA.
;
_computing_cell_refinement       
;
Molecular Structure Corporation (1994) MSC/AFC Diffractometer
Control Software MSC, 3200 Research Forest Drive, The Woodlands,
TX 77381, USA.
;
_computing_data_reduction        
;
Sheldrick, G. M. (1997) SHELXS97, Program for the Solution
of Crystal Structure,University of Gottingen, Germany.
;
_computing_structure_solution    
;
Sheldrick, G. M. (1997) SHELXS97, Program for the Solution
of Crystal Structure,University of Gottingen, Germany.
;
_computing_structure_refinement  
;
Sheldrick, G. M. (1997) SHELXL97, Program for the Refinement
of Crystal Structure,University of Gottingen, Germany.
;
_computing_molecular_graphics    
;
Interactive Molecular Graphics XP, Virsion 4.2 for MSDOS (1990),
Siemens AnalyticalX-ray Instruments Inc., Madison, Wisconsin,USA.
;
_computing_publication_material  
;
Sheldrick, G. M. (1997) SHELXL97, Program for the refinement
of Crystal Structure,University of Gottingen, Germany.
;

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0122(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         467
_refine_ls_number_parameters     28
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0240
_refine_ls_wR_factor_ref         0.0600
_refine_ls_wR_factor_gt          0.0586
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_restrained_S_all      0.969
_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 0.0000 0.0000 0.0000 0.02238(19) Uani 1 6 d S . .
O1 O 0.22092(13) 0.21080(13) 0.05426(4) 0.0382(3) Uani 1 1 d . . .
N N 0.5804(6) 0.2471(6) 0.0833 0.0418(14) Uani 0.33 2 d SP . .
C1 C 0.2155(3) 0.3333 0.0833 0.0312(4) Uani 1 2 d S . .
C2 C 0.6667 0.3333 0.03002(17) 0.0615(9) Uani 1 3 d S . .
H1 H 0.109(4) 0.3333 0.0833 0.056(8) Uiso 1 2 d S . .

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 0.0221(2) 0.0221(2) 0.0230(3) 0.000 0.000 0.01104(10)
O1 0.0339(5) 0.0351(5) 0.0453(6) -0.0157(4) -0.0085(4) 0.0170(4)
N 0.0297(19) 0.0297(19) 0.068(4) 0.0022(12) -0.0022(12) 0.016(2)
C1 0.0282(6) 0.0283(9) 0.0372(11) -0.0017(8) -0.0009(4) 0.0141(5)
C2 0.0697(13) 0.0697(13) 0.0450(18) 0.000 0.000 0.0348(7)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1 2.1874(9) . ?
Mn1 O1 2.1874(9) 19 ?
Mn1 O1 2.1874(9) 21 ?
Mn1 O1 2.1874(9) 2 ?
Mn1 O1 2.1874(9) 20 ?
Mn1 O1 2.1874(9) 3 ?
O1 C1 1.2385(13) . ?
N N 1.245(9) 2_655 ?
N N 1.245(9) 3_665 ?
N C2 1.416(4) . ?
N C2 1.416(4) 16_544 ?
C1 O1 1.2385(13) 17_554 ?
C2 N 1.416(4) 2_655 ?
C2 N 1.416(4) 3_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
O1 Mn1 O1 180.00(4) . 19 ?
O1 Mn1 O1 89.07(4) . 21 ?
O1 Mn1 O1 90.93(4) 19 21 ?
O1 Mn1 O1 90.93(4) . 2 ?
O1 Mn1 O1 89.07(4) 19 2 ?
O1 Mn1 O1 89.07(4) 21 2 ?
O1 Mn1 O1 89.07(4) . 20 ?
O1 Mn1 O1 90.93(4) 19 20 ?
O1 Mn1 O1 90.93(4) 21 20 ?
O1 Mn1 O1 180.00(5) 2 20 ?
O1 Mn1 O1 90.93(4) . 3 ?
O1 Mn1 O1 89.07(4) 19 3 ?
O1 Mn1 O1 180.00(5) 21 3 ?
O1 Mn1 O1 90.93(4) 2 3 ?
O1 Mn1 O1 89.07(4) 20 3 ?
C1 O1 Mn1 127.18(11) . . ?
N N N 60.000(1) 2_655 3_665 ?
N N C2 63.92(17) 2_655 . ?
N N C2 63.92(17) 3_665 . ?
N N C2 63.92(17) 2_655 16_544 ?
N N C2 63.92(17) 3_665 16_544 ?
C2 N C2 119.0(4) . 16_544 ?
O1 C1 O1 126.7(2) . 17_554 ?
N C2 N 52.2(3) 2_655 . ?
N C2 N 52.2(3) 2_655 3_665 ?
N C2 N 52.2(3) . 3_665 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        30.45
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.067

#===END

data_Co(CHOO)3.(NH2(CH3)2)
_database_code_depnum_ccdc_archive 'CCDC 246992'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         Co(CHOO)3.(NH2(CH3)2)
_chemical_formula_sum            'C5 H11 Co N O6'
_chemical_formula_weight         240.08

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           trigonal
_symmetry_space_group_name_H-M   R-3c

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

_cell_length_a                   8.1989(12)
_cell_length_b                   8.1989(12)
_cell_length_c                   22.224(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1293.8(4)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5202
_cell_measurement_theta_min      4.66
_cell_measurement_theta_max      30.44

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             738
_exptl_absorpt_coefficient_mu    1.989
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
ABSCOR by T.Higashi    8 March, 1995
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_detector_area_resol_mean '100x100 microns'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5202
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         4.66
_diffrn_reflns_theta_max         30.44
_reflns_number_total             442
_reflns_number_gt                337
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
Molecular Structure Corporation (1994) MSC/AFC Diffractometer
Control Software MSC, 3200 Research Forest Drive, The Woodlands,
TX 77381, USA.
;
_computing_cell_refinement       
;
Molecular Structure Corporation (1994) MSC/AFC Diffractometer
Control Software MSC, 3200 Research Forest Drive, The Woodlands,
TX 77381, USA.'
;
_computing_data_reduction        
;
Sheldrick, G. M. (1997) SHELXS97, Program for the Solution
of Crystal Structure,University of Gottingen, Germany.
;
_computing_structure_solution    
;
Sheldrick, G. M. (1997) SHELXS97, Program for the Solution
of Crystal Structure,University of Gottingen, Germany.
;
_computing_structure_refinement  
;
Sheldrick, G. M. (1997) SHELXL97, Program for the Refinement
of Crystal Structure,University of Gottingen, Germany.
;
_computing_molecular_graphics    
;
Interactive Molecular Graphics XP, Virsion 4.2 for MSDOS (1990),
Siemens AnalyticalX-ray Instruments Inc., Madison, Wisconsin,USA.
;
_computing_publication_material  
;
Sheldrick, G. M. (1997) SHELXL97, Program for the refinement
of Crystal Structure,University of Gottingen, Germany.'
;

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0127P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0067(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         442
_refine_ls_number_parameters     26
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0247
_refine_ls_wR_factor_ref         0.0448
_refine_ls_wR_factor_gt          0.0438
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_restrained_S_all      0.877
_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 0.3333 0.6667 0.1667 0.01612(17) Uani 1 6 d S . .
O1 O 0.34145(15) 0.45821(14) 0.11327(4) 0.0269(3) Uani 1 1 d . . .
N1 N 0.6667 0.4210(7) 0.0833 0.0326(13) Uani 0.33 2 d SP . .
C1 C 0.2090(2) 0.3333 0.0833 0.0229(5) Uani 1 2 d S . .
H1 H 0.0956 0.3333 0.0833 0.028 Uiso 1 2 calc SR . .
C2 C 0.6667 0.3333 0.13830(13) 0.0524(9) Uani 1 3 d S . .

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 0.01635(19) 0.01635(19) 0.0156(2) 0.000 0.000 0.00818(9)
O1 0.0252(5) 0.0255(6) 0.0304(5) -0.0099(4) -0.0046(4) 0.0128(5)
N1 0.028(3) 0.025(2) 0.046(3) 0.0035(12) 0.007(2) 0.0138(15)
C1 0.0211(8) 0.0221(11) 0.0259(9) -0.0001(8) 0.0000(4) 0.0110(5)
C2 0.0631(14) 0.0631(14) 0.0310(14) 0.000 0.000 0.0315(7)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.1089(10) 25_565 ?
Co1 O1 2.1089(10) 26_455 ?
Co1 O1 2.1089(10) 27 ?
Co1 O1 2.1088(10) 3_565 ?
Co1 O1 2.1088(10) 2_665 ?
Co1 O1 2.1088(10) . ?
O1 C1 1.2483(14) . ?
N1 N1 1.245(10) 2_655 ?
N1 N1 1.245(10) 3_665 ?
N1 C2 1.417(4) 16_544 ?
N1 C2 1.417(4) . ?
C1 O1 1.2483(14) 17_554 ?
C2 N1 1.417(4) 3_665 ?
C2 N1 1.417(4) 2_655 ?

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 91.44(4) 25_565 26_455 ?
O1 Co1 O1 91.44(4) 25_565 27 ?
O1 Co1 O1 91.44(4) 26_455 27 ?
O1 Co1 O1 88.56(4) 25_565 3_565 ?
O1 Co1 O1 88.56(4) 26_455 3_565 ?
O1 Co1 O1 180.0 27 3_565 ?
O1 Co1 O1 88.56(4) 25_565 2_665 ?
O1 Co1 O1 180.0 26_455 2_665 ?
O1 Co1 O1 88.56(4) 27 2_665 ?
O1 Co1 O1 91.44(4) 3_565 2_665 ?
O1 Co1 O1 180.0 25_565 . ?
O1 Co1 O1 88.56(4) 26_455 . ?
O1 Co1 O1 88.56(4) 27 . ?
O1 Co1 O1 91.44(4) 3_565 . ?
O1 Co1 O1 91.44(4) 2_665 . ?
C1 O1 Co1 126.71(11) . . ?
N1 N1 N1 60.0 2_655 3_665 ?
N1 N1 C2 63.95(17) 2_655 16_544 ?
N1 N1 C2 63.95(17) 3_665 16_544 ?
N1 N1 C2 63.95(17) 2_655 . ?
N1 N1 C2 63.95(17) 3_665 . ?
C2 N1 C2 119.1(4) 16_544 . ?
O1 C1 O1 125.27(19) 17_554 . ?
N1 C2 N1 52.1(3) 3_665 2_655 ?
N1 C2 N1 52.1(3) 3_665 . ?
N1 C2 N1 52.1(3) 2_655 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Co1 O1 C1 74(4) 25_565 . . . ?
O1 Co1 O1 C1 61.53(5) 26_455 . . . ?
O1 Co1 O1 C1 153.01(9) 27 . . . ?
O1 Co1 O1 C1 -26.99(9) 3_565 . . . ?
O1 Co1 O1 C1 -118.47(5) 2_665 . . . ?
Co1 O1 C1 O1 -177.95(9) . . . 17_554 ?
N1 N1 C2 N1 67.63(11) 2_655 . . 3_665 ?
C2 N1 C2 N1 33.82(6) 16_544 . . 3_665 ?
N1 N1 C2 N1 -67.63(11) 3_665 . . 2_655 ?
C2 N1 C2 N1 -33.82(6) 16_544 . . 2_655 ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        30.44
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.070

#===END

data_Ni(CHOO)3-NH2(CH3)2
_database_code_depnum_ccdc_archive 'CCDC 246993'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         Ni(CHOO)3-NH2(CH3)2
_chemical_formula_sum            'C5 H11 N Ni O6'
_chemical_formula_weight         239.86

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R-3c

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

_cell_length_a                   8.1989(12)
_cell_length_b                   8.1989(12)
_cell_length_c                   22.224(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1293.8(4)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3708
_cell_measurement_theta_min      3.41
_cell_measurement_theta_max      30.24

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             744
_exptl_absorpt_coefficient_mu    2.249
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.510
_exptl_absorpt_correction_T_max  0.570

_exptl_special_details           
;
ABSCOR by T.Higashi    8 March, 1995
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_detector_area_resol_mean '100x100 microns'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3708
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.41
_diffrn_reflns_theta_max         30.24
_reflns_number_total             434
_reflns_number_gt                372
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
Molecular Structure Corporation (1994) MSC/AFC Diffractometer
Control Software MSC, 3200 Research Forest Drive, The Woodlands,
TX 77381, USA.
;
_computing_cell_refinement       
;
Molecular Structure Corporation (1994) MSC/AFC Diffractometer
Control Software MSC, 3200 Research Forest Drive, The Woodlands,
TX 77381, USA.
;
_computing_data_reduction        
;
Sheldrick, G. M. (1997) SHELXS97, Program for the Solution
of Crystal Structure,University of Gottingen, Germany.
;
_computing_structure_solution    
;
Sheldrick, G. M. (1997) SHELXS97, Program for the Solution
of Crystal Structure,University of Gottingen, Germany.
;
_computing_structure_refinement  
;
Sheldrick, G. M. (1997) SHELXL97, Program for the Refinement
of Crystal Structure,University of Gottingen, Germany.
;
_computing_molecular_graphics    
;
Interactive Molecular Graphics XP, Virsion 4.2 for MSDOS (1990),
Siemens AnalyticalX-ray Instruments Inc., Madison, Wisconsin,USA.
;
_computing_publication_material  
;
Sheldrick, G. M. (1997) SHELXL97, Program for the refinement
of Crystal Structure,University of Gottingen, Germany.
;

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0105(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         434
_refine_ls_number_parameters     26
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0199
_refine_ls_wR_factor_ref         0.0482
_refine_ls_wR_factor_gt          0.0476
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_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
Ni1 Ni 0.3333 0.6667 0.1667 0.01515(15) Uani 1 6 d S . .
O1 O 0.33975(13) 0.45908(13) 0.11342(4) 0.0251(2) Uani 1 1 d . . .
N1 N 0.6667 0.4199(7) 0.0833 0.0330(12) Uani 0.33 2 d SP . .
C1 C 0.2066(2) 0.3333 0.0833 0.0209(4) Uani 1 2 d S . .
H1 H 0.0931 0.3333 0.0833 0.025 Uiso 1 2 calc SR . .
C2 C 0.6667 0.3333 0.13850(14) 0.0501(8) Uani 1 3 d S . .

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
Ni1 0.01484(17) 0.01484(17) 0.0158(2) 0.000 0.000 0.00742(9)
O1 0.0232(5) 0.0237(5) 0.0288(4) -0.0084(4) -0.0037(4) 0.0120(4)
N1 0.022(2) 0.0231(19) 0.054(3) 0.0017(11) 0.003(2) 0.0108(12)
C1 0.0187(6) 0.0199(9) 0.0246(7) -0.0004(7) -0.0002(3) 0.0100(4)
C2 0.0611(13) 0.0611(13) 0.0281(12) 0.000 0.000 0.0305(6)

_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
Ni1 O1 2.0951(9) 3_565 ?
Ni1 O1 2.0951(9) 2_665 ?
Ni1 O1 2.0951(9) 27 ?
Ni1 O1 2.0951(9) . ?
Ni1 O1 2.0951(9) 26_455 ?
Ni1 O1 2.0951(9) 25_565 ?
O1 C1 1.2557(12) . ?
N1 N1 1.229(10) 2_655 ?
N1 N1 1.229(10) 3_665 ?
N1 C2 1.416(4) . ?
N1 C2 1.417(4) 16_544 ?
C1 O1 1.2557(12) 17_554 ?
C2 N1 1.416(4) 3_665 ?
C2 N1 1.416(4) 2_655 ?

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 Ni1 O1 91.23(4) 3_565 2_665 ?
O1 Ni1 O1 180.0 3_565 27 ?
O1 Ni1 O1 88.77(4) 2_665 27 ?
O1 Ni1 O1 91.23(4) 3_565 . ?
O1 Ni1 O1 91.23(4) 2_665 . ?
O1 Ni1 O1 88.77(4) 27 . ?
O1 Ni1 O1 88.77(4) 3_565 26_455 ?
O1 Ni1 O1 180.0 2_665 26_455 ?
O1 Ni1 O1 91.23(4) 27 26_455 ?
O1 Ni1 O1 88.77(4) . 26_455 ?
O1 Ni1 O1 88.77(4) 3_565 25_565 ?
O1 Ni1 O1 88.77(4) 2_665 25_565 ?
O1 Ni1 O1 91.23(4) 27 25_565 ?
O1 Ni1 O1 180.00(5) . 25_565 ?
O1 Ni1 O1 91.23(4) 26_455 25_565 ?
C1 O1 Ni1 127.08(9) . . ?
N1 N1 N1 60.0 2_655 3_665 ?
N1 N1 C2 64.30(17) 2_655 . ?
N1 N1 C2 64.30(17) 3_665 . ?
N1 N1 C2 64.30(17) 2_655 16_544 ?
N1 N1 C2 64.30(17) 3_665 16_544 ?
C2 N1 C2 119.9(4) . 16_544 ?
O1 C1 O1 125.33(17) . 17_554 ?
N1 C2 N1 51.4(3) 3_665 2_655 ?
N1 C2 N1 51.4(3) 3_665 . ?
N1 C2 N1 51.4(3) 2_655 . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        30.24
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.070

#===END


data_p163
_database_code_depnum_ccdc_archive 'CCDC 703288'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H11 N O6 Zn'
_chemical_formula_weight         246.52

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   R-3c

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

_cell_length_a                   8.1924(8)
_cell_length_b                   8.192
_cell_length_c                   22.277(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1294.81(18)
_cell_formula_units_Z            6
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.897
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             756
_exptl_absorpt_coefficient_mu    2.845
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      273(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       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2979
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0121
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.40
_diffrn_reflns_theta_max         27.32
_reflns_number_total             318
_reflns_number_gt                285
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+3.1769P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         318
_refine_ls_number_parameters     31
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0236
_refine_ls_wR_factor_ref         0.0602
_refine_ls_wR_factor_gt          0.0581
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.142
_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
Zn Zn 0.0000 0.0000 0.0000 0.0231(2) Uani 1 6 d S . .
O1 O -0.0079(2) 0.2086(2) 0.05383(7) 0.0342(4) Uani 1 1 d . . .
C1 C 0.1236(4) 0.3333 0.0833 0.0296(7) Uani 1 2 d S . .
C2 C 0.6667 0.3333 0.1376(2) 0.0573(14) Uani 1 3 d SD . .
N N 0.6667 0.2462(11) 0.0833 0.043(2) Uani 0.33 2 d SPD . .
H2 H 0.71(2) 0.255(16) 0.1577(13) 0.35(5) Uiso 1 1 d D . .
H1 H 0.226(4) 0.3333 0.0833 0.012(7) Uiso 1 2 d S . .

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
Zn 0.0232(2) 0.0232(2) 0.0230(3) 0.000 0.000 0.01160(12)
O1 0.0320(8) 0.0330(8) 0.0371(8) -0.0109(7) -0.0051(7) 0.0160(7)
C1 0.0278(12) 0.0269(15) 0.0338(16) 0.0013(12) 0.0007(6) 0.0135(8)
C2 0.068(2) 0.068(2) 0.035(3) 0.000 0.000 0.0342(11)
N 0.038(5) 0.031(3) 0.062(6) 0.003(2) 0.006(4) 0.019(2)

_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
Zn O1 2.1149(15) 21 ?
Zn O1 2.1149(14) 19 ?
Zn O1 2.1149(15) 3 ?
Zn O1 2.1149(14) . ?
Zn O1 2.1149(14) 2 ?
Zn O1 2.1149(14) 20 ?
O1 C1 1.239(2) . ?
C1 O1 1.239(2) 17_554 ?
C1 H1 0.84(3) . ?
C2 N 1.404(6) . ?
C2 N 1.404(6) 2_655 ?
C2 N 1.404(6) 3_665 ?
C2 H2 0.998(10) . ?
N N 1.237(16) 2_655 ?
N N 1.237(16) 3_665 ?
N C2 1.404(6) 16_544 ?

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 Zn O1 91.02(6) 21 19 ?
O1 Zn O1 180.00(10) 21 3 ?
O1 Zn O1 88.98(6) 19 3 ?
O1 Zn O1 88.98(6) 21 . ?
O1 Zn O1 180.00(10) 19 . ?
O1 Zn O1 91.02(6) 3 . ?
O1 Zn O1 88.98(6) 21 2 ?
O1 Zn O1 88.98(6) 19 2 ?
O1 Zn O1 91.02(6) 3 2 ?
O1 Zn O1 91.02(6) . 2 ?
O1 Zn O1 91.02(6) 21 20 ?
O1 Zn O1 91.02(6) 19 20 ?
O1 Zn O1 88.98(6) 3 20 ?
O1 Zn O1 88.98(6) . 20 ?
O1 Zn O1 180.00(16) 2 20 ?
C1 O1 Zn 127.02(17) . . ?
O1 C1 O1 125.7(3) 17_554 . ?
O1 C1 H1 117.17(15) 17_554 . ?
O1 C1 H1 117.17(15) . . ?
N C2 N 52.3(6) . 2_655 ?
N C2 N 52.3(6) . 3_665 ?
N C2 N 52.3(6) 2_655 3_665 ?
N C2 H2 87.9(9) . . ?
N C2 H2 117(7) 2_655 . ?
N C2 H2 138(3) 3_665 . ?
N N N 60.000(5) 2_655 3_665 ?
N N C2 63.9(3) 2_655 . ?
N N C2 63.9(3) 3_665 . ?
N N C2 63.9(3) 2_655 16_544 ?
N N C2 63.9(3) 3_665 16_544 ?
C2 N C2 118.9(7) . 16_544 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Zn O1 C1 -152.22(15) 21 . . . ?
O1 Zn O1 C1 -148(58) 19 . . . ?
O1 Zn O1 C1 27.78(15) 3 . . . ?
O1 Zn O1 C1 118.81(9) 2 . . . ?
O1 Zn O1 C1 -61.19(9) 20 . . . ?
Zn O1 C1 O1 177.27(14) . . . 17_554 ?
N C2 N N 67.68(19) 3_665 . . 2_655 ?
N C2 N N -67.68(19) 2_655 . . 3_665 ?
N C2 N C2 -33.84(9) 2_655 . . 16_544 ?
N C2 N C2 33.84(9) 3_665 . . 16_544 ?

_diffrn_measured_fraction_theta_max 0.964
_diffrn_reflns_theta_full        27.32
_diffrn_measured_fraction_theta_full 0.964
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.065