Complete ligand substitution and oxidation of the metal center in the photochemical reaction of CpM(CO)<sub>2</sub>I (M = Fe, Ru) with chelating β-diketones.
Jarzyński, Szymon; Doroszko, Cyprian; Jamroz, Daria; Stefanowska-Kątna, Kinga; Walkowiak, Jędrzej; Wojtulewski, Sławomir; Zakrzewski, Janusz; Rudolf, Bogna; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5935–5943; doi:10.1039/d5dt00294j

data_7718342
_publ_section_title
;
 Complete ligand substitution and oxidation of the metal center in the
 photochemical reaction of CpM(CO)<sub>2</sub>I (M = Fe, Ru) with
 chelating &#x3b2;-diketones.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5935
_journal_page_last               5943
_journal_paper_doi               10.1039/d5dt00294j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C33 H33 Fe O9'
_chemical_formula_sum            'C33 H33 Fe O9'
_chemical_formula_weight         629.44
_chemical_name_systematic        tris(4-methoxybenzoylacetonato)iron(III)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-15
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-18 deposited with the CCDC.	2025-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.346(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2832(7)
_cell_length_b                   15.6780(8)
_cell_length_c                   13.2979(5)
_cell_measurement_reflns_used    13017
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      32.2390
_cell_measurement_theta_min      2.9680
_cell_volume                     2953.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4052
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -69.00 108.00   1.00  178.69    --   19.56   0.00  30.00  177
  2  \w     39.00 108.00   1.00  178.69    --   19.56 178.00-120.00   69
  3  \w   -108.00 -61.00   1.00  178.69    --  -19.63-178.00 150.00   47
  4  \w    -60.00 -27.00   1.00  178.69    --   19.56 -19.00 -30.00   33
  5  \w     -9.00  93.00   1.00  178.69    --   19.56  57.00 120.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Mo at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0409508000
_diffrn_orient_matrix_UB_12      -0.0239229000
_diffrn_orient_matrix_UB_13      -0.0175091000
_diffrn_orient_matrix_UB_21      0.0286808000
_diffrn_orient_matrix_UB_22      -0.0324665000
_diffrn_orient_matrix_UB_23      -0.0172592000
_diffrn_orient_matrix_UB_31      0.0025022000
_diffrn_orient_matrix_UB_32      -0.0205343000
_diffrn_orient_matrix_UB_33      0.0478215000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33711
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.128
_diffrn_reflns_theta_min         2.590
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_T_max  0.618
_exptl_absorpt_correction_T_min  0.137
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (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            'clear dark pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       plate
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         7948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0668
_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^)+(0.0713P)^2^+5.5010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1732
_refine_ls_wR_factor_ref         0.1857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6257
_reflns_number_total             7948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00294j2.cif
_cod_data_source_block           sjr-417
_cod_depositor_comments          'Adding full bibliography for 7718342.cif.'
_cod_database_code               7718342
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C132  H132  Fe4  O36  '
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.793
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11A(H11A), C7A(H7A), C3B(H3B), C10B(H10B), C10A(H10A), C11B(H11B), C3A(H3A),
 C7B(H7B), C8A(H8A), C8B(H8B), C3C(H3C), C11C(H11C), C7C(H7C), C10C(H10C),
 C8C(H8C)
2.b Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C5B(H5BA,H5BB,H5BC), C5A(H5AA,H5AB,
 H5AC), C5C(H5CA,H5CB,H5CC), C1C(H1CA,H1CB,H1CC)
;
_shelx_res_checksum              580
_shelx_hkl_checksum              96019
_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 1.924
_oxdiff_exptl_absorpt_empirical_full_min 0.294