2,3-Diamino-4,5-diarylcyclopentadienone iron carbonyl complexes as catalysts for reductive amination reactions
Körner, Lukas; Bockfeld, Dirk; Bannenberg, Thomas; Tamm, Matthias; Catalysis Science & Technology 14 (2024) 4522–4532; doi:10.1039/D4CY00372A

data_1572064
_publ_section_title
;
 2,3-Diamino-4,5-diarylcyclopentadienone iron carbonyl complexes as
 catalysts for reductive amination reactions
;
_journal_issue                   16
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              4522
_journal_page_last               4532
_journal_paper_doi               10.1039/D4CY00372A
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C33 H31 F6 Fe N3 O3 [0.5 (C2 H3 N1)]'
_chemical_formula_sum            'C34 H32.5 F6 Fe N3.5 O3'
_chemical_formula_weight         707.98
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-03-06 deposited with the CCDC.	2024-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                106.515(3)
_cell_angle_beta                 110.781(4)
_cell_angle_gamma                94.220(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7552(4)
_cell_length_b                   11.5325(3)
_cell_length_c                   14.6781(6)
_cell_measurement_reflns_used    31930
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.3480
_cell_measurement_theta_min      3.3540
_cell_volume                     1600.72(12)
_computing_cell_refinement       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_publication_material
'OLEX2 v1.3 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)'
_computing_structure_refinement
'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, C71, 3-8)'
_computing_structure_solution
'SHELXT 2018/2 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_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_unetI/netI     0.0042
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6848
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.574
_diffrn_reflns_theta_min         3.415
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.446
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.358
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.64a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       irregular
_exptl_crystal_F_000             730
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.052
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         6848
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0606
_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^)+(0.1010P)^2^+2.0608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1657
_refine_ls_wR_factor_ref         0.1675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6677
_reflns_number_total             6848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cy00372a3.cif
_cod_data_source_block           lk42db
_cod_depositor_comments
'Adding full bibliography for 1572060--1572070.cif.'
_cod_original_cell_volume        1600.72(11)
_cod_original_formula_sum        'C34 H32.50 F6 Fe N3.50 O3'
_cod_database_code               1572064
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.470
_shelx_estimated_absorpt_t_max   0.776
_oxdiff_exptl_absorpt_empirical_full_min 0.574
_oxdiff_exptl_absorpt_empirical_full_max 1.782
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_smtbx_masks_special_details
;
 0.5 molecules of acetonitrile per Asymmetric unit have been identified
 but could not be refined satisfactorily. Therefore, a solvent mask, the Olex2
 implementation of the program SQUEEZE (Spek, A. L. (2015). Acta Cryst.
 C71, 9-18.) has been used to mathematically remove the electron density of
 these molecules. 21 electrons were found in a volume of 129\%A^3^ in 1 void
 per unit cell. This is consistent with the presence of 0.5[C2H3N] per
 Asymmetric Unit which account for 22 electrons per unit cell. The sum
 formula and derived parameters are based on 0.5 molecules of C2H3N per
 Asymmetric unit.
;
_shelx_res_checksum              1385
_shelx_hkl_checksum              79803
_shelx_fab_checksum              73285