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_2242333
_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_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)3 [Mn (N C S)5]'
_chemical_formula_moiety         '3(C7 H11 N2 +), C5 Mn N5 S5 3-'
_chemical_formula_sum            'C26 H33 Mn N11 S5'
_chemical_formula_weight         714.87
_chemical_name_systematic
;
Tris[4-(dimethylamino)pyridinium]
pentakis(thiocyanato-\k<i>N</i>)manganate(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90.0980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8320(2)
_cell_length_b                   28.1610(5)
_cell_length_c                   11.3392(2)
_cell_measurement_reflns_used    45580
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.004
_cell_measurement_theta_min      1.446
_cell_volume                     3458.90(11)
_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 0.998
_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  0.0373
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            45580
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.004
_diffrn_reflns_theta_min         1.446
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  0.9154
_exptl_absorpt_correction_T_min  0.7894
_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    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.238
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.028(18)
_refine_ls_extinction_coef       0.0053(7)
_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   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     789
_refine_ls_number_reflns         13568
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+1.5196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                12684
_reflns_number_total             13568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5426sup1.cif
_cod_data_source_block           Compound2
_cod_database_code               2242333
_cod_database_fobs_code          2242333
_shelx_hkl_checksum              91707
_shelx_res_checksum              96056
_shelxl_version_number           2.014