Crystal structure of the co-crystal <i>fac</i>-triaquatris(thiocyanato-κ<i>N</i>)iron(III)–2,3-dimethylpyrazine (1/3)
Kucheriv, Olesia I.; Shylin, Sergii I.; Ilina, Tetiana A.; Dechert, Sebastian; Gural'skiy, Il'ya A.; Acta Crystallographica Section E 71 (2015) 374–376; doi:10.1107/S2056989015004831

data_2240504
_publ_section_title
;
 Crystal structure of the co-crystal
 <i>fac</i>-triaquatris(thiocyanato-\k<i>N</i>)iron(III)--2,3-dimethylpyrazine
 (1/3)
;
_journal_coeditor_code           XU5840
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              374
_journal_page_last               376
_journal_paper_doi               10.1107/S2056989015004831
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Fe (N C S)3 (H2 O1)3], 3C6 H8 N2'
_chemical_formula_moiety         'C3 H6 Fe1 N3 O3 S3, 3(C6 H8 N2)'
_chemical_formula_sum            'C21 H30 Fe N9 O3 S3'
_chemical_formula_weight         608.57
_chemical_name_systematic
;
<i>fac</i>-Triaquatris(thiocyanato-\k<i>N</i>)iron(III)--2,3-dimethylpyrazine
(1/3)
;
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   16.9383(12)
_cell_length_b                   16.9383(12)
_cell_length_c                   17.6259(13)
_cell_measurement_temperature    133(2)
_cell_volume                     4379.5(5)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_reduction
;
X-RED (Stoe & Cie, 2002)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      133.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5784
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.755
_diffrn_reflns_theta_min         2.405
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.9389
_exptl_absorpt_correction_T_min  0.9081
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-RED; Stoe & Cie, 2002)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             1902
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.278
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 685 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1903
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0297P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0701
_reflns_number_gt                1716
_reflns_number_total             1903
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu5840sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        4379.5(7)
_cod_database_code               2240504