#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:09:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179233 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/53/4315370.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_4315370
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            'C6 H4 Mn2 N10 O2'
_chemical_formula_weight         358.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 102.06(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.676(2)
_cell_length_b                   7.0135(14)
_cell_length_c                   14.839(3)
_cell_measurement_reflns_used    9411
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     1188.3(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9715
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_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    2.145
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0213P)²+0.7924P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0640
_reflns_number_gt                1632
_reflns_number_total             2088
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9021257_si_002_2.cif
_cod_data_source_block           2
_cod_database_code               4315370
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
N7 N 0.9335(3) 1.2131(4) 0.5262(2) 0.0364(8) Uani 1 1 d . . .
N6 N 0.8510(3) 1.1363(4) 0.4803(2) 0.0281(7) Uani 1 1 d . . .
O2 O 1.35683(18) 0.8740(3) 0.90314(14) 0.0239(5) Uani 1 1 d . . .
O1 O 1.40723(18) 0.5690(3) 0.93464(14) 0.0197(5) Uani 1 1 d . . .
C6 C 1.3426(3) 0.6993(4) 0.8884(2) 0.0162(7) Uani 1 1 d . . .
C2 C 1.2428(3) 0.4513(4) 0.7743(2) 0.0247(8) Uani 1 1 d . . .
H2A H 1.2948 0.3588 0.8032 0.030 Uiso 1 1 calc R . .
C3 C 1.2457(3) 0.6360(4) 0.8097(2) 0.0185(7) Uani 1 1 d . . .
C4 C 1.1606(3) 0.7666(4) 0.7684(2) 0.0240(8) Uani 1 1 d . . .
H4A H 1.1577 0.8885 0.7925 0.029 Uiso 1 1 calc R . .
Mn1 Mn 0.58773(4) 1.00188(7) 0.41751(3) 0.01676(13) Uani 1 1 d . . .
Mn2 Mn 0.5000 1.5000 0.5000 0.01568(15) Uani 1 2 d S . .
Mn3 Mn 1.0000 0.5000 0.5000 0.02100(17) Uani 1 2 d S . .
N8 N 0.5270(2) 1.3036(3) 0.38037(17) 0.0237(6) Uani 1 1 d . . .
N3 N 0.7367(2) 0.6650(4) 0.49544(17) 0.0224(6) Uani 1 1 d . . .
N9 N 0.4957(2) 1.3619(3) 0.30354(18) 0.0210(6) Uani 1 1 d . . .
N4 N 0.6353(2) 0.6991(3) 0.46417(18) 0.0214(6) Uani 1 1 d . . .
N1 N 1.0810(2) 0.5359(3) 0.65153(18) 0.0255(7) Uani 1 1 d . . .
N2 N 0.8347(2) 0.6342(4) 0.5274(2) 0.0365(8) Uani 1 1 d . . .
C5 C 1.0801(3) 0.7096(5) 0.6902(2) 0.0285(8) Uani 1 1 d . . .
H5A H 1.0226 0.7959 0.6631 0.034 Uiso 1 1 calc R . .
C1 C 1.1604(3) 0.4086(5) 0.6948(2) 0.0282(8) Uani 1 1 d . . .
H1A H 1.1600 0.2865 0.6703 0.034 Uiso 1 1 calc R . .
N5 N 0.7713(3) 1.0578(4) 0.4324(2) 0.0368(8) Uani 1 1 d . . .
N10 N 0.4647(3) 1.4191(4) 0.2293(2) 0.0392(8) Uani 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
N6 N7 Mn3 125.6(2) . 1_565 ?
N5 N6 N7 177.6(4) . . ?
C6 O2 Mn2 125.16(19) . 2_746 ?
C6 O1 Mn1 124.02(18) . 4_676 ?
C6 O1 Mn1 124.43(19) . 2_746 ?
Mn1 O1 Mn1 103.50(8) 4_676 2_746 ?
O2 C6 O1 124.1(3) . . ?
O2 C6 C3 118.3(3) . . ?
O1 C6 C3 117.6(3) . . ?
C1 C2 C3 118.5(3) . . ?
C1 C2 H2A 120.7 . . ?
C3 C2 H2A 120.7 . . ?
C4 C3 C2 119.0(3) . . ?
C4 C3 C6 119.7(3) . . ?
C2 C3 C6 121.3(3) . . ?
C5 C4 C3 118.2(3) . . ?
C5 C4 H4A 120.9 . . ?
C3 C4 H4A 120.9 . . ?
N5 Mn1 N10 102.36(12) . 2_645 ?
N5 Mn1 O1 167.60(10) . 4_475 ?
N10 Mn1 O1 88.87(10) 2_645 4_475 ?
N5 Mn1 O1 92.28(10) . 2_756 ?
N10 Mn1 O1 165.35(10) 2_645 2_756 ?
O1 Mn1 O1 76.50(8) 4_475 2_756 ?
N5 Mn1 N8 96.30(11) . . ?
N10 Mn1 N8 89.86(10) 2_645 . ?
O1 Mn1 N8 88.88(9) 4_475 . ?
O1 Mn1 N8 89.13(8) 2_756 . ?
N5 Mn1 N4 87.94(10) . . ?
N10 Mn1 N4 93.13(10) 2_645 . ?
O1 Mn1 N4 86.19(8) 4_475 . ?
O1 Mn1 N4 86.73(8) 2_756 . ?
N8 Mn1 N4 174.19(9) . . ?
O2 Mn2 O2 180.0 2_756 4_485 ?
O2 Mn2 N4 94.18(9) 2_756 3_676 ?
O2 Mn2 N4 85.82(9) 4_485 3_676 ?
O2 Mn2 N4 85.82(9) 2_756 1_565 ?
O2 Mn2 N4 94.18(9) 4_485 1_565 ?
N4 Mn2 N4 180.0 3_676 1_565 ?
O2 Mn2 N8 93.24(9) 2_756 . ?
O2 Mn2 N8 86.76(9) 4_485 . ?
N4 Mn2 N8 91.52(9) 3_676 . ?
N4 Mn2 N8 88.48(9) 1_565 . ?
O2 Mn2 N8 86.76(9) 2_756 3_686 ?
O2 Mn2 N8 93.24(9) 4_485 3_686 ?
N4 Mn2 N8 88.48(9) 3_676 3_686 ?
N4 Mn2 N8 91.52(9) 1_565 3_686 ?
N8 Mn2 N8 180.000(1) . 3_686 ?
N7 Mn3 N7 180.0 1_545 3_776 ?
N7 Mn3 N2 89.86(11) 1_545 3_766 ?
N7 Mn3 N2 90.14(11) 3_776 3_766 ?
N7 Mn3 N2 90.14(11) 1_545 . ?
N7 Mn3 N2 89.86(11) 3_776 . ?
N2 Mn3 N2 180.000(1) 3_766 . ?
N7 Mn3 N1 90.89(10) 1_545 . ?
N7 Mn3 N1 89.11(10) 3_776 . ?
N2 Mn3 N1 91.70(10) 3_766 . ?
N2 Mn3 N1 88.30(10) . . ?
N7 Mn3 N1 89.11(10) 1_545 3_766 ?
N7 Mn3 N1 90.89(10) 3_776 3_766 ?
N2 Mn3 N1 88.30(10) 3_766 3_766 ?
N2 Mn3 N1 91.70(10) . 3_766 ?
N1 Mn3 N1 180.0 . 3_766 ?
N9 N8 Mn1 124.8(2) . . ?
N9 N8 Mn2 117.7(2) . . ?
Mn1 N8 Mn2 117.04(11) . . ?
N2 N3 N4 178.5(3) . . ?
N10 N9 N8 179.4(3) . . ?
N3 N4 Mn2 117.9(2) . 1_545 ?
N3 N4 Mn1 117.6(2) . . ?
Mn2 N4 Mn1 120.88(11) 1_545 . ?
C5 N1 C1 117.5(3) . . ?
C5 N1 Mn3 119.0(2) . . ?
C1 N1 Mn3 120.2(2) . . ?
N3 N2 Mn3 143.9(3) . . ?
N1 C5 C4 123.4(3) . . ?
N1 C5 H5A 118.3 . . ?
C4 C5 H5A 118.3 . . ?
N1 C1 C2 123.1(3) . . ?
N1 C1 H1A 118.4 . . ?
C2 C1 H1A 118.4 . . ?
N6 N5 Mn1 142.3(3) . . ?
N9 N10 Mn1 174.3(3) . 2_655 ?
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
N7 N6 1.186(4) . ?
N7 Mn3 2.221(3) 1_565 ?
N6 N5 1.182(4) . ?
O2 C6 1.249(3) . ?
O2 Mn2 2.154(2) 2_746 ?
O1 C6 1.289(3) . ?
O1 Mn1 2.231(2) 4_676 ?
O1 Mn1 2.232(2) 2_746 ?
C6 C3 1.513(4) . ?
C2 C1 1.389(4) . ?
C2 C3 1.396(4) . ?
C2 H2A 0.9300 . ?
C3 C4 1.396(4) . ?
C4 C5 1.391(4) . ?
C4 H4A 0.9300 . ?
Mn1 N5 2.145(3) . ?
Mn1 N10 2.213(3) 2_645 ?
Mn1 O1 2.231(2) 4_475 ?
Mn1 O1 2.232(2) 2_756 ?
Mn1 N8 2.263(2) . ?
Mn1 N4 2.267(3) . ?
Mn2 O2 2.154(2) 2_756 ?
Mn2 O2 2.154(2) 4_485 ?
Mn2 N4 2.254(2) 3_676 ?
Mn2 N4 2.254(2) 1_565 ?
Mn2 N8 2.320(3) . ?
Mn2 N8 2.320(3) 3_686 ?
Mn3 N7 2.221(3) 1_545 ?
Mn3 N7 2.221(3) 3_776 ?
Mn3 N2 2.260(3) 3_766 ?
Mn3 N2 2.260(3) . ?
Mn3 N1 2.264(3) . ?
Mn3 N1 2.264(3) 3_766 ?
N8 N9 1.194(3) . ?
N3 N2 1.164(4) . ?
N3 N4 1.201(3) . ?
N9 N10 1.158(3) . ?
N4 Mn2 2.254(2) 1_545 ?
N1 C5 1.348(4) . ?
N1 C1 1.349(4) . ?
C5 H5A 0.9300 . ?
C1 H1A 0.9300 . ?
N10 Mn1 2.213(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
Mn3 N7 N6 N5 81(9) 1_565 . . . ?
Mn2 O2 C6 O1 5.7(4) 2_746 . . . ?
Mn2 O2 C6 C3 -172.52(19) 2_746 . . . ?
Mn1 O1 C6 O2 -75.7(3) 4_676 . . . ?
Mn1 O1 C6 O2 67.8(4) 2_746 . . . ?
Mn1 O1 C6 C3 102.5(3) 4_676 . . . ?
Mn1 O1 C6 C3 -113.9(2) 2_746 . . . ?
C1 C2 C3 C4 4.8(5) . . . . ?
C1 C2 C3 C6 -172.0(3) . . . . ?
O2 C6 C3 C4 -13.2(4) . . . . ?
O1 C6 C3 C4 168.4(3) . . . . ?
O2 C6 C3 C2 163.6(3) . . . . ?
O1 C6 C3 C2 -14.8(4) . . . . ?
C2 C3 C4 C5 -3.5(5) . . . . ?
C6 C3 C4 C5 173.3(3) . . . . ?
N5 Mn1 N8 N9 95.1(3) . . . . ?
N10 Mn1 N8 N9 -7.3(3) 2_645 . . . ?
O1 Mn1 N8 N9 -96.2(3) 4_475 . . . ?
O1 Mn1 N8 N9 -172.7(3) 2_756 . . . ?
N4 Mn1 N8 N9 -128.3(9) . . . . ?
N5 Mn1 N8 Mn2 -93.58(14) . . . . ?
N10 Mn1 N8 Mn2 164.00(14) 2_645 . . . ?
O1 Mn1 N8 Mn2 75.13(12) 4_475 . . . ?
O1 Mn1 N8 Mn2 -1.39(12) 2_756 . . . ?
N4 Mn1 N8 Mn2 43.0(10) . . . . ?
O2 Mn2 N8 N9 -153.5(2) 2_756 . . . ?
O2 Mn2 N8 N9 26.5(2) 4_485 . . . ?
N4 Mn2 N8 N9 112.3(2) 3_676 . . . ?
N4 Mn2 N8 N9 -67.7(2) 1_565 . . . ?
N8 Mn2 N8 N9 73(100) 3_686 . . . ?
O2 Mn2 N8 Mn1 34.58(13) 2_756 . . . ?
O2 Mn2 N8 Mn1 -145.42(13) 4_485 . . . ?
N4 Mn2 N8 Mn1 -59.70(13) 3_676 . . . ?
N4 Mn2 N8 Mn1 120.30(13) 1_565 . . . ?
N8 Mn2 N8 Mn1 -99(100) 3_686 . . . ?
Mn1 N8 N9 N10 137(39) . . . . ?
Mn2 N8 N9 N10 -34(39) . . . . ?
N2 N3 N4 Mn2 -86(13) . . . 1_545 ?
N2 N3 N4 Mn1 73(13) . . . . ?
N5 Mn1 N4 N3 11.0(2) . . . . ?
N10 Mn1 N4 N3 113.3(2) 2_645 . . . ?
O1 Mn1 N4 N3 -158.0(2) 4_475 . . . ?
O1 Mn1 N4 N3 -81.4(2) 2_756 . . . ?
N8 Mn1 N4 N3 -125.9(9) . . . . ?
N5 Mn1 N4 Mn2 169.17(14) . . . 1_545 ?
N10 Mn1 N4 Mn2 -88.55(15) 2_645 . . 1_545 ?
O1 Mn1 N4 Mn2 0.10(12) 4_475 . . 1_545 ?
O1 Mn1 N4 Mn2 76.78(13) 2_756 . . 1_545 ?
N8 Mn1 N4 Mn2 32.3(10) . . . 1_545 ?
N7 Mn3 N1 C5 -143.5(3) 1_545 . . . ?
N7 Mn3 N1 C5 36.5(3) 3_776 . . . ?
N2 Mn3 N1 C5 126.7(3) 3_766 . . . ?
N2 Mn3 N1 C5 -53.3(3) . . . . ?
N1 Mn3 N1 C5 -50(100) 3_766 . . . ?
N7 Mn3 N1 C1 57.8(3) 1_545 . . . ?
N7 Mn3 N1 C1 -122.2(3) 3_776 . . . ?
N2 Mn3 N1 C1 -32.0(3) 3_766 . . . ?
N2 Mn3 N1 C1 148.0(3) . . . . ?
N1 Mn3 N1 C1 151(100) 3_766 . . . ?
N4 N3 N2 Mn3 -176(100) . . . . ?
N7 Mn3 N2 N3 -79.0(4) 1_545 . . . ?
N7 Mn3 N2 N3 101.0(4) 3_776 . . . ?
N2 Mn3 N2 N3 91(100) 3_766 . . . ?
N1 Mn3 N2 N3 -169.9(4) . . . . ?
N1 Mn3 N2 N3 10.1(4) 3_766 . . . ?
C1 N1 C5 C4 4.0(5) . . . . ?
Mn3 N1 C5 C4 -155.3(3) . . . . ?
C3 C4 C5 N1 -0.9(5) . . . . ?
C5 N1 C1 C2 -2.6(5) . . . . ?
Mn3 N1 C1 C2 156.4(3) . . . . ?
C3 C2 C1 N1 -1.7(5) . . . . ?
N7 N6 N5 Mn1 -177(100) . . . . ?
N10 Mn1 N5 N6 161.2(4) 2_645 . . . ?
O1 Mn1 N5 N6 -44.3(7) 4_475 . . . ?
O1 Mn1 N5 N6 -19.4(4) 2_756 . . . ?
N8 Mn1 N5 N6 70.0(4) . . . . ?
N4 Mn1 N5 N6 -106.0(4) . . . . ?
N8 N9 N10 Mn1 -149(37) . . . 2_655 ?
