Merging cyclopentadienone tuning and CO to isonitrile substitution to develop photo-activated iron cyclopentadienone catalysts.
Gounon, Clémence; Quintil, Gaëtan; Pécaut, Jacques; Clémancey, Martin; Bjornsson, Ragnar; Quintard, Adrien; Kochem, Amélie; Dalton transactions (Cambridge, England : 2003) 54 (2025) 14111–14122; doi:10.1039/d5dt01184a

data_7719266
_publ_section_title
;
 Merging cyclopentadienone tuning and CO to isonitrile substitution to
 develop photo-activated iron cyclopentadienone catalysts.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14111
_journal_page_last               14122
_journal_paper_doi               10.1039/d5dt01184a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C40 H28 Fe N2 O7'
_chemical_formula_sum            'C40 H28 Fe N2 O7'
_chemical_formula_weight         704.49
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-30
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_audit_update_record
;
2025-07-01 deposited with the CCDC.	2025-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.001(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9281(4)
_cell_length_b                   11.7464(2)
_cell_length_c                   17.5839(4)
_cell_measurement_reflns_used    7838
_cell_measurement_temperature    150.05(10)
_cell_measurement_theta_max      28.9050
_cell_measurement_theta_min      2.3290
_cell_volume                     3277.39(12)
_computing_cell_refinement       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9653
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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      5.00  94.00   1.00   30.00    --   25.41  57.00 120.00   89
  2  \w    -47.00  51.00   1.00   30.00    --   25.41 -37.00 120.00   98
  3  \w    -97.00  -7.00   1.00   30.00    --  -27.28 -54.00-121.00   90
  4  \w    -71.00  46.00   1.00   30.00    --  -27.28  19.00  60.00  117
  5  \w      5.00  42.00   1.00   30.00    --   25.41  57.00  30.00   37
  6  \w     39.00 101.00   1.00   30.00    --   25.41 178.00   0.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0019772000
_diffrn_orient_matrix_UB_12      0.0258485000
_diffrn_orient_matrix_UB_13      -0.0365610000
_diffrn_orient_matrix_UB_21      0.0371887000
_diffrn_orient_matrix_UB_22      -0.0292491000
_diffrn_orient_matrix_UB_23      -0.0079900000
_diffrn_orient_matrix_UB_31      -0.0247159000
_diffrn_orient_matrix_UB_32      -0.0460752000
_diffrn_orient_matrix_UB_33      -0.0154674000
_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  0.0461
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38926
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.087
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.941
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.57a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent light bronze'
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         10002
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0590P)^2^+1.6481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1442
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6612
_reflns_number_total             10002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01184a2.cif
_cod_data_source_block           cg004_autored
_cod_depositor_comments          'Adding full bibliography for 7719266.cif.'
_cod_database_code               7719266
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Fe1 N2 O7 C40 H28'
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.714
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
;
_shelx_res_checksum              22661
_shelx_hkl_checksum              17598
_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 1.751
_oxdiff_exptl_absorpt_empirical_full_min 0.852