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

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Xiao-Ming Chen'
_publ_contact_author_email       CXM@MAIL.SYSU.EDU.CN

_publ_section_title              
;
3D geometrically frustrated magnets assembled by
transition metal ion and 1,2,3-triazole-4,5-dicarboxylate as triangular
nodes
;
loop_
_publ_author_name
'Xiao-Ming Chen.'
'Jian-Bin Lin.'
'Wei Xue.'
'Wei-Xiong Zhang.'
;
Yan-Zhen Zheng
;

# Attachment '1.cif'

data_a
_database_code_depnum_ccdc_archive 'CCDC 691173'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H9 Co N4 O4.50'
_chemical_formula_weight         268.10

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           Cubic
_symmetry_space_group_name_H-M   P2(1)3

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

_cell_length_a                   9.8941(7)
_cell_length_b                   9.8941(7)
_cell_length_c                   9.8941(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     968.57(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.839
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             544
_exptl_absorpt_coefficient_mu    1.780
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8283
_exptl_absorpt_correction_T_max  0.8421
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9834
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         26.00
_reflns_number_total             650
_reflns_number_gt                620
_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 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)+(0.0461P)²+0.1254P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(5)
_refine_ls_number_reflns         650
_refine_ls_number_parameters     97
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0282
_refine_ls_wR_factor_ref         0.0721
_refine_ls_wR_factor_gt          0.0701
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co -0.63780(4) 0.13780(4) -0.13780(4) 0.0625(2) Uani 1 3 d S . .
C1 C -0.4736(12) -0.0995(10) -0.2461(10) 0.089(2) Uani 0.33 1 d PD A -1
C2 C -0.5543(7) -0.1484(6) -0.3656(6) 0.0447(12) Uani 0.33 1 d PD A -1
C3 C -0.6704(7) -0.0981(6) -0.4263(7) 0.0447(12) Uani 0.33 1 d PD A -1
C4 C -0.7581(12) 0.0215(11) -0.3971(11) 0.089(2) Uani 0.33 1 d PD A -1
N1 N -0.5180(7) -0.2607(6) -0.4347(6) 0.0554(10) Uani 0.33 1 d PD . -1
N2 N -0.6070(8) -0.2787(9) -0.5327(10) 0.0554(10) Uani 0.33 1 d PD B -1
N3 N -0.6982(6) -0.1829(6) -0.5293(7) 0.0554(10) Uani 0.33 1 d PD . -1
O1 O -0.4239(14) -0.2157(9) -0.2270(14) 0.096(3) Uani 0.33 1 d PD . -1
O2 O -0.4762(15) -0.0152(11) -0.1501(10) 0.095(3) Uani 0.33 1 d PD A -1
O3 O -0.7736(16) 0.1187(11) -0.3174(10) 0.095(3) Uani 0.33 1 d PD A -1
O4 O -0.8011(13) 0.0298(11) -0.5163(10) 0.096(3) Uani 0.33 1 d PD . -1
N4 N -0.399(4) -0.130(3) 0.105(3) 0.135(9) Uani 0.33 1 d PD C -1
H4A H -0.4106 -0.0921 0.1870 0.162 Uiso 0.33 1 d PR C -1
H4B H -0.4470 -0.0835 0.0441 0.162 Uiso 0.33 1 d PR C -1
C5 C -0.443(3) -0.270(3) 0.110(2) 0.139(6) Uani 0.33 1 d PD C -1
H5A H -0.5387 -0.2546 0.1310 0.209 Uiso 0.33 1 d PR C -1
H5B H -0.4019 -0.3238 0.1824 0.209 Uiso 0.33 1 d PR C -1
H5C H -0.4358 -0.3193 0.0243 0.209 Uiso 0.33 1 d PR C -1
C6 C -0.256(4) -0.130(3) 0.069(3) 0.139(6) Uani 0.33 1 d PD C -1
H6A H -0.2144 -0.0414 0.0579 0.209 Uiso 0.33 1 d PR C -1
H6B H -0.2493 -0.1811 -0.0157 0.209 Uiso 0.33 1 d PR C -1
H6C H -0.2097 -0.1801 0.1411 0.209 Uiso 0.33 1 d PR C -1
O1W O -0.326(2) -0.029(4) 0.367(2) 0.162(11) Uani 0.17 1 d P . .
H1WA H -0.3099 -0.0958 0.4195 0.244 Uiso 0.17 1 d PR . .
H1WB H -0.2562 0.0207 0.3627 0.244 Uiso 0.17 1 d PR . .


_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 N1 1.975(6) 3_454 ?
Co1 N1 1.975(6) 8_454 ?
Co1 N1 1.975(6) 10_454 ?
Co1 N3 1.996(6) 11_444 ?
Co1 N3 1.996(6) 5_565 ?
Co1 N3 1.996(6) 2_355 ?
Co1 O1 2.065(10) 3_454 ?
Co1 O1 2.065(10) 8_454 ?
Co1 O1 2.065(10) 10_454 ?
Co1 O4 2.135(9) 5_565 ?
Co1 O4 2.135(9) 11_444 ?
Co1 O4 2.135(9) 2_355 ?
C1 O2 1.264(9) . ?
C1 O1 1.265(9) . ?
C1 C2 1.506(9) . ?
C2 N1 1.353(8) . ?
C2 C3 1.389(7) . ?
C3 N3 1.348(8) . ?
C3 C4 1.496(9) . ?
C4 O3 1.254(9) . ?
C4 O4 1.256(9) . ?
N1 N2 1.322(8) . ?
N1 Co1 1.975(6) 3_444 ?
N2 N3 1.309(8) . ?
N3 Co1 1.996(6) 2_354 ?
O1 Co1 2.065(10) 3_444 ?
O4 Co1 2.135(9) 2_354 ?
N4 C5 1.453(10) . ?
N4 C6 1.453(10) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
C5 O1W 1.18(4) 12_455 ?
C5 H5A 0.9800 . ?
C5 H5B 0.9799 . ?
C5 H5C 0.9801 . ?
C6 O1W 1.36(4) 6_445 ?
C6 H6A 0.9800 . ?
C6 H6B 0.9801 . ?
C6 H6C 0.9799 . ?
O1W C5 1.18(4) 6_445 ?
O1W C6 1.36(4) 12_455 ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8499 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Co1 N1 107.36(18) 3_454 8_454 ?
N1 Co1 N1 107.36(18) 3_454 10_454 ?
N1 Co1 N1 107.36(18) 8_454 10_454 ?
N1 Co1 N3 138.0(3) 3_454 11_444 ?
N1 Co1 N3 41.2(2) 8_454 11_444 ?
N1 Co1 N3 109.0(3) 10_454 11_444 ?
N1 Co1 N3 41.2(2) 3_454 5_565 ?
N1 Co1 N3 109.0(3) 8_454 5_565 ?
N1 Co1 N3 138.0(3) 10_454 5_565 ?
N3 Co1 N3 112.07(17) 11_444 5_565 ?
N1 Co1 N3 109.0(3) 3_454 2_355 ?
N1 Co1 N3 138.0(3) 8_454 2_355 ?
N1 Co1 N3 41.2(2) 10_454 2_355 ?
N3 Co1 N3 112.07(17) 11_444 2_355 ?
N3 Co1 N3 112.07(17) 5_565 2_355 ?
N1 Co1 O1 69.4(4) 3_454 3_454 ?
N1 Co1 O1 96.4(4) 8_454 3_454 ?
N1 Co1 O1 155.7(4) 10_454 3_454 ?
N3 Co1 O1 85.2(4) 11_444 3_454 ?
N3 Co1 O1 29.0(3) 5_565 3_454 ?
N3 Co1 O1 115.6(5) 2_355 3_454 ?
N1 Co1 O1 155.7(4) 3_454 8_454 ?
N1 Co1 O1 69.4(4) 8_454 8_454 ?
N1 Co1 O1 96.4(4) 10_454 8_454 ?
N3 Co1 O1 29.0(3) 11_444 8_454 ?
N3 Co1 O1 115.6(5) 5_565 8_454 ?
N3 Co1 O1 85.2(4) 2_355 8_454 ?
O1 Co1 O1 86.8(5) 3_454 8_454 ?
N1 Co1 O1 96.4(4) 3_454 10_454 ?
N1 Co1 O1 155.7(4) 8_454 10_454 ?
N1 Co1 O1 69.4(4) 10_454 10_454 ?
N3 Co1 O1 115.6(5) 11_444 10_454 ?
N3 Co1 O1 85.2(4) 5_565 10_454 ?
N3 Co1 O1 29.0(3) 2_355 10_454 ?
O1 Co1 O1 86.8(5) 3_454 10_454 ?
O1 Co1 O1 86.8(5) 8_454 10_454 ?
N1 Co1 O4 30.1(3) 3_454 5_565 ?
N1 Co1 O4 114.3(4) 8_454 5_565 ?
N1 Co1 O4 77.5(4) 10_454 5_565 ?
N3 Co1 O4 155.4(4) 11_444 5_565 ?
N3 Co1 O4 68.9(4) 5_565 5_565 ?
N3 Co1 O4 88.7(4) 2_355 5_565 ?
O1 Co1 O4 97.9(5) 3_454 5_565 ?
O1 Co1 O4 173.5(6) 8_454 5_565 ?
O1 Co1 O4 89.0(6) 10_454 5_565 ?
N1 Co1 O4 77.5(4) 3_454 11_444 ?
N1 Co1 O4 30.1(3) 8_454 11_444 ?
N1 Co1 O4 114.3(4) 10_454 11_444 ?
N3 Co1 O4 68.9(4) 11_444 11_444 ?
N3 Co1 O4 88.7(4) 5_565 11_444 ?
N3 Co1 O4 155.4(4) 2_355 11_444 ?
O1 Co1 O4 89.0(6) 3_454 11_444 ?
O1 Co1 O4 97.9(5) 8_454 11_444 ?
O1 Co1 O4 173.5(6) 10_454 11_444 ?
O4 Co1 O4 86.7(5) 5_565 11_444 ?
N1 Co1 O4 114.3(4) 3_454 2_355 ?
N1 Co1 O4 77.5(4) 8_454 2_355 ?
N1 Co1 O4 30.1(3) 10_454 2_355 ?
N3 Co1 O4 88.7(4) 11_444 2_355 ?
N3 Co1 O4 155.4(4) 5_565 2_355 ?
N3 Co1 O4 68.9(4) 2_355 2_355 ?
O1 Co1 O4 173.5(6) 3_454 2_355 ?
O1 Co1 O4 89.0(6) 8_454 2_355 ?
O1 Co1 O4 97.9(5) 10_454 2_355 ?
O4 Co1 O4 86.7(5) 5_565 2_355 ?
O4 Co1 O4 86.7(5) 11_444 2_355 ?
O2 C1 O1 119.7(10) . . ?
O2 C1 C2 142.3(11) . . ?
O1 C1 C2 91.8(9) . . ?
N1 C2 C3 107.2(5) . . ?
N1 C2 C1 121.3(8) . . ?
C3 C2 C1 131.5(8) . . ?
N3 C3 C2 105.8(5) . . ?
N3 C3 C4 121.3(8) . . ?
C2 C3 C4 132.9(9) . . ?
O3 C4 O4 120.0(9) . . ?
O3 C4 C3 143.1(11) . . ?
O4 C4 C3 93.9(9) . . ?
N2 N1 C2 107.7(6) . . ?
N2 N1 Co1 135.9(5) . 3_444 ?
C2 N1 Co1 116.2(5) . 3_444 ?
N3 N2 N1 110.0(7) . . ?
N2 N3 C3 109.2(6) . . ?
N2 N3 Co1 135.1(6) . 2_354 ?
C3 N3 Co1 115.7(5) . 2_354 ?
C1 O1 Co1 131.0(11) . 3_444 ?
C1 O2 Co1 120.6(9) . . ?
C4 O3 Co1 119.5(8) . . ?
C4 O4 Co1 125.0(10) . 2_354 ?
C5 N4 C6 107.5(10) . . ?
C5 N4 H4A 109.4 . . ?
C6 N4 H4A 110.4 . . ?
C5 N4 H4B 110.5 . . ?
C6 N4 H4B 110.5 . . ?
H4A N4 H4B 108.5 . . ?
O1W C5 N4 149(2) 12_455 . ?
O1W C5 H5A 78.1 12_455 . ?
N4 C5 H5A 98.5 . . ?
O1W C5 H5B 42.6 12_455 . ?
N4 C5 H5B 114.4 . . ?
H5A C5 H5B 109.5 . . ?
O1W C5 H5C 94.6 12_455 . ?
N4 C5 H5C 114.9 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O1W C6 N4 161(2) 6_445 . ?
O1W C6 H6A 82.7 6_445 . ?
N4 C6 H6A 115.9 . . ?
O1W C6 H6B 61.7 6_445 . ?
N4 C6 H6B 106.2 . . ?
H6A C6 H6B 109.5 . . ?
O1W C6 H6C 68.1 6_445 . ?
N4 C6 H6C 106.1 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 O1W C6 14(2) 6_445 12_455 ?
C5 O1W H1WA 114.6 6_445 . ?
C6 O1W H1WA 112.5 12_455 . ?
C5 O1W H1WB 121.7 6_445 . ?
C6 O1W H1WB 112.3 12_455 . ?
H1WA O1W H1WB 109.5 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.146
_refine_diff_density_rms         0.047

# Attachment '2.cif'

data_d
_database_code_depnum_ccdc_archive 'CCDC 691174'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H8 Mn N4 O4.50'
_chemical_formula_weight         263.10

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           Cubic
_symmetry_space_group_name_H-M   P2(1)3

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

_cell_length_a                   10.2304(4)
_cell_length_b                   10.2304(4)
_cell_length_c                   10.2304(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1070.72(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             532
_exptl_absorpt_coefficient_mu    1.240
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8757
_exptl_absorpt_correction_T_max  0.8861
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9249
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0134
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.82
_diffrn_reflns_theta_max         24.82
_reflns_number_total             627
_reflns_number_gt                596
_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 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)+(0.1401P)²+1.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_number_reflns         627
_refine_ls_number_parameters     82
_refine_ls_number_restraints     113
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0905
_refine_ls_wR_factor_ref         0.2546
_refine_ls_wR_factor_gt          0.2513
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_restrained_S_all      1.146
_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 -0.37401(19) -0.12599(19) -0.87401(19) 0.0973(11) Uani 1 3 d SU . .
C1 C -0.520(3) 0.136(3) -0.763(2) 0.100(7) Uani 0.33 1 d PDU A -1
C2 C -0.4396(13) 0.1695(16) -0.6470(14) 0.067(5) Uani 0.33 1 d PDU A -1
C3 C -0.3298(14) 0.1097(14) -0.5980(17) 0.067(5) Uani 0.33 1 d PDU A -1
C4 C -0.232(2) 0.003(2) -0.610(2) 0.100(7) Uani 0.33 1 d PDU A -1
N1 N -0.4649(17) 0.2715(15) -0.5671(16) 0.089(4) Uani 0.33 1 d PDU . -1
N2 N -0.375(2) 0.274(2) -0.4743(17) 0.089(4) Uani 0.33 1 d PDU B -1
N3 N -0.2921(18) 0.177(2) -0.4908(16) 0.089(4) Uani 0.33 1 d PDU . -1
O1 O -0.610(3) 0.219(3) -0.772(4) 0.181(12) Uani 0.33 1 d PDU . -1
O2 O -0.507(3) 0.048(3) -0.849(3) 0.131(7) Uani 0.33 1 d PDU A -1
O3 O -0.223(3) -0.077(3) -0.701(3) 0.131(7) Uani 0.33 1 d PDU A -1
O4 O -0.210(4) -0.020(4) -0.493(3) 0.181(12) Uani 0.33 1 d PDU . -1
N4 N -0.367(2) 0.367(2) -1.133(2) 0.28(2) Uani 1 3 d SDU . .
H4A H -0.3158 0.3158 -1.1842 0.333 Uiso 1 3 calc SR . .
C5 C -0.484(3) 0.298(2) -1.097(6) 0.34(3) Uani 0.67 1 d PDU . .
H5A H -0.5493 0.3104 -1.1634 0.505 Uiso 0.67 1 calc PR . .
H5B H -0.5159 0.3304 -1.0151 0.505 Uiso 0.67 1 calc PR . .
H5C H -0.4648 0.2063 -1.0891 0.505 Uiso 0.67 1 calc PR . .
O1W O -0.601(2) 0.101(2) -1.101(2) 0.197(19) Uani 0.50 3 d SPU . .
H1WA H -0.6638 0.1070 -1.0490 0.296 Uiso 0.17 1 d PR . .
H1WB H -0.6320 0.0979 -1.1805 0.296 Uiso 0.17 1 d PR . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 N1 2.045(14) 10_553 ?
Mn1 N1 2.045(14) 3_443 ?
Mn1 N1 2.045(14) 8_454 ?
Mn1 O4 2.11(3) 5_554 ?
Mn1 O4 2.11(3) 2_454 ?
Mn1 O4 2.11(3) 11_444 ?
Mn1 N3 2.141(13) 2_454 ?
Mn1 N3 2.141(13) 11_444 ?
Mn1 N3 2.141(13) 5_554 ?
Mn1 O1 2.19(3) 10_553 ?
Mn1 O1 2.19(3) 8_454 ?
Mn1 O1 2.19(3) 3_443 ?
C1 O1 1.255(10) . ?
C1 O2 1.257(10) . ?
C1 C2 1.490(9) . ?
C2 N1 1.350(9) . ?
C2 C3 1.374(9) . ?
C3 N3 1.350(9) . ?
C3 C4 1.485(9) . ?
C4 O4 1.245(10) . ?
C4 O3 1.246(10) . ?
N1 N2 1.319(9) . ?
N1 Mn1 2.045(14) 3_453 ?
N2 N3 1.319(9) . ?
N3 Mn1 2.141(13) 2_455 ?
O1 Mn1 2.19(3) 3_453 ?
O4 Mn1 2.11(3) 2_455 ?
N4 C5 1.437(10) 10_563 ?
N4 C5 1.437(10) . ?
N4 C5 1.437(10) 7_353 ?
N4 H4A 0.9100 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
O1W H1WA 0.8359 . ?
O1W H1WB 0.8710 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Mn1 N1 109.1(5) 10_553 3_443 ?
N1 Mn1 N1 109.1(5) 10_553 8_454 ?
N1 Mn1 N1 109.1(5) 3_443 8_454 ?
N1 Mn1 O4 81.0(11) 10_553 5_554 ?
N1 Mn1 O4 28.1(10) 3_443 5_554 ?
N1 Mn1 O4 121.6(11) 8_454 5_554 ?
N1 Mn1 O4 28.1(10) 10_553 2_454 ?
N1 Mn1 O4 121.6(11) 3_443 2_454 ?
N1 Mn1 O4 81.0(11) 8_454 2_454 ?
O4 Mn1 O4 96.7(16) 5_554 2_454 ?
N1 Mn1 O4 121.6(11) 10_553 11_444 ?
N1 Mn1 O4 81.0(11) 3_443 11_444 ?
N1 Mn1 O4 28.1(10) 8_454 11_444 ?
O4 Mn1 O4 96.7(16) 5_554 11_444 ?
O4 Mn1 O4 96.7(16) 2_454 11_444 ?
N1 Mn1 N3 38.2(6) 10_553 2_454 ?
N1 Mn1 N3 110.6(6) 3_443 2_454 ?
N1 Mn1 N3 135.7(6) 8_454 2_454 ?
O4 Mn1 N3 87.8(10) 5_554 2_454 ?
O4 Mn1 N3 61.7(13) 2_454 2_454 ?
O4 Mn1 N3 158.4(11) 11_444 2_454 ?
N1 Mn1 N3 110.6(6) 10_553 11_444 ?
N1 Mn1 N3 135.7(6) 3_443 11_444 ?
N1 Mn1 N3 38.2(6) 8_454 11_444 ?
O4 Mn1 N3 158.4(11) 5_554 11_444 ?
O4 Mn1 N3 87.8(10) 2_454 11_444 ?
O4 Mn1 N3 61.7(13) 11_444 11_444 ?
N3 Mn1 N3 112.7(5) 2_454 11_444 ?
N1 Mn1 N3 135.7(6) 10_553 5_554 ?
N1 Mn1 N3 38.2(6) 3_443 5_554 ?
N1 Mn1 N3 110.6(6) 8_454 5_554 ?
O4 Mn1 N3 61.7(13) 5_554 5_554 ?
O4 Mn1 N3 158.4(11) 2_454 5_554 ?
O4 Mn1 N3 87.8(10) 11_444 5_554 ?
N3 Mn1 N3 112.7(5) 2_454 5_554 ?
N3 Mn1 N3 112.7(5) 11_444 5_554 ?
N1 Mn1 O1 76.7(8) 10_553 10_553 ?
N1 Mn1 O1 102.3(12) 3_443 10_553 ?
N1 Mn1 O1 143.4(12) 8_454 10_553 ?
O4 Mn1 O1 94.9(16) 5_554 10_553 ?
O4 Mn1 O1 98.4(15) 2_454 10_553 ?
O4 Mn1 O1 159.6(13) 11_444 10_553 ?
N3 Mn1 O1 38.5(9) 2_454 10_553 ?
N3 Mn1 O1 105.3(12) 11_444 10_553 ?
N3 Mn1 O1 83.1(11) 5_554 10_553 ?
N1 Mn1 O1 102.3(12) 10_553 8_454 ?
N1 Mn1 O1 143.4(12) 3_443 8_454 ?
N1 Mn1 O1 76.7(8) 8_454 8_454 ?
O4 Mn1 O1 159.6(13) 5_554 8_454 ?
O4 Mn1 O1 94.9(16) 2_454 8_454 ?
O4 Mn1 O1 98.4(15) 11_444 8_454 ?
N3 Mn1 O1 83.1(11) 2_454 8_454 ?
N3 Mn1 O1 38.5(9) 11_444 8_454 ?
N3 Mn1 O1 105.3(12) 5_554 8_454 ?
O1 Mn1 O1 66.8(14) 10_553 8_454 ?
N1 Mn1 O1 143.4(12) 10_553 3_443 ?
N1 Mn1 O1 76.7(8) 3_443 3_443 ?
N1 Mn1 O1 102.3(11) 8_454 3_443 ?
O4 Mn1 O1 98.4(15) 5_554 3_443 ?
O4 Mn1 O1 159.6(13) 2_454 3_443 ?
O4 Mn1 O1 94.9(16) 11_444 3_443 ?
N3 Mn1 O1 105.3(12) 2_454 3_443 ?
N3 Mn1 O1 83.1(11) 11_444 3_443 ?
N3 Mn1 O1 38.5(9) 5_554 3_443 ?
O1 Mn1 O1 66.8(14) 10_553 3_443 ?
O1 Mn1 O1 66.8(14) 8_454 3_443 ?
O1 C1 O2 120.6(18) . . ?
O1 C1 C2 108(2) . . ?
O2 C1 C2 131(2) . . ?
N1 C2 C3 106.2(9) . . ?
N1 C2 C1 123.9(16) . . ?
C3 C2 C1 129.9(18) . . ?
N3 C3 C2 107.7(9) . . ?
N3 C3 C4 104.4(18) . . ?
C2 C3 C4 147.9(19) . . ?
O4 C4 O3 126(2) . . ?
O4 C4 C3 100(2) . . ?
O3 C4 C3 127(2) . . ?
N2 N1 C2 108.5(9) . . ?
N2 N1 Mn1 139.7(13) . 3_453 ?
C2 N1 Mn1 111.9(11) . 3_453 ?
N3 N2 N1 110.0(10) . . ?
N2 N3 C3 107.6(9) . . ?
N2 N3 Mn1 128.6(13) . 2_455 ?
C3 N3 Mn1 123.8(14) . 2_455 ?
C1 O1 Mn1 120(3) . 3_453 ?
C1 O2 Mn1 135.0(18) . . ?
C4 O3 Mn1 129.7(17) . . ?
C4 O4 Mn1 120(2) . 2_455 ?
C5 N4 C5 109(2) 10_563 . ?
C5 N4 C5 109(2) 10_563 7_353 ?
C5 N4 C5 109(2) . 7_353 ?
C5 N4 H4A 110.0 10_563 . ?
C5 N4 H4A 110.0 . . ?
C5 N4 H4A 110.0 7_353 . ?
N4 C5 H5A 109.5 . . ?
N4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
H1WA O1W H1WB 108.8 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.82
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.091

# Attachment '3.cif'

data_b
_database_code_depnum_ccdc_archive 'CCDC 691175'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H9.20 Mn N4 O6.60'
_chemical_formula_weight         273.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   P6(1)

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

_cell_length_a                   14.3295(6)
_cell_length_b                   14.3295(6)
_cell_length_c                   10.0523(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1787.55(18)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             834
_exptl_absorpt_coefficient_mu    1.129
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8400
_exptl_absorpt_correction_T_max  0.9251
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12457
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         26.04
_reflns_number_total             2349
_reflns_number_gt                2278
_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 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)+(0.0968P)²+0.5141P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_number_reflns         2349
_refine_ls_number_parameters     133
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0478
_refine_ls_wR_factor_ref         0.1324
_refine_ls_wR_factor_gt          0.1314
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_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 0.87483(4) 0.33960(4) 0.06239(6) 0.0283(2) Uani 1 1 d . . .
C1 C 0.6813(4) 0.2203(3) -0.1351(4) 0.0361(9) Uani 1 1 d . . .
C2 C 0.6094(3) 0.1285(3) -0.0480(4) 0.0269(7) Uani 1 1 d . . .
C3 C 0.6234(3) 0.0793(3) 0.0626(4) 0.0271(7) Uani 1 1 d . . .
C4 C 0.7142(3) 0.0973(3) 0.1525(4) 0.0336(8) Uani 1 1 d . . .
N1 N 0.5050(2) 0.0703(2) -0.0833(4) 0.0318(7) Uani 1 1 d . . .
N2 N 0.4563(3) -0.0118(3) 0.0005(4) 0.0348(8) Uani 1 1 d . . .
N3 N 0.5263(2) -0.0083(2) 0.0889(3) 0.0299(7) Uani 1 1 d . . .
O1 O 0.6362(3) 0.2399(3) -0.2302(4) 0.0532(9) Uani 1 1 d . . .
O2 O 0.7815(2) 0.2716(3) -0.1149(3) 0.0469(8) Uani 1 1 d . . .
O3 O 0.7975(3) 0.1875(3) 0.1578(4) 0.0616(11) Uani 1 1 d . . .
O4 O 0.6970(2) 0.0185(2) 0.2235(4) 0.0432(7) Uani 1 1 d . . .
N4 N 0.2822(5) -0.2344(4) -0.0647(7) 0.0804(17) Uani 1 1 d . . .
H4A H 0.2419 -0.2516 -0.1390 0.121 Uiso 1 1 d R . .
H4B H 0.3311 -0.1637 -0.0696 0.121 Uiso 1 1 d R . .
H4C H 0.3168 -0.2709 -0.0825 0.121 Uiso 1 1 d R . .
H4D H 0.2376 -0.2676 0.0041 0.121 Uiso 1 1 d R . .
O1W O 0.1238(9) -0.3176(9) 0.1214(14) 0.174(5) Uiso 1 1 d . . .
H1WA H 0.1516 -0.3089 0.1984 0.261 Uiso 1 1 d R . .
H1WB H 0.0702 -0.3110 0.0994 0.261 Uiso 1 1 d R . .
O2W O -0.038(2) -0.286(2) 0.059(3) 0.261(8) Uiso 0.60 1 d P . .
H2WA H -0.0515 -0.2530 0.1199 0.392 Uiso 0.60 1 d PR . .
H2WB H -0.0364 -0.2481 -0.0074 0.392 Uiso 0.60 1 d PR . .
O3W O -0.091(3) -0.173(3) 0.241(4) 0.261(8) Uiso 0.50 1 d P . .
H3WA H -0.0369 -0.1405 0.2923 0.392 Uiso 0.50 1 d PR . .
H3WB H -0.1570 -0.2057 0.2652 0.392 Uiso 0.50 1 d PR . .
O4W O -0.029(3) -0.191(2) -0.227(4) 0.261(8) Uiso 0.50 1 d P . .
H4WA H -0.0294 -0.2344 -0.2848 0.392 Uiso 0.50 1 d PR . .
H4WB H -0.0785 -0.1857 -0.2661 0.392 Uiso 0.50 1 d PR . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O3 2.118(3) . ?
Mn1 O2 2.147(3) . ?
Mn1 O4 2.201(3) 5_664 ?
Mn1 O1 2.206(3) 2_655 ?
Mn1 N1 2.227(3) 2_655 ?
Mn1 N3 2.240(3) 5_664 ?
C1 O2 1.261(5) . ?
C1 O1 1.262(6) . ?
C1 C2 1.484(5) . ?
C2 N1 1.347(5) . ?
C2 C3 1.383(6) . ?
C3 N3 1.355(4) . ?
C3 C4 1.497(5) . ?
C4 O3 1.248(5) . ?
C4 O4 1.252(5) . ?
N1 N2 1.326(5) . ?
N1 Mn1 2.227(3) 3_664 ?
N2 N3 1.322(5) . ?
N3 Mn1 2.240(3) 6_545 ?
O1 Mn1 2.206(3) 3_664 ?
O4 Mn1 2.201(3) 6_545 ?
N4 H4A 0.8999 . ?
N4 H4B 0.9000 . ?
N4 H4C 0.9000 . ?
N4 H4D 0.9000 . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8499 . ?
O2W H2WA 0.8501 . ?
O2W H2WB 0.8499 . ?
O3W H3WA 0.8500 . ?
O3W H3WB 0.8500 . ?
O4W H4WA 0.8498 . ?
O4W H4WB 0.8501 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Mn1 O2 91.30(14) . . ?
O3 Mn1 O4 85.90(15) . 5_664 ?
O2 Mn1 O4 109.42(14) . 5_664 ?
O3 Mn1 O1 101.12(17) . 2_655 ?
O2 Mn1 O1 84.91(13) . 2_655 ?
O4 Mn1 O1 164.06(13) 5_664 2_655 ?
O3 Mn1 N1 95.10(15) . 2_655 ?
O2 Mn1 N1 158.38(13) . 2_655 ?
O4 Mn1 N1 91.65(13) 5_664 2_655 ?
O1 Mn1 N1 73.60(12) 2_655 2_655 ?
O3 Mn1 N3 155.35(16) . 5_664 ?
O2 Mn1 N3 83.58(11) . 5_664 ?
O4 Mn1 N3 73.27(11) 5_664 5_664 ?
O1 Mn1 N3 102.41(14) 2_655 5_664 ?
N1 Mn1 N3 98.47(12) 2_655 5_664 ?
O2 C1 O1 123.5(4) . . ?
O2 C1 C2 120.4(4) . . ?
O1 C1 C2 116.1(4) . . ?
N1 C2 C3 107.1(3) . . ?
N1 C2 C1 117.2(3) . . ?
C3 C2 C1 135.5(3) . . ?
N3 C3 C2 106.7(3) . . ?
N3 C3 C4 116.3(3) . . ?
C2 C3 C4 137.1(3) . . ?
O3 C4 O4 124.3(4) . . ?
O3 C4 C3 120.2(4) . . ?
O4 C4 C3 115.3(3) . . ?
N2 N1 C2 108.1(3) . . ?
N2 N1 Mn1 137.4(3) . 3_664 ?
C2 N1 Mn1 114.1(2) . 3_664 ?
N3 N2 N1 109.9(3) . . ?
N2 N3 C3 108.2(3) . . ?
N2 N3 Mn1 136.1(2) . 6_545 ?
C3 N3 Mn1 113.6(2) . 6_545 ?
C1 O1 Mn1 118.5(3) . 3_664 ?
C1 O2 Mn1 131.9(3) . . ?
C4 O3 Mn1 141.6(3) . . ?
C4 O4 Mn1 119.9(2) . 6_545 ?
H4A N4 H4B 107.2 . . ?
H4A N4 H4C 98.1 . . ?
H4B N4 H4C 107.3 . . ?
H4A N4 H4D 107.6 . . ?
H4B N4 H4D 125.8 . . ?
H4C N4 H4D 107.3 . . ?
H1WA O1W H1WB 127.2 . . ?
H2WA O2W H2WB 99.1 . . ?
H3WA O3W H3WB 126.5 . . ?
H4WA O4W H4WB 92.4 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.04
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.125


