Crystal structure of octakis(4-methoxypyridinium) bis(4-methoxypyridine-κ<i>N</i>)tetrakis(thiocyanato-κ<i>N</i>)ferrate(III) bis[(4-methoxypyridine-κ<i>N</i>)pentakis(thiocyanato-κ<i>N</i>)ferrate(III)] hexakis(thiocyanato-κ<i>N</i>)ferrate(III) with iron in three different octahedral coordination environments
Jochim, Aleksej; Jess, Inke; Näther, Christian; Acta Crystallographica Section E 74 (2018) 287–291; doi:10.1107/S2056989018001883

data_2242366
_publ_section_title
;
 Crystal structure of octakis(4-methoxypyridinium)
 bis(4-methoxypyridine-\k<i>N</i>)tetrakis(thiocyanato-\k<i>N</i>)ferrate(III)
 bis[(4-methoxypyridine-\k<i>N</i>)pentakis(thiocyanato-\k<i>N</i>)ferrate(III)]
 hexakis(thiocyanato-\k<i>N</i>)ferrate(III) with iron in three different
 octahedral coordination environments
;
_journal_coeditor_code           WM5434
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              287
_journal_page_last               291
_journal_paper_doi               10.1107/S2056989018001883
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac
;
(C6 H8 N O)8 [Fe (N C S)4 (C6 H7 N O)2]
[Fe (N C S)5 (C6 H7 N O)]2 [Fe (N C S)6]
;
_chemical_formula_moiety
;
8(C6 H8 N O +), C16 H14 Fe N6 O2 S4 -,
2(C11 H7 Fe N6 O1 S5 2-), C6 Fe N6 S6 3-
;
_chemical_formula_sum            'C92 H92 Fe4 N32 O12 S20'
_chemical_formula_weight         2702.57
_chemical_name_systematic
;Bis(4-methoxypyridine-\k<i>N</i>)tetrakis(thiocyanato-\k<i>N</i>)ferrate(III)
bis[(4-methoxypyridine-\k<i>N</i>)pentakis(thiocyanato-\k<i>N</i>)ferrate(III)]
hexakis(thiocyanato-\k<i>N</i>)ferrate(III)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 113.864(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.5034(8)
_cell_length_b                   10.51990(10)
_cell_length_c                   35.7432(8)
_cell_measurement_reflns_used    41955
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      25.005
_cell_measurement_theta_min      1.254
_cell_volume                     12208.5(4)
_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 (Sheldrick, 2008) and DIAMOND (Brandenburg, 2014)
;
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0495
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            41955
_diffrn_reflns_theta_full        25.005
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_min         1.254
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.8059
_exptl_absorpt_correction_T_min  0.6070
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(<i>X-RED</i> and <i>X-SHAPE</i>; Stoe & Cie, 2008)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       block
_exptl_crystal_F_000             5552
_exptl_crystal_size_max          0.4189
_exptl_crystal_size_mid          0.2261
_exptl_crystal_size_min          0.1314
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.668
_refine_ls_extinction_coef       0.00035(6)
_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   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         10715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0524P)^2^+13.0479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1061
_reflns_number_gt                9204
_reflns_number_total             10715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5434sup1.cif
_cod_data_source_block           I
_cod_database_code               2242366
_shelx_hkl_checksum              23831
_shelx_res_checksum              53032
_cod_database_fobs_code 2242366