#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/59/2235974.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2235974
loop_
_publ_author_name
'Wang, Jun'
'Zhu, Wubiao'
'Li, Jichang'
_publ_section_title
;
 catena-Poly[[(2-{[2-(dimethylammonio)ethyl]iminomethyl}pyridine-κ²N,N')bis(thiocyanato-κN)manganese(II)]-μ-thiocyanato-κ²N:S]
;
_journal_coeditor_code           RZ2792
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1131
_journal_paper_doi               10.1107/S1600536812032874
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Mn (N C S)3 (C10 H16 N3)]'
_chemical_formula_moiety         'C13 H16 Mn N6 S3'
_chemical_formula_sum            'C13 H16 Mn N6 S3'
_chemical_formula_weight         407.44
_chemical_name_systematic
;
catena-Poly[[(2-{[2-(dimethylammonio)ethyl]iminomethyl}pyridine-
κ²N,N')bis(thiocyanato-κN)manganese(II)]-
μ-thiocyanato-κ²N:S]
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.5603(12)
_cell_length_b                   11.0699(15)
_cell_length_c                   37.346(5)
_cell_measurement_reflns_used    3600
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      1.16
_cell_volume                     3539.0(8)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_diffrn_measurement_method       'φ and ω scan'
_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  0.0757
_diffrn_reflns_av_sigmaI/netI    0.0564
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            18847
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.18
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_T_max  0.8880
_exptl_absorpt_correction_T_min  0.7695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.349
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0430
_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)+(0.0371P)²+0.1816P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0980
_reflns_number_gt                2397
_reflns_number_total             3660
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            rz2792.cif
_cod_data_source_block           I
_cod_database_code               2235974
_cod_database_fobs_code          2235974
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'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
C C1 0.8026(4) 1.0515(3) 0.29186(7) 0.0365(7) Uani d . 1 1
H H1 0.8775 1.1075 0.2848 0.044 Uiso calc R 1 1
C C2 0.6523(4) 1.0652(3) 0.27924(8) 0.0427(8) Uani d . 1 1
H H2 0.6263 1.1293 0.2643 0.051 Uiso calc R 1 1
C C3 0.5419(4) 0.9820(3) 0.28924(8) 0.0470(9) Uani d . 1 1
H H3A 0.4396 0.9885 0.2811 0.056 Uiso calc R 1 1
C C4 0.5847(4) 0.8885(3) 0.31150(8) 0.0390(8) Uani d . 1 1
H H4 0.5115 0.8311 0.3185 0.047 Uiso calc R 1 1
C C5 0.7368(4) 0.8806(3) 0.32342(7) 0.0328(7) Uani d . 1 1
C C6 0.7882(4) 0.7845(3) 0.34732(8) 0.0365(8) Uani d . 1 1
H H6 0.7188 0.7237 0.3539 0.044 Uiso calc R 1 1
C C7 0.9714(4) 0.6847(3) 0.38312(8) 0.0400(8) Uani d . 1 1
H H7A 1.0726 0.6528 0.3762 0.048 Uiso calc R 1 1
H H7B 0.8954 0.6198 0.3818 0.048 Uiso calc R 1 1
C C8 0.9784(4) 0.7345(3) 0.42070(8) 0.0381(8) Uani d . 1 1
H H8A 1.0409 0.8076 0.4207 0.046 Uiso calc R 1 1
H H8B 0.8736 0.7561 0.4283 0.046 Uiso calc R 1 1
C C9 1.2174(4) 0.6312(3) 0.44276(10) 0.0601(11) Uani d . 1 1
H H9A 1.2693 0.7068 0.4469 0.090 Uiso calc R 1 1
H H9B 1.2399 0.6036 0.4189 0.090 Uiso calc R 1 1
H H9C 1.2538 0.5726 0.4598 0.090 Uiso calc R 1 1
C C10 1.0076(5) 0.6853(4) 0.48428(8) 0.0679(12) Uani d . 1 1
H H10A 1.0542 0.6297 0.5009 0.102 Uiso calc R 1 1
H H10B 0.8963 0.6854 0.4874 0.102 Uiso calc R 1 1
H H10C 1.0477 0.7650 0.4885 0.102 Uiso calc R 1 1
C C11 1.3790(4) 0.8798(3) 0.39279(8) 0.0358(7) Uani d . 1 1
C C12 0.9167(4) 1.0407(3) 0.41865(10) 0.0411(8) Uani d . 1 1
C C13 1.2401(4) 1.1848(3) 0.30617(8) 0.0351(7) Uani d . 1 1
Mn Mn1 1.07355(5) 0.94723(4) 0.344285(12) 0.03482(15) Uani d . 1 1
N N1 0.8468(3) 0.9621(2) 0.31373(6) 0.0312(6) Uani d . 1 1
N N2 0.9266(3) 0.7830(2) 0.35923(6) 0.0335(6) Uani d . 1 1
N N3 1.0459(3) 0.6475(2) 0.44693(7) 0.0398(7) Uani d . 1 1
N N4 1.2709(3) 0.8875(2) 0.37436(7) 0.0469(7) Uani d . 1 1
N N5 0.9625(4) 1.0375(2) 0.38952(8) 0.0500(8) Uani d . 1 1
N N6 1.1752(3) 1.1042(2) 0.31952(7) 0.0447(7) Uani d . 1 1
H H3 0.9996 0.5806 0.4412 0.067 Uiso d R 1 1
S S1 1.53139(11) 0.87179(8) 0.41894(2) 0.0482(3) Uani d . 1 1
S S2 0.85784(14) 1.04061(10) 0.46007(2) 0.0646(3) Uani d . 1 1
S S3 1.32720(10) 1.29615(7) 0.28601(2) 0.0427(2) Uani d . 1 1
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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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_site_symmetry_3
_geom_angle
N1 C1 C2 . 123.6(3)
N1 C1 H1 . 118.2
C2 C1 H1 . 118.2
C3 C2 C1 . 118.4(3)
C3 C2 H2 . 120.8
C1 C2 H2 . 120.8
C2 C3 C4 . 119.0(3)
C2 C3 H3A . 120.5
C4 C3 H3A . 120.5
C3 C4 C5 . 119.6(3)
C3 C4 H4 . 120.2
C5 C4 H4 . 120.2
N1 C5 C4 . 121.9(3)
N1 C5 C6 . 116.1(3)
C4 C5 C6 . 122.0(3)
N2 C6 C5 . 120.5(3)
N2 C6 H6 . 119.8
C5 C6 H6 . 119.8
N2 C7 C8 . 107.8(2)
N2 C7 H7A . 110.1
C8 C7 H7A . 110.1
N2 C7 H7B . 110.1
C8 C7 H7B . 110.1
H7A C7 H7B . 108.5
N3 C8 C7 . 113.0(2)
N3 C8 H8A . 109.0
C7 C8 H8A . 109.0
N3 C8 H8B . 109.0
C7 C8 H8B . 109.0
H8A C8 H8B . 107.8
N3 C9 H9A . 109.5
N3 C9 H9B . 109.5
H9A C9 H9B . 109.5
N3 C9 H9C . 109.5
H9A C9 H9C . 109.5
H9B C9 H9C . 109.5
N3 C10 H10A . 109.5
N3 C10 H10B . 109.5
H10A C10 H10B . 109.5
N3 C10 H10C . 109.5
H10A C10 H10C . 109.5
H10B C10 H10C . 109.5
N4 C11 S1 . 178.9(3)
N5 C12 S2 . 177.5(3)
N6 C13 S3 . 177.7(3)
N4 Mn1 N6 . 98.99(11)
N4 Mn1 N5 . 94.55(11)
N6 Mn1 N5 . 98.00(10)
N4 Mn1 N1 . 165.80(10)
N6 Mn1 N1 . 94.10(9)
N5 Mn1 N1 . 89.04(10)
N4 Mn1 N2 . 93.50(10)
N6 Mn1 N2 . 166.41(10)
N5 Mn1 N2 . 86.27(10)
N1 Mn1 N2 . 72.99(9)
N4 Mn1 S3 8_855 89.10(8)
N6 Mn1 S3 8_855 91.43(7)
N5 Mn1 S3 8_855 169.22(8)
N1 Mn1 S3 8_855 85.06(6)
N2 Mn1 S3 8_855 83.38(6)
C1 N1 C5 . 117.3(3)
C1 N1 Mn1 . 127.3(2)
C5 N1 Mn1 . 114.49(19)
C6 N2 C7 . 118.1(3)
C6 N2 Mn1 . 114.85(19)
C7 N2 Mn1 . 126.8(2)
C9 N3 C10 . 110.4(3)
C9 N3 C8 . 113.1(3)
C10 N3 C8 . 110.4(3)
C9 N3 H3 . 108.7
C10 N3 H3 . 111.8
C8 N3 H3 . 102.2
C11 N4 Mn1 . 165.9(3)
C12 N5 Mn1 . 152.9(3)
C13 N6 Mn1 . 175.2(3)
C13 S3 Mn1 8_865 103.08(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 N1 . 1.337(3)
C1 C2 . 1.379(4)
C1 H1 . 0.9300
C2 C3 . 1.371(5)
C2 H2 . 0.9300
C3 C4 . 1.377(4)
C3 H3A . 0.9300
C4 C5 . 1.379(4)
C4 H4 . 0.9300
C5 N1 . 1.354(4)
C5 C6 . 1.457(4)
C6 N2 . 1.266(4)
C6 H6 . 0.9300
C7 N2 . 1.459(3)
C7 C8 . 1.509(4)
C7 H7A . 0.9700
C7 H7B . 0.9700
C8 N3 . 1.490(4)
C8 H8A . 0.9700
C8 H8B . 0.9700
C9 N3 . 1.487(4)
C9 H9A . 0.9600
C9 H9B . 0.9600
C9 H9C . 0.9600
C10 N3 . 1.492(4)
C10 H10A . 0.9600
C10 H10B . 0.9600
C10 H10C . 0.9600
C11 N4 . 1.157(4)
C11 S1 . 1.632(3)
C12 N5 . 1.157(4)
C12 S2 . 1.627(4)
C13 N6 . 1.162(4)
C13 S3 . 1.626(3)
Mn1 N4 . 2.133(3)
Mn1 N6 . 2.153(3)
Mn1 N5 . 2.181(3)
Mn1 N1 . 2.257(2)
Mn1 N2 . 2.280(2)
Mn1 S3 8_855 2.8731(10)
N3 H3 . 0.8675
S3 Mn1 8_865 2.8732(10)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N3 H3 S1 8_855 0.87 2.47 3.294(3) 158.7
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_site_symmetry_1
_geom_torsion
N1 C1 C2 C3 . -0.8(5)
C1 C2 C3 C4 . 0.3(5)
C2 C3 C4 C5 . 0.3(5)
C3 C4 C5 N1 . -0.3(5)
C3 C4 C5 C6 . 179.3(3)
N1 C5 C6 N2 . 3.2(4)
C4 C5 C6 N2 . -176.4(3)
N2 C7 C8 N3 . -171.4(3)
C2 C1 N1 C5 . 0.8(4)
C2 C1 N1 Mn1 . -167.9(2)
C4 C5 N1 C1 . -0.2(4)
C6 C5 N1 C1 . -179.9(2)
C4 C5 N1 Mn1 . 169.9(2)
C6 C5 N1 Mn1 . -9.8(3)
N4 Mn1 N1 C1 . -163.6(4)
N6 Mn1 N1 C1 . -6.4(2)
N5 Mn1 N1 C1 . 91.5(2)
N2 Mn1 N1 C1 . 177.9(2)
S3 Mn1 N1 C1 8_855 -97.5(2)
N4 Mn1 N1 C5 . 27.5(5)
N6 Mn1 N1 C5 . -175.4(2)
N5 Mn1 N1 C5 . -77.4(2)
N2 Mn1 N1 C5 . 8.97(19)
S3 Mn1 N1 C5 8_855 93.54(19)
C5 C6 N2 C7 . 179.9(2)
C5 C6 N2 Mn1 . 5.0(4)
C8 C7 N2 C6 . -104.8(3)
C8 C7 N2 Mn1 . 69.3(3)
N4 Mn1 N2 C6 . 177.1(2)
N6 Mn1 N2 C6 . -26.1(5)
N5 Mn1 N2 C6 . 82.8(2)
N1 Mn1 N2 C6 . -7.4(2)
S3 Mn1 N2 C6 8_855 -94.2(2)
N4 Mn1 N2 C7 . 2.8(2)
N6 Mn1 N2 C7 . 159.5(4)
N5 Mn1 N2 C7 . -91.6(2)
N1 Mn1 N2 C7 . 178.3(2)
S3 Mn1 N2 C7 8_855 91.4(2)
C7 C8 N3 C9 . 72.4(4)
C7 C8 N3 C10 . -163.3(3)
N6 Mn1 N4 C11 . 48.5(11)
N5 Mn1 N4 C11 . -50.4(11)
N1 Mn1 N4 C11 . -154.6(9)
N2 Mn1 N4 C11 . -136.9(11)
S3 Mn1 N4 C11 8_855 139.8(11)
N4 Mn1 N5 C12 . -50.7(6)
N6 Mn1 N5 C12 . -150.4(6)
N1 Mn1 N5 C12 . 115.6(6)
N2 Mn1 N5 C12 . 42.5(6)
S3 Mn1 N5 C12 8_855 58.8(9)
