Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Partha Mukherjee'
_publ_contact_author_address     
;
Inorganic and Physical Chemistry
Indian Institute of Science
Bangalore
560012
INDIA
;

_publ_contact_author_email       PSM@IPC.IISC.ERNET.IN

_publ_section_title              
;
Dual role of azide in the formation of a 3D
coordination polymer containing bridging 5-pyrimidinecarboxylate
;
loop_
_publ_author_name
'Partha Mukherjee'
'Rajesh Chakraborty'
'Oindrila Sengupta'

# Attachment 'final-cif.cif'

data_os15lt_m
_database_code_depnum_ccdc_archive 'CCDC 655473'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H3 Mn N5 O2.25'
_chemical_formula_sum            'C5 H3 Mn N5 O2.25'
_chemical_formula_weight         224.06

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           Tetragonal
_symmetry_space_group_name_H-M   P4(2)/nmc
_symmetry_space_group_name_Hall  'P 4ac 2a'

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

_cell_length_a                   10.4583(3)
_cell_length_b                   10.4583(3)
_cell_length_c                   13.6296(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1490.75(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3967
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      28.0

_exptl_crystal_description       'rectangular block'
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.997
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888
_exptl_absorpt_coefficient_mu    1.744
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8180
_exptl_absorpt_correction_T_max  0.8731
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
'none'
;

_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  'CCD area detector'
_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            12245
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0117
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         28.02
_reflns_number_total             1001
_reflns_number_gt                832
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'WINGX for Windows(Farrugia, 1997)'
_computing_publication_material  'CIFTAB in SHELXL97 (Sheldrick, 1997)'

_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^)+(0.0431P)^2^+1.5421P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1001
_refine_ls_number_parameters     73
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0802
_refine_ls_wR_factor_gt          0.0756
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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 0.43282(2) 0.56718(2) 0.2500 0.01328(15) Uani 1 2 d S . .
O1 O 0.35735(12) 0.47351(13) 0.12126(9) 0.0182(3) Uani 1 1 d . . .
N1 N 0.4168(2) 0.7500 0.17067(16) 0.0232(5) Uani 1 2 d S . .
N2 N 0.4148(3) 0.7500 0.08090(19) 0.0346(7) Uani 1 2 d S . .
N3 N 0.4119(4) 0.7500 -0.0056(2) 0.0557(11) Uani 1 2 d S . .
N4 N 0.63634(15) 0.54746(16) 0.18210(11) 0.0198(3) Uani 1 1 d . . .
C1 C 0.63823(18) 0.54543(19) 0.08350(13) 0.0201(4) Uani 1 1 d . . .
H1 H 0.5608 0.5452 0.0499 0.024 Uiso 1 1 calc R . .
C2 C 0.7500 0.5437(2) 0.03010(17) 0.0154(5) Uani 1 2 d S . .
C3 C 0.7500 0.5480(3) 0.22745(19) 0.0194(5) Uani 1 2 d S . .
H3 H 0.7500 0.5488 0.2957 0.023 Uiso 1 2 calc SR . .
C4 C 0.2500 0.4686(2) 0.08046(17) 0.0138(5) Uani 1 2 d S . .
O1W O 0.2500 0.7500 -1.344(3) 0.34(2) Uani 0.50 4 d SP . .

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 0.01581(17) 0.01581(17) 0.0082(2) -0.00051(10) -0.00051(10) -0.00054(13)
O1 0.0180(6) 0.0256(7) 0.0110(6) -0.0030(5) -0.0023(5) -0.0003(5)
N1 0.0372(14) 0.0168(11) 0.0156(11) 0.000 -0.0064(10) 0.000
N2 0.0587(19) 0.0218(13) 0.0231(13) 0.000 -0.0036(13) 0.000
N3 0.118(3) 0.0271(15) 0.0217(13) 0.000 -0.0030(17) 0.000
N4 0.0185(8) 0.0297(9) 0.0112(7) -0.0044(6) 0.0010(6) -0.0020(7)
C1 0.0163(9) 0.0304(10) 0.0136(8) -0.0039(7) -0.0006(7) -0.0012(8)
C2 0.0180(12) 0.0176(12) 0.0107(11) -0.0022(9) 0.000 0.000
C3 0.0208(13) 0.0272(14) 0.0103(11) -0.0025(10) 0.000 0.000
C4 0.0165(11) 0.0149(12) 0.0101(11) -0.0019(9) 0.000 0.000
O1W 0.095(16) 0.38(4) 0.53(6) 0.000 0.000 0.000

_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 2.1591(12) . ?
Mn1 O1 2.1591(12) 8_665 ?
Mn1 N1 2.2030(11) . ?
Mn1 N1 2.2030(11) 11_566 ?
Mn1 N4 2.3300(16) . ?
Mn1 N4 2.3300(16) 8_665 ?
O1 C4 1.2539(16) . ?
N1 N2 1.224(3) . ?
N1 Mn1 2.2030(11) 12_666 ?
N2 N3 1.179(4) . ?
N4 C3 1.3399(19) . ?
N4 C1 1.344(2) . ?
C1 C2 1.377(2) . ?
C2 C1 1.377(2) 14_755 ?
C2 C4 1.512(3) 9_665 ?
C3 N4 1.3399(19) 14_755 ?
C4 O1 1.2539(16) 14_655 ?
C4 C2 1.512(3) 9_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 172.86(7) . 8_665 ?
O1 Mn1 N1 88.11(6) . . ?
O1 Mn1 N1 96.67(6) 8_665 . ?
O1 Mn1 N1 96.67(6) . 11_566 ?
O1 Mn1 N1 88.11(6) 8_665 11_566 ?
N1 Mn1 N1 96.25(13) . 11_566 ?
O1 Mn1 N4 88.34(5) . . ?
O1 Mn1 N4 86.60(5) 8_665 . ?
N1 Mn1 N4 87.21(8) . . ?
N1 Mn1 N4 173.99(6) 11_566 . ?
O1 Mn1 N4 86.60(5) . 8_665 ?
O1 Mn1 N4 88.34(5) 8_665 8_665 ?
N1 Mn1 N4 173.99(6) . 8_665 ?
N1 Mn1 N4 87.21(8) 11_566 8_665 ?
N4 Mn1 N4 89.78(8) . 8_665 ?
C4 O1 Mn1 134.94(13) . . ?
N2 N1 Mn1 119.48(5) . 12_666 ?
N2 N1 Mn1 119.48(5) . . ?
Mn1 N1 Mn1 120.44(10) 12_666 . ?
N3 N2 N1 179.5(4) . . ?
C3 N4 C1 116.63(17) . . ?
C3 N4 Mn1 128.81(13) . . ?
C1 N4 Mn1 114.33(13) . . ?
N4 C1 C2 122.76(18) . . ?
C1 C2 C1 116.2(2) 14_755 . ?
C1 C2 C4 121.85(11) 14_755 9_665 ?
C1 C2 C4 121.85(11) . 9_665 ?
N4 C3 N4 125.0(2) . 14_755 ?
O1 C4 O1 127.1(2) 14_655 . ?
O1 C4 C2 116.44(11) 14_655 9_665 ?
O1 C4 C2 116.44(11) . 9_665 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.02
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.075