Crystal structures of bis[4-(dimethylamino)pyridinium] tetrakis(thiocyanato-κ<i>N</i>)manganate(II) and tris[4-(dimethylamino)pyridinium] pentakis(thiocyanato-κ<i>N</i>)manganate(II)
Neumann, Tristan; Jess, Inke; Näther, Christian; Acta Crystallographica Section E 74 (2018) 15–20; doi:10.1107/S2056989017017510

data_2242332
_publ_section_title
;
 Crystal structures of bis[4-(dimethylamino)pyridinium]
 tetrakis(thiocyanato-\k<i>N</i>)manganate(II) and
 tris[4-(dimethylamino)pyridinium]
 pentakis(thiocyanato-\k<i>N</i>)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-\k<i>N</i>)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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0601P)^2^+0.0944P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            wm5426sup1.cif
_cod_data_source_block           Compound1
_cod_database_code               2242332
_cod_database_fobs_code          2242332
_shelx_hkl_checksum              99487
_shelx_res_checksum              26810
_shelxl_version_number           2.014