#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:11:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179316 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/13/4321316.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4321316
loop_
_publ_author_name
'Wenbin Lin'
'Mary E. Chapman'
'Zhiyong Wang'
'Gordon T. Yee'
_publ_section_title
;
 Three-Dimensional Manganese(II) Coordination Polymers Based on
 m-Pyridinecarboxylates: Synthesis, X-ray Structures, and Magnetic
 Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4169
_journal_page_last               4173
_journal_paper_doi               10.1021/ic000227v
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C12 H8 Mn N2 O4'
_chemical_formula_weight         299.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.7560(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9180(8)
_cell_length_b                   9.3492(5)
_cell_length_c                   8.8051(5)
_cell_measurement_temperature    198(2)
_cell_volume                     1115.20(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3551
_diffrn_reflns_theta_full        28.23
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    1.195
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             604
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.0046(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         1331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0451P)²+1.1731P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0738
_reflns_number_gt                1289
_reflns_number_total             1331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000227v_1.cif
_cod_data_source_block           Compound1
_cod_database_code               4321316
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.38387(3) 0.2500 0.01380(13) Uani 1 2 d S . .
O2 O 0.38154(7) 0.35412(12) -0.00112(12) 0.0194(2) Uani 1 1 d . . .
C1 C 0.36020(10) 0.39523(13) -0.14844(17) 0.0148(3) Uani 1 1 d . . .
C2 C 0.25407(10) 0.37219(13) -0.27441(17) 0.0162(3) Uani 1 1 d . . .
C3 C 0.22015(13) 0.4280(2) -0.4348(2) 0.0324(4) Uani 1 1 d . . .
O1 O 0.41752(7) 0.45051(12) -0.20120(13) 0.0230(2) Uani 1 1 d . . .
N1 N 0.09295(9) 0.27353(13) -0.33573(14) 0.0197(3) Uani 1 1 d . . .
C6 C 0.18800(10) 0.29556(15) -0.23257(16) 0.0187(3) Uani 1 1 d . . .
C4 C 0.12215(15) 0.4062(3) -0.5436(2) 0.0469(6) Uani 1 1 d . . .
C5 C 0.06143(12) 0.3291(2) -0.4899(2) 0.0334(4) Uani 1 1 d . . .
H6 H 0.2092(17) 0.256(2) -0.125(3) 0.042(6) Uiso 1 1 d . . .
H5 H -0.0036(18) 0.309(2) -0.560(3) 0.041(6) Uiso 1 1 d . . .
H3 H 0.2598(17) 0.480(2) -0.470(3) 0.037(5) Uiso 1 1 d . . .
H4 H 0.099(2) 0.442(3) -0.643(4) 0.064(8) Uiso 1 1 d . . .
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'
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 86.76(6) 5_665 6_566 ?
O1 Mn1 O2 100.27(4) 5_665 . ?
O1 Mn1 O2 90.34(4) 6_566 . ?
O1 Mn1 O2 90.34(4) 5_665 2_655 ?
O1 Mn1 O2 100.27(4) 6_566 2_655 ?
O2 Mn1 O2 165.44(6) . 2_655 ?
O1 Mn1 N1 170.79(4) 5_665 7 ?
O1 Mn1 N1 85.53(4) 6_566 7 ?
O2 Mn1 N1 84.83(4) . 7 ?
O2 Mn1 N1 86.08(4) 2_655 7 ?
O1 Mn1 N1 85.53(4) 5_665 8_556 ?
O1 Mn1 N1 170.79(4) 6_566 8_556 ?
O2 Mn1 N1 86.08(4) . 8_556 ?
O2 Mn1 N1 84.83(4) 2_655 8_556 ?
N1 Mn1 N1 102.56(6) 7 8_556 ?
C1 O2 Mn1 138.47(9) . . ?
O1 C1 O2 126.50(13) . . ?
O1 C1 C2 117.08(12) . . ?
O2 C1 C2 116.41(12) . . ?
C3 C2 C6 117.89(13) . . ?
C3 C2 C1 120.91(13) . . ?
C6 C2 C1 121.20(12) . . ?
C2 C3 C4 118.51(15) . . ?
C1 O1 Mn1 157.34(10) . 5_665 ?
C5 N1 C6 116.68(12) . . ?
C5 N1 Mn1 124.27(10) . 7 ?
C6 N1 Mn1 118.47(9) . 7 ?
N1 C6 C2 124.51(12) . . ?
C5 C4 C3 119.42(15) . . ?
N1 C5 C4 122.98(15) . . ?
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 2.1305(10) 5_665 ?
Mn1 O1 2.1305(10) 6_566 ?
Mn1 O2 2.1947(10) . ?
Mn1 O2 2.1948(10) 2_655 ?
Mn1 N1 2.3526(12) 7 ?
Mn1 N1 2.3526(12) 8_556 ?
O2 C1 1.2593(17) . ?
C1 O1 1.2437(16) . ?
C1 C2 1.5208(19) . ?
C2 C3 1.387(2) . ?
C2 C6 1.3872(18) . ?
C3 C4 1.387(2) . ?
O1 Mn1 2.1305(10) 5_665 ?
N1 C5 1.3413(19) . ?
N1 C6 1.3414(18) . ?
N1 Mn1 2.3526(12) 7 ?
C4 C5 1.386(2) . ?
