#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:09:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179233 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/53/4315369.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_4315369
loop_
_publ_author_name
'Qian Yang'
'Jiong-Peng Zhao'
'Bo-Wen Hu'
'Xiao-Feng Zhang'
'Xian-He Bu'
_publ_section_title
;
 New Manganese(II) Azido Coordination Polymers with Nicotinic/Isonicotinic
 Acids as Coligands: Synthesis, Structure, and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3746
_journal_page_last               3751
_journal_paper_doi               10.1021/ic9021257
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C12 H10 Mn3 N14 O5'
_chemical_formula_weight         595.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.45(3)
_cell_angle_beta                 98.74(3)
_cell_angle_gamma                98.23(3)
_cell_formula_units_Z            1
_cell_length_a                   6.9439(14)
_cell_length_b                   7.8714(16)
_cell_length_c                   9.840(2)
_cell_measurement_reflns_used    5037
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     508.0(2)
_computing_cell_refinement       'Bruker SMART APEX II'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  SCX-MINI
_diffrn_measurement_method       'phi and omega scans'
_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  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4397
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.898
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.945
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             295
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         1794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0344P)²+0.6188P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0790
_reflns_number_gt                1624
_reflns_number_total             1794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9021257_si_002_1.cif
_cod_data_source_block           1
_cod_original_cell_volume        508.02(18)
_cod_database_code               4315369
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
N3 N -0.1255(4) 0.7321(3) 0.5330(3) 0.0206(6) Uani 1 1 d . . .
N1 N 0.0922(4) 0.6174(4) 0.6799(3) 0.0277(6) Uani 1 1 d . . .
O1 O 0.6507(4) 0.6706(3) 1.2157(2) 0.0319(6) Uani 1 1 d . . .
C6 C 0.7317(5) 0.8149(4) 1.1981(3) 0.0210(7) Uani 1 1 d . . .
Mn1 Mn 1.0000 0.0000 0.5000 0.01654(17) Uani 1 2 d S . .
Mn2 Mn 0.35738(7) 0.47835(6) 0.63331(4) 0.01611(15) Uani 1 1 d . . .
N5 N 0.6796(4) 0.2521(3) 0.5593(3) 0.0203(6) Uani 1 1 d . . .
N4 N 0.6092(4) 0.3774(3) 0.5446(3) 0.0209(6) Uani 1 1 d . . .
N6 N 0.7455(5) 0.1294(4) 0.5729(3) 0.0385(8) Uani 1 1 d . . .
N7 N 0.5447(4) 0.7137(3) 0.8010(3) 0.0213(6) Uani 1 1 d . . .
C1 C 0.6167(5) 0.8684(4) 0.7763(3) 0.0230(7) Uani 1 1 d . . .
H1A H 0.5922 0.8793 0.6835 0.028 Uiso 1 1 calc R . .
C4 C 0.6930(4) 0.8394(4) 1.0491(3) 0.0201(6) Uani 1 1 d . . .
C5 C 0.5833(5) 0.7033(4) 0.9368(3) 0.0268(7) Uani 1 1 d . . .
H5A H 0.5327 0.5974 0.9563 0.032 Uiso 1 1 calc R . .
C3 C 0.7651(5) 0.9978(4) 1.0204(3) 0.0234(7) Uani 1 1 d . . .
H3A H 0.8391 1.0930 1.0930 0.028 Uiso 1 1 calc R . .
C2 C 0.7252(5) 1.0121(4) 0.8818(3) 0.0274(7) Uani 1 1 d . . .
H2A H 0.7712 1.1176 0.8601 0.033 Uiso 1 1 calc R . .
O2 O 0.8421(4) 0.9393(3) 1.2908(2) 0.0327(6) Uani 1 1 d . . .
N2 N -0.0139(4) 0.6740(3) 0.6072(3) 0.0174(5) Uani 1 1 d . . .
O1W O 0.0000 0.5000 0.0000 0.309(10) Uani 1 2 d S . .
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'
Mn Mn 0.3368 0.7283 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 N3 Mn1 115.09(19) . 1_465 ?
N2 N3 Mn2 114.49(19) . 2_566 ?
Mn1 N3 Mn2 123.43(11) 1_465 2_566 ?
N2 N1 Mn2 130.2(2) . . ?
C6 O1 Mn2 142.4(2) . 2_667 ?
O2 C6 O1 126.4(3) . . ?
O2 C6 C4 116.5(3) . . ?
O1 C6 C4 117.0(3) . . ?
O2 Mn1 O2 180.0 1_544 2_767 ?
O2 Mn1 N3 93.47(9) 1_544 1_645 ?
O2 Mn1 N3 86.53(9) 2_767 1_645 ?
O2 Mn1 N3 86.53(9) 1_544 2_666 ?
O2 Mn1 N3 93.47(9) 2_767 2_666 ?
N3 Mn1 N3 180.0 1_645 2_666 ?
O2 Mn1 N6 91.77(11) 1_544 2_756 ?
O2 Mn1 N6 88.23(11) 2_767 2_756 ?
N3 Mn1 N6 86.42(10) 1_645 2_756 ?
N3 Mn1 N6 93.58(10) 2_666 2_756 ?
O2 Mn1 N6 88.23(11) 1_544 . ?
O2 Mn1 N6 91.77(11) 2_767 . ?
N3 Mn1 N6 93.58(10) 1_645 . ?
N3 Mn1 N6 86.42(10) 2_666 . ?
N6 Mn1 N6 180.000(1) 2_756 . ?
O1 Mn2 N4 96.62(10) 2_667 . ?
O1 Mn2 N7 90.37(9) 2_667 . ?
N4 Mn2 N7 96.16(10) . . ?
O1 Mn2 N3 92.47(9) 2_667 2_566 ?
N4 Mn2 N3 92.89(10) . 2_566 ?
N7 Mn2 N3 170.14(9) . 2_566 ?
O1 Mn2 N4 173.36(10) 2_667 2_666 ?
N4 Mn2 N4 76.88(10) . 2_666 ?
N7 Mn2 N4 91.64(9) . 2_666 ?
N3 Mn2 N4 86.61(9) 2_566 2_666 ?
O1 Mn2 N1 97.47(10) 2_667 . ?
N4 Mn2 N1 165.83(10) . . ?
N7 Mn2 N1 85.31(10) . . ?
N3 Mn2 N1 84.96(10) 2_566 . ?
N4 Mn2 N1 89.00(10) 2_666 . ?
N6 N5 N4 179.1(3) . . ?
N5 N4 Mn2 128.9(2) . . ?
N5 N4 Mn2 125.9(2) . 2_666 ?
Mn2 N4 Mn2 103.12(10) . 2_666 ?
N5 N6 Mn1 135.8(2) . . ?
C1 N7 C5 116.6(3) . . ?
C1 N7 Mn2 124.4(2) . . ?
C5 N7 Mn2 119.0(2) . . ?
N7 C1 C2 123.2(3) . . ?
N7 C1 H1A 118.4 . . ?
C2 C1 H1A 118.4 . . ?
C5 C4 C3 117.8(3) . . ?
C5 C4 C6 120.7(3) . . ?
C3 C4 C6 121.5(3) . . ?
N7 C5 C4 124.3(3) . . ?
N7 C5 H5A 117.8 . . ?
C4 C5 H5A 117.8 . . ?
C4 C3 C2 118.8(3) . . ?
C4 C3 H3A 120.6 . . ?
C2 C3 H3A 120.6 . . ?
C1 C2 C3 119.3(3) . . ?
C1 C2 H2A 120.3 . . ?
C3 C2 H2A 120.3 . . ?
C6 O2 Mn1 141.1(2) . 1_566 ?
N1 N2 N3 179.2(3) . . ?
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
N3 N2 1.195(3) . ?
N3 Mn1 2.278(3) 1_465 ?
N3 Mn2 2.278(3) 2_566 ?
N1 N2 1.155(4) . ?
N1 Mn2 2.324(3) . ?
O1 C6 1.255(4) . ?
O1 Mn2 2.098(2) 2_667 ?
C6 O2 1.239(4) . ?
C6 C4 1.512(4) . ?
Mn1 O2 2.092(2) 1_544 ?
Mn1 O2 2.092(2) 2_767 ?
Mn1 N3 2.278(3) 1_645 ?
Mn1 N3 2.278(3) 2_666 ?
Mn1 N6 2.288(3) 2_756 ?
Mn1 N6 2.288(3) . ?
Mn2 O1 2.098(2) 2_667 ?
Mn2 N4 2.234(3) . ?
Mn2 N7 2.255(3) . ?
Mn2 N3 2.278(3) 2_566 ?
Mn2 N4 2.320(3) 2_666 ?
N5 N6 1.152(4) . ?
N5 N4 1.190(3) . ?
N4 Mn2 2.320(3) 2_666 ?
N7 C1 1.338(4) . ?
N7 C5 1.346(4) . ?
C1 C2 1.377(5) . ?
C1 H1A 0.9300 . ?
C4 C5 1.382(4) . ?
C4 C3 1.383(4) . ?
C5 H5A 0.9300 . ?
C3 C2 1.384(4) . ?
C3 H3A 0.9300 . ?
C2 H2A 0.9300 . ?
O2 Mn1 2.092(2) 1_566 ?
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
Mn2 O1 C6 O2 -7.3(6) 2_667 . . . ?
Mn2 O1 C6 C4 172.1(2) 2_667 . . . ?
N2 N1 Mn2 O1 -154.0(3) . . . 2_667 ?
N2 N1 Mn2 N4 19.6(6) . . . . ?
N2 N1 Mn2 N7 116.2(3) . . . . ?
N2 N1 Mn2 N3 -62.2(3) . . . 2_566 ?
N2 N1 Mn2 N4 24.5(3) . . . 2_666 ?
N6 N5 N4 Mn2 54(19) . . . . ?
N6 N5 N4 Mn2 -107(19) . . . 2_666 ?
O1 Mn2 N4 N5 14.4(3) 2_667 . . . ?
N7 Mn2 N4 N5 105.5(3) . . . . ?
N3 Mn2 N4 N5 -78.5(3) 2_566 . . . ?
N4 Mn2 N4 N5 -164.3(3) 2_666 . . . ?
N1 Mn2 N4 N5 -159.3(3) . . . . ?
O1 Mn2 N4 Mn2 178.66(10) 2_667 . . 2_666 ?
N7 Mn2 N4 Mn2 -90.25(11) . . . 2_666 ?
N3 Mn2 N4 Mn2 85.84(11) 2_566 . . 2_666 ?
N4 Mn2 N4 Mn2 0.0 2_666 . . 2_666 ?
N1 Mn2 N4 Mn2 5.0(4) . . . 2_666 ?
N4 N5 N6 Mn1 128(19) . . . . ?
O2 Mn1 N6 N5 -66.7(4) 1_544 . . . ?
O2 Mn1 N6 N5 113.3(4) 2_767 . . . ?
N3 Mn1 N6 N5 -160.0(4) 1_645 . . . ?
N3 Mn1 N6 N5 20.0(4) 2_666 . . . ?
N6 Mn1 N6 N5 22(100) 2_756 . . . ?
O1 Mn2 N7 C1 177.7(3) 2_667 . . . ?
N4 Mn2 N7 C1 81.0(3) . . . . ?
N3 Mn2 N7 C1 -75.6(6) 2_566 . . . ?
N4 Mn2 N7 C1 4.0(3) 2_666 . . . ?
N1 Mn2 N7 C1 -84.9(3) . . . . ?
O1 Mn2 N7 C5 -4.6(3) 2_667 . . . ?
N4 Mn2 N7 C5 -101.3(2) . . . . ?
N3 Mn2 N7 C5 102.1(5) 2_566 . . . ?
N4 Mn2 N7 C5 -178.3(2) 2_666 . . . ?
N1 Mn2 N7 C5 92.8(3) . . . . ?
C5 N7 C1 C2 0.0(5) . . . . ?
Mn2 N7 C1 C2 177.8(3) . . . . ?
O2 C6 C4 C5 175.4(3) . . . . ?
O1 C6 C4 C5 -4.0(5) . . . . ?
O2 C6 C4 C3 -4.7(5) . . . . ?
O1 C6 C4 C3 175.8(3) . . . . ?
C1 N7 C5 C4 -1.0(5) . . . . ?
Mn2 N7 C5 C4 -178.8(3) . . . . ?
C3 C4 C5 N7 1.1(5) . . . . ?
C6 C4 C5 N7 -179.0(3) . . . . ?
C5 C4 C3 C2 -0.3(5) . . . . ?
C6 C4 C3 C2 179.8(3) . . . . ?
N7 C1 C2 C3 0.7(5) . . . . ?
C4 C3 C2 C1 -0.5(5) . . . . ?
O1 C6 O2 Mn1 11.8(6) . . . 1_566 ?
C4 C6 O2 Mn1 -167.6(3) . . . 1_566 ?
Mn2 N1 N2 N3 150(21) . . . . ?
Mn1 N3 N2 N1 133(21) 1_465 . . . ?
Mn2 N3 N2 N1 -75(21) 2_566 . . . ?
