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_2243951
_publ_section_title
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 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 (C14 H10) (C9 H9 N)3]'
_chemical_formula_moiety         'C41 H37 Fe N3'
_chemical_formula_sum            'C41 H37 Fe N3'
_chemical_formula_weight         627.58
_chemical_name_systematic
;
[(1,2,3,4-\h)-Anthracene]tris(2,6-dimethylphenyl isocyanide)iron
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 93.057(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8528(11)
_cell_length_b                   10.9022(10)
_cell_length_c                   24.927(2)
_cell_measurement_reflns_used    2566
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.29
_cell_measurement_theta_min      2.48
_cell_volume                     3216.5(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      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens SMART CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0873
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24459
_diffrn_reflns_theta_full        25.065
_diffrn_reflns_theta_max         25.065
_diffrn_reflns_theta_min         1.636
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.347
_refine_ls_extinction_coef       0.0108(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2018/3 (Sheldrick 2015)
;
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         5687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0505P)^2^+1.1491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1202
_reflns_number_gt                4023
_reflns_number_total             5687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yz2014sup1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2243951
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.961
_shelx_hkl_checksum              25820
_shelx_res_checksum              21634
_cod_database_fobs_code 2243951