Iron(0) tricarbonyl η<sup>4</sup>-1-azadiene complexes and their catalytic performance in the hydroboration of ketones, aldehydes and aldimines <i>via</i> a non-iron hydride pathway.
Luo, Jiabin; Cui, Chuanguo; Xiao, Zhiyin; Zhong, Wei; Lu, Chunxin; Jiang, Xiujuan; Li, Xueming; Liu, Xiaoming; Dalton transactions (Cambridge, England : 2003)  (2022) –; doi:10.1039/d2dt01673g

data_7710698
_publ_section_title
;
 Iron(0) tricarbonyl \h<sup>4</sup>-1-azadiene complexes and their
 catalytic performance in the hydroboration of ketones, aldehydes and
 aldimines <i>via</i> a non-iron hydride pathway.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt01673g
_journal_year                    2022
_chemical_formula_moiety         'C22 H15 Fe N O3'
_chemical_formula_sum            'C22 H15 Fe N O3'
_chemical_formula_weight         397.20
_chemical_properties_physical    Light-sensitive,Photo-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2022-04-03 deposited with the CCDC.	2022-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.203(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.427(2)
_cell_length_b                   7.6710(5)
_cell_length_c                   21.6488(18)
_cell_measurement_reflns_used    3084
_cell_measurement_temperature    298
_cell_measurement_theta_max      29.2030
_cell_measurement_theta_min      3.8570
_cell_volume                     3771.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0802
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -8.00  21.00   1.00    7.50    --  -15.89 -99.00 150.00   29
  2  \w    -51.00  33.00   1.00    7.50    --   16.20 -57.00-150.00   84
  3  \w     36.00  82.00   1.00    7.50    --   16.20  57.00-180.00   46
  4  \w     16.00  80.00   1.00    7.50    --   16.20  38.00 -30.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0019053000
_diffrn_orient_matrix_UB_12      -0.0056052000
_diffrn_orient_matrix_UB_13      -0.0332047000
_diffrn_orient_matrix_UB_21      0.0310767000
_diffrn_orient_matrix_UB_22      0.0066203000
_diffrn_orient_matrix_UB_23      0.0060614000
_diffrn_orient_matrix_UB_31      0.0023556000
_diffrn_orient_matrix_UB_32      -0.0919805000
_diffrn_orient_matrix_UB_33      0.0024441000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.852
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8767
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.304
_diffrn_reflns_theta_min         2.949
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/hexane'
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+0.4215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1346
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2875
_reflns_number_total             4393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01673g2.cif
_cod_data_source_block           201104-ljb035-nainh2fecox
_cod_database_code               7710698
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C, H, O, N, Fe'
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.773
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H4), C2(H2), C3(H3)
2.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C8(H8), C10(H10), C20(H20), C11(H11), C14(H14), C18(H18), C19(H19),
 C16(H16), C15(H15), C7(H7), C12(H12)
;
_shelx_res_checksum              13648
_olex2_date_sample_completion    2020-11-04
_olex2_date_sample_data_collection 2020-11-04
_olex2_date_sample_submission    2020-11-04
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.604
_oxdiff_exptl_absorpt_empirical_full_min 0.661