#------------------------------------------------------------------------------
#$Date: 2018-01-26 10:35:08 +0200 (Fri, 26 Jan 2018) $
#$Revision: 205716 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/23/2242332.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_2242332
loop_
_publ_author_name
'Neumann, Tristan'
'Jess, Inke'
'Näther, Christian'
_publ_section_title
;
 Crystal structures of bis[4-(dimethylamino)pyridinium]
 tetrakis(thiocyanato-κN)manganate(II) and
 tris[4-(dimethylamino)pyridinium]
 pentakis(thiocyanato-κN)manganate(II)
;
_journal_coeditor_code           WM5426
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              15
_journal_page_last               20
_journal_paper_doi               10.1107/S2056989017017510
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '(C7 H11 N2)2 [Mn (N C S)4]'
_chemical_formula_moiety         '2(C7 H11 N2 +), C4 Mn N4 S4 2-'
_chemical_formula_sum            'C18 H22 Mn N8 S4'
_chemical_formula_weight         533.61
_chemical_name_systematic
;
Bis[4-(dimethylamino)pyridinium]
tetrakis(thiocyanato-κN)manganate(II)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                93.748(4)
_cell_angle_beta                 90.464(4)
_cell_angle_gamma                112.585(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5079(4)
_cell_length_b                   10.4356(5)
_cell_length_c                   14.9899(7)
_cell_measurement_reflns_used    17932
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.999
_cell_measurement_theta_min      2.119
_cell_volume                     1225.39(10)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2008)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2008)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2008)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         2.119
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_T_max  0.9149
_exptl_absorpt_correction_T_min  0.5929
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-SHAPE and X-RED32; Stoe & Cie, 2008)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             550
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.530
_refine_ls_extinction_coef       0.017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0601P)²+0.0944P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0975
_reflns_number_gt                4633
_reflns_number_total             5342
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5426sup1.cif
_cod_data_source_block           Compound1
_cod_database_code               2242332
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2.014
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_occupancy
Mn Mn1 0.90952(3) 0.88265(3) 1.18620(2) 0.03782(10) Uani d 1
N N1 0.6639(2) 0.74716(16) 1.15632(11) 0.0426(3) Uani d 1
C C1 0.5334(2) 0.65751(19) 1.13644(12) 0.0388(4) Uani d 1
S S1 0.35333(7) 0.53200(6) 1.10859(4) 0.05316(15) Uani d 1
N N2 1.0772(2) 0.80600(17) 1.23903(11) 0.0451(4) Uani d 1
C C2 1.1541(2) 0.76211(19) 1.28340(12) 0.0402(4) Uani d 1
S S2 1.26376(9) 0.70138(7) 1.34362(4) 0.06153(18) Uani d 1
N N3 0.9843(2) 1.05670(15) 1.11196(10) 0.0415(3) Uani d 1
C C3 0.9911(2) 1.13584(17) 1.05982(12) 0.0356(3) Uani d 1
S S3 0.99897(6) 1.24678(4) 0.98674(3) 0.04241(13) Uani d 1
N N4 0.8810(2) 0.98070(17) 1.31098(11) 0.0470(4) Uani d 1
C C4 0.8722(2) 1.04124(18) 1.37713(13) 0.0400(4) Uani d 1
S S4 0.85130(7) 1.12578(5) 1.46840(3) 0.05017(14) Uani d 1
N N11 0.6345(2) 1.00661(18) 0.90468(12) 0.0496(4) Uani d 1
H H11A 0.7252 1.0809 0.9219 0.060 Uiso calc 1
C C11 0.5288(3) 1.0139(2) 0.84009(15) 0.0488(5) Uani d 1
H H11 0.5525 1.0994 0.8137 0.059 Uiso calc 1
C C12 0.3886(2) 0.90088(19) 0.81197(14) 0.0427(4) Uani d 1
H H12 0.3155 0.9081 0.7660 0.051 Uiso calc 1
C C13 0.3498(2) 0.77195(18) 0.85038(12) 0.0370(4) Uani d 1
C C14 0.4655(2) 0.7706(2) 0.91879(13) 0.0441(4) Uani d 1
H H14 0.4458 0.6875 0.9474 0.053 Uiso calc 1
C C15 0.6036(3) 0.8871(2) 0.94344(14) 0.0498(5) Uani d 1
H H15 0.6802 0.8844 0.9890 0.060 Uiso calc 1
N N12 0.2129(2) 0.65910(15) 0.82409(11) 0.0418(3) Uani d 1
C C16 0.0935(3) 0.6621(2) 0.75498(14) 0.0514(5) Uani d 1
H H16A 0.0405 0.7267 0.7753 0.077 Uiso calc 1
H H16B 0.0053 0.5686 0.7429 0.077 Uiso calc 1
H H16C 0.1545 0.6930 0.7002 0.077 Uiso calc 1
C C17 0.1683(3) 0.5301(2) 0.86837(16) 0.0534(5) Uani d 1
H H17A 0.2515 0.4884 0.8543 0.080 Uiso calc 1
H H17B 0.0544 0.4651 0.8473 0.080 Uiso calc 1
H H17C 0.1691 0.5500 0.9332 0.080 Uiso calc 1
N N21 0.2097(2) 0.34211(19) 0.56590(13) 0.0546(4) Uani d 1
H H21A 0.1323 0.2595 0.5488 0.066 Uiso calc 1
C C21 0.3276(3) 0.3541(2) 0.62914(15) 0.0523(5) Uani d 1
H H21 0.3262 0.2730 0.6550 0.063 Uiso calc 1
C C22 0.4485(3) 0.4792(2) 0.65702(13) 0.0465(4) Uani d 1
H H22 0.5300 0.4850 0.7024 0.056 Uiso calc 1
C C23 0.4545(2) 0.60157(19) 0.61898(12) 0.0389(4) Uani d 1
C C24 0.3267(3) 0.5837(2) 0.55258(14) 0.0483(4) Uani d 1
H H24 0.3240 0.6623 0.5250 0.058 Uiso calc 1
C C25 0.2088(3) 0.4556(2) 0.52819(15) 0.0550(5) Uani d 1
H H25 0.1237 0.4454 0.4837 0.066 Uiso calc 1
N N22 0.5730(2) 0.72629(17) 0.64412(12) 0.0487(4) Uani d 1
C C26 0.7061(3) 0.7430(3) 0.71058(18) 0.0656(6) Uani d 1
H H26A 0.6552 0.6923 0.7626 0.098 Uiso calc 1
H H26B 0.7660 0.8420 0.7292 0.098 Uiso calc 1
H H26C 0.7870 0.7061 0.6847 0.098 Uiso calc 1
C C27 0.5877(4) 0.8505(2) 0.59983(18) 0.0678(7) Uani d 1
H H27A 0.6025 0.8358 0.5357 0.102 Uiso calc 1
H H27B 0.6864 0.9301 0.6255 0.102 Uiso calc 1
H H27C 0.4842 0.8691 0.6085 0.102 Uiso calc 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'
S S 0.1246 0.1234 '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_publ_flag
N1 Mn1 N2 118.35(7) y
N1 Mn1 N3 112.93(6) y
N2 Mn1 N3 123.57(7) y
N1 Mn1 N4 101.27(7) y
N2 Mn1 N4 93.83(7) y
N3 Mn1 N4 97.99(6) y
C1 N1 Mn1 171.10(15) ?
N1 C1 S1 179.42(18) ?
C2 N2 Mn1 166.86(16) ?
N2 C2 S2 178.85(18) ?
C3 N3 Mn1 164.22(15) ?
N3 C3 S3 179.51(17) ?
C4 N4 Mn1 175.99(16) ?
N4 C4 S4 177.36(18) ?
C11 N11 C15 120.80(18) ?
C11 N11 H11A 119.6 ?
C15 N11 H11A 119.6 ?
N11 C11 C12 120.89(18) ?
N11 C11 H11 119.6 ?
C12 C11 H11 119.6 ?
C11 C12 C13 120.75(18) ?
C11 C12 H12 119.6 ?
C13 C12 H12 119.6 ?
N12 C13 C12 122.07(16) ?
N12 C13 C14 122.04(16) ?
C12 C13 C14 115.89(17) ?
C15 C14 C13 120.35(18) ?
C15 C14 H14 119.8 ?
C13 C14 H14 119.8 ?
N11 C15 C14 121.32(19) ?
N11 C15 H15 119.3 ?
C14 C15 H15 119.3 ?
C13 N12 C16 121.63(16) ?
C13 N12 C17 121.40(16) ?
C16 N12 C17 116.78(16) ?
N12 C16 H16A 109.5 ?
N12 C16 H16B 109.5 ?
H16A C16 H16B 109.5 ?
N12 C16 H16C 109.5 ?
H16A C16 H16C 109.5 ?
H16B C16 H16C 109.5 ?
N12 C17 H17A 109.5 ?
N12 C17 H17B 109.5 ?
H17A C17 H17B 109.5 ?
N12 C17 H17C 109.5 ?
H17A C17 H17C 109.5 ?
H17B C17 H17C 109.5 ?
C21 N21 C25 120.47(18) ?
C21 N21 H21A 119.8 ?
C25 N21 H21A 119.8 ?
N21 C21 C22 121.43(19) ?
N21 C21 H21 119.3 ?
C22 C21 H21 119.3 ?
C21 C22 C23 120.43(19) ?
C21 C22 H22 119.8 ?
C23 C22 H22 119.8 ?
N22 C23 C22 122.04(17) ?
N22 C23 C24 121.91(17) ?
C22 C23 C24 116.06(18) ?
C25 C24 C23 120.49(18) ?
C25 C24 H24 119.8 ?
C23 C24 H24 119.8 ?
N21 C25 C24 121.1(2) ?
N21 C25 H25 119.4 ?
C24 C25 H25 119.4 ?
C23 N22 C26 121.46(18) ?
C23 N22 C27 121.96(18) ?
C26 N22 C27 116.23(19) ?
N22 C26 H26A 109.5 ?
N22 C26 H26B 109.5 ?
H26A C26 H26B 109.5 ?
N22 C26 H26C 109.5 ?
H26A C26 H26C 109.5 ?
H26B C26 H26C 109.5 ?
N22 C27 H27A 109.5 ?
N22 C27 H27B 109.5 ?
H27A C27 H27B 109.5 ?
N22 C27 H27C 109.5 ?
H27A C27 H27C 109.5 ?
H27B C27 H27C 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 N1 2.0495(17) y
Mn1 N2 2.0600(16) y
Mn1 N3 2.0810(16) y
Mn1 N4 2.1336(17) y
N1 C1 1.165(2) ?
C1 S1 1.6169(19) ?
N2 C2 1.159(2) ?
C2 S2 1.6133(19) ?
N3 C3 1.159(2) ?
C3 S3 1.6286(18) ?
N4 C4 1.159(3) ?
C4 S4 1.627(2) ?
N11 C11 1.342(3) ?
N11 C15 1.344(3) ?
N11 H11A 0.8800 ?
C11 C12 1.356(3) ?
C11 H11 0.9500 ?
C12 C13 1.419(2) ?
C12 H12 0.9500 ?
C13 N12 1.333(2) ?
C13 C14 1.420(3) ?
C14 C15 1.354(3) ?
C14 H14 0.9500 ?
C15 H15 0.9500 ?
N12 C16 1.455(2) ?
N12 C17 1.458(2) ?
C16 H16A 0.9800 ?
C16 H16B 0.9800 ?
C16 H16C 0.9800 ?
C17 H17A 0.9800 ?
C17 H17B 0.9800 ?
C17 H17C 0.9800 ?
N21 C21 1.339(3) ?
N21 C25 1.348(3) ?
N21 H21A 0.8800 ?
C21 C22 1.351(3) ?
C21 H21 0.9500 ?
C22 C23 1.416(3) ?
C22 H22 0.9500 ?
C23 N22 1.332(2) ?
C23 C24 1.418(3) ?
C24 C25 1.351(3) ?
C24 H24 0.9500 ?
C25 H25 0.9500 ?
N22 C26 1.454(3) ?
N22 C27 1.458(3) ?
C26 H26A 0.9800 ?
C26 H26B 0.9800 ?
C26 H26C 0.9800 ?
C27 H27A 0.9800 ?
C27 H27B 0.9800 ?
C27 H27C 0.9800 ?
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
N11 H11A S3 . 0.88 2.45 3.3129(18) 166.0
C12 H12 N4 2_677 0.95 2.67 3.548(2) 154.7
C14 H14 S1 . 0.95 2.94 3.788(2) 149.1
N21 H21A S4 1_444 0.88 2.51 3.2771(19) 146.5
C21 H21 N4 2_667 0.95 2.64 3.440(3) 141.9
C24 H24 S2 1_454 0.95 2.85 3.548(2) 131.4

_cod_database_fobs_code 2242332
