Crystal structures of two novel iron isocyanides from the reaction of 2,6-dimethylphenyl isocyanide, CNXyl, with bis(anthracene)ferrate({-}1)
Brennessel, William W.; Ellis, John E.; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S205698902101313X

data_2243952
_publ_section_title
;
 Crystal structures of two novel iron isocyanides from the reaction of
 2,6-dimethylphenyl isocyanide, CNXyl, with bis(anthracene)ferrate({-}1)
;
_journal_coeditor_code           YZ2014
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205698902101313X
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          '[Fe (C54 H56 N6) (C9 H9 N)3], 2C4 H8 O'
_chemical_formula_moiety         'C81 H83 Fe N9, 2(C4 H8 O)'
_chemical_formula_sum            'C89 H99 Fe N9 O2'
_chemical_formula_weight         1382.62
_chemical_name_systematic
;{5,6-Bis(2,6-dimethylanilino)-3-(2,6-dimethylphenyl)-1,2,7-tris[(2,6-dimethylphenyl)imino]-3-azoniahept-3-ene-1,4,7-triido}tris(2,6-dimethylphenyl
isocyanide)iron tetrahydrofuran 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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                85.342(3)
_cell_angle_beta                 74.001(3)
_cell_angle_gamma                70.884(3)
_cell_formula_units_Z            2
_cell_length_a                   13.8912(10)
_cell_length_b                   15.4941(11)
_cell_length_c                   19.7902(14)
_cell_measurement_reflns_used    3451
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.65
_cell_measurement_theta_min      2.31
_cell_volume                     3868.5(5)
_computing_cell_refinement
;
SAINT (Bruker, 2003)
;
_computing_data_collection
;
SMART (Bruker, 2003)
;
_computing_data_reduction
;
SAINT (Bruker, 2003)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR97 (Altomare <i>et al</i>., 1999)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31905
_diffrn_reflns_theta_full        25.067
_diffrn_reflns_theta_max         25.067
_diffrn_reflns_theta_min         1.609
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.249
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       block
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1192
_refine_ls_number_reflns         13640
_refine_ls_number_restraints     382
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0600P)^2^+0.9501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                9367
_reflns_number_total             13640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yz2014sup1.cif
_cod_data_source_block           2
_cod_database_code               2243952
_shelx_estimated_absorpt_t_min   0.920
_shelx_estimated_absorpt_t_max   0.943
_shelx_hkl_checksum              47460
_shelx_res_checksum              58989
_cod_database_fobs_code 2243952