Multi-phosphine-chelated iron-carbide clusters <i>via</i> redox-promoted ligand exchange on an inert hexa-iron-carbide carbonyl cluster, [Fe<sub>6</sub>(μ<sub>6</sub>-C)(μ<sub>2</sub>-CO)<sub>4</sub>(CO)<sub>12</sub>]<sup>2</sup>.
Cobb, Caitlyn R.; Ngo, Ren K.; Dick, Emily J.; Lynch, Vincent M.; Rose, Michael J.; Chemical science 15 (2024) 11455–11471; doi:10.1039/d4sc01370k

data_1571975
_publ_section_title
;
 Multi-phosphine-chelated iron-carbide clusters <i>via</i> redox-promoted
 ligand exchange on an inert hexa-iron-carbide carbonyl cluster,
 [Fe<sub>6</sub>(&#x3bc;<sub>6</sub>-C)(&#x3bc;<sub>2</sub>-CO)<sub>4</sub>(CO)<sub>12</sub>]<sup>2</sup>.
;
_journal_issue                   29
_journal_name_full               'Chemical science'
_journal_page_first              11455
_journal_page_last               11471
_journal_paper_doi               10.1039/d4sc01370k
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C56 H39 Fe5 O14 P3'
_chemical_formula_sum            'C56 H39 Fe5 O14 P3'
_chemical_formula_weight         1308.03
_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     dual
_audit_creation_date             2023-03-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-06-02 deposited with the CCDC.	2024-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                85.773(5)
_cell_angle_beta                 76.692(7)
_cell_angle_gamma                89.678(5)
_cell_formula_units_Z            2
_cell_length_a                   9.4782(8)
_cell_length_b                   15.6679(7)
_cell_length_c                   18.6940(10)
_cell_measurement_reflns_used    5090
_cell_measurement_temperature    100.0(6)
_cell_measurement_theta_max      76.3730
_cell_measurement_theta_min      2.8430
_cell_volume                     2694.0(3)
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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    -89.00 -64.00   0.50   30.00    --  -48.57-158.00  91.00   50
  2  \w    -89.00 -26.00   0.50   30.00    --  -48.57 119.00 -29.00  126
  3  \w   -107.00 -72.00   0.50   30.00    --  -48.57 158.00 125.00   70
  4  \w     73.00  98.00   0.50   30.00    --   48.57-158.00  91.00   50
  5  \w     26.00  51.00   0.50   30.00    --   48.57-119.00-113.00   50
  6  \w     51.00 119.00   0.50   30.00    --   48.57 158.00 125.00  136
  7  \w   -108.00 -83.00   0.50   40.00    -- -105.12 158.00 125.00   50
  8  \w   -112.00 -87.00   0.50   40.00    -- -105.12-158.00  91.00   50
  9  \w   -138.00 -87.00   0.50   40.00    -- -105.12-119.00-113.00  102
 10  \w   -109.00 -73.00   0.50   40.00    -- -105.12 119.00 -29.00   72
 11  \w     81.00 106.00   0.50   40.00    --  105.12 158.00 125.00   50
 12  \w     34.00 107.00   0.50   40.00    --  105.12-119.00-113.00  146
 13  \w     95.00 125.00   0.50   40.00    --  105.12 119.00 -29.00   60
 14  \w     34.00 133.00   0.50   40.00    --  105.12-158.00  91.00  198
 15  \w    -26.00  20.00   0.50   30.00    --  -48.57  19.00-120.00   92
 16  \w   -120.00 -83.00   0.50   30.00    --  -48.57-125.00  90.00   74
 17  \w   -119.00 -28.00   0.50   30.00    --  -48.57 -77.00 -90.00  182
 18  \w    -42.00  24.00   0.50   30.00    --  -48.57  38.00 150.00  132
 19  \w     78.00 118.00   0.50   30.00    --   48.57 125.00-120.00   80
 20  \w   -155.00 -83.00   0.50   40.00    -- -105.12 -95.00-150.00  144
 21  \w    -68.00 -39.00   0.50   40.00    -- -105.12  61.00 -60.00   58
 22  \w   -177.00-100.00   0.50   40.00    -- -105.12 -62.00  98.99  154
 23  \w   -125.00 -89.00   0.50   40.00    -- -105.12 -64.00  -0.73   72
 24  \w   -104.00 -33.00   0.50   40.00    -- -105.12  77.00   0.00  142
 25  \w    -82.00 -35.00   0.50   40.00    -- -105.12  77.00 120.00   94
 26  \w   -109.00 -64.00   0.50   40.00    -- -105.12 125.00-150.00   90
 27  \w   -170.00-130.00   0.50   40.00    -- -105.12 -64.00  -0.73   80
 28  \w   -155.00-129.00   0.50   40.00    -- -105.12 -15.00-150.00   52
 29  \w   -108.00 -70.00   0.50   40.00    -- -105.12 115.00 101.98   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1280399000
_diffrn_orient_matrix_UB_12      -0.0375399000
_diffrn_orient_matrix_UB_13      -0.0258885000
_diffrn_orient_matrix_UB_21      -0.0711106000
_diffrn_orient_matrix_UB_22      -0.0316712000
_diffrn_orient_matrix_UB_23      0.0801216000
_diffrn_orient_matrix_UB_31      -0.0803091000
_diffrn_orient_matrix_UB_32      0.0854976000
_diffrn_orient_matrix_UB_33      0.0110248000
_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  0.1154
_diffrn_reflns_av_unetI/netI     0.1132
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16464
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        50.431
_diffrn_reflns_theta_max         50.431
_diffrn_reflns_theta_min         2.828
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.949
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_correction_T_min  0.386
_exptl_absorpt_correction_type   'gaussian and multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       needle
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.136
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.045
_refine_diff_density_max         1.134
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         5542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0693
_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^)+(0.1036P)^2^+5.0159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1823
_refine_ls_wR_factor_ref         0.1980
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4045
_reflns_number_total             5542
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01370k3.cif
_cod_data_source_block           compound7_auto
_cod_depositor_comments
'Adding full bibliography for 1571968--1571976.cif.'
_cod_database_code               1571975
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Fe5 C56 O14 P3 H37 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C21(H21), C22(H22), C23(H23),
 C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33),
  C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41),
 C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              34425
_shelx_fab_checksum              55725
_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 2.930
_oxdiff_exptl_absorpt_empirical_full_min 0.390