Cyclopentadienone triisocyanide iron complexes: general synthesis and crystal structures of tris(2,6-dimethylphenyl isocyanide)(η4-tetraphenylcyclopentadienone)iron and tris(naphthalen-2-yl isocyanide)(η4-tetraphenylcyclopentadienone)iron acetone hemisolvate
Bütikofer, André; Chen, Peter; Acta Crystallographica Section E Crystallographic Communications 79 (2023) –; doi:10.1107/S205698902300498X

data_2022784
_publ_section_title
;
 Cyclopentadienone triisocyanide iron complexes: general synthesis and
 crystal structures of tris(2,6-dimethylphenyl
 isocyanide)(\h4-tetraphenylcyclopentadienone)iron and
 tris(naphthalen-2-yl isocyanide)(\h4-tetraphenylcyclopentadienone)iron
 acetone hemisolvate
;
_journal_coeditor_code           MW2197
_journal_issue                   7
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S205698902300498X
_journal_volume                  79
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_iupac          '[Fe (C9 H9 N)3 (C29 H20 O)]'
_chemical_formula_moiety         'C56 H47 Fe N3 O'
_chemical_formula_sum            'C56 H47 Fe N3 O'
_chemical_formula_weight         833.81
_chemical_name_systematic
;
Tris(2,6-dimethylphenyl isocyanide)(\h^4^-tetraphenylcyclopentadienone)iron
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7473(3)
_cell_length_b                   12.1998(2)
_cell_length_c                   20.9668(4)
_cell_measurement_reflns_used    11706
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.3330
_cell_measurement_theta_min      3.6120
_cell_volume                     4283.80(13)
_computing_cell_refinement
;
CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33622
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.118
_diffrn_reflns_theta_min         3.623
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.164
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2021)
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       needle
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.402
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1989 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.008(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         7440
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0630P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1093
_reflns_number_gt                6449
_reflns_number_total             7440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mw2197sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        4283.81(13)
_cod_database_code               2022784
_shelx_estimated_absorpt_t_min   0.666
_shelx_estimated_absorpt_t_max   0.939
_shelx_hkl_checksum              369
_shelx_res_checksum              6890
_cod_database_fobs_code 2022784