Coordination chemistry of polynitriles. Part 9. Decacyanoferrocene revisited. Crystal and molecular structure of <i>cis</i>-[{C~5~(CN)~5~}~2~(MeCN)~4~Fe]
Sünkel, Karlheinz; Blockhaus, Tobias; Acta Crystallographica Section C 78 (2022) –; doi:10.1107/S2053229622000365

data_2022517
_publ_section_title
;
 Coordination chemistry of polynitriles. Part 9. Decacyanoferrocene
 revisited. Crystal and molecular structure of
 <i>cis</i>-[{C~5~(CN)~5~}~2~(MeCN)~4~Fe]
;
_journal_coeditor_code           EQ3004
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229622000365
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          '[Fe (C10 N5)2 (C2 H3 N)4], 1.8C2 H3 N'
_chemical_formula_moiety         'C28 H12 Fe N14, 1.8(C2 H3 N)'
_chemical_formula_sum            'C31.6 H17.4 Fe N15.8'
_chemical_formula_weight         674.29
_chemical_name_systematic
'Tetrakis(acetonitrile-\k<i>N</i>)bis(pentacyanocyclopentadienido-\k<i>N</i>)iron(II) acetonitrile disolvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                62.528(2)
_cell_angle_beta                 82.929(2)
_cell_angle_gamma                77.210(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9972(7)
_cell_length_b                   12.8711(7)
_cell_length_c                   13.0907(8)
_cell_measurement_reflns_used    8142
_cell_measurement_temperature    109(2)
_cell_measurement_theta_max      26.5292
_cell_measurement_theta_min      2.7407
_cell_volume                     1748.47(18)
_computing_cell_refinement
;
APEX2 (Bruker, 2011)
;
_computing_data_collection
;
APEX2 (Bruker, 2011)
;
_computing_data_reduction
;
SAINT (Bruker, 2011)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      109(2)
_diffrn_detector_area_resol_mean 7.391
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'mix of omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0666
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17051
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.428
_diffrn_reflns_theta_min         3.039
_diffrn_source                   'rotating anode generator'
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.626
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         7081
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0639
_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^)+(0.0525P)^2^+4.4167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1477
_refine_ls_wR_factor_ref         0.1627
_reflns_number_gt                5145
_reflns_number_total             7081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            eq3004sup1.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C31.60 H17.40 Fe N15.80'
_cod_database_code               2022517
_shelx_estimated_absorpt_t_min   0.976
_shelx_estimated_absorpt_t_max   0.986
_shelx_hkl_checksum              42184
_shelx_res_checksum              12193
_cod_database_fobs_code 2022517