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_1571971
_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         'C49 H39 Fe3 O7 P3, 0.5(C7 H8)'
_chemical_formula_sum            'C52.5 H43 Fe3 O7 P3'
_chemical_formula_weight         1046.33
_chemical_name_systematic        10
_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   geom
_audit_creation_date             2023-06-03
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2023-06-06 deposited with the CCDC.	2024-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.7080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.22120(10)
_cell_length_b                   19.70640(10)
_cell_length_c                   19.6407(2)
_cell_measurement_reflns_used    51180
_cell_measurement_temperature    100.0(4)
_cell_measurement_theta_max      75.9810
_cell_measurement_theta_min      2.2360
_cell_volume                     4675.66(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (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_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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    -44.00  24.00   0.50    5.00    --  -48.29  37.00 -23.00  136
  2  \w   -121.00 -37.00   0.50    5.00    --  -48.29 -37.00-178.00  168
  3  \w    -24.00  38.00   0.50    5.00    --   48.29 -37.00-178.00  124
  4  \w     38.00 121.00   0.50    5.00    --   48.29  37.00 -23.00  166
  5  \w   -177.00 -94.00   0.50   12.00    -- -104.52 -37.00-178.00  166
  6  \w     94.00 177.00   0.50   12.00    --  104.52  37.00 -23.00  166
  7  \w   -119.00 -87.00   0.50    5.00    --  -48.29-125.00 -60.00   64
  8  \w    -26.00  26.00   0.50    5.00    --  -48.29  19.00 120.00  104
  9  \w    -70.00  24.00   0.50    5.00    --  -48.29  77.00 -30.00  188
 10  \w     82.00 120.00   0.50    5.00    --   48.29  57.00 -90.00   76
 11  \w     -7.00  81.00   0.50    5.00    --   48.29 -99.00-180.00  176
 12  \w   -111.00 -32.00   0.50   12.00    -- -104.52 125.00-150.00  158
 13  \w   -177.00 -94.00   0.50   12.00    -- -104.52 -15.00 -60.00  166
 14  \w   -111.00 -32.00   0.50   12.00    -- -104.52 125.00   0.00  158
 15  \w   -107.00 -32.00   0.50   12.00    -- -104.52 103.00  58.92  150
 16  \w   -177.00-100.00   0.50   12.00    -- -104.52 -77.00  90.00  154
 17  \w    -75.00 -32.00   0.50   12.00    -- -104.52  61.00  30.00   86
 18  \w   -177.00-100.00   0.50   12.00    -- -104.52 -77.00  60.00  154
 19  \w   -108.00 -32.00   0.50   12.00    -- -104.52 114.00 -33.07  152
 20  \w   -177.00 -94.00   0.50   12.00    -- -104.52 -45.00 150.00  166
 21  \w     32.00 105.00   0.50   12.00    --  104.52 -95.00 -30.00  146
 22  \w     32.00  69.00   0.50   12.00    --  104.52 -61.00 120.00   74
 23  \w     32.00 105.00   0.50   12.00    --  104.52 -95.00 150.00  146
 24  \w     32.00  69.00   0.50   12.00    --  104.52 -61.00 -30.00   74
 25  \w    100.00 177.00   0.50   12.00    --  104.52  77.00-120.00  154
 26  \w     32.00 105.00   0.50   12.00    --  104.52 -95.00-180.00  146
 27  \w     32.00 111.00   0.50   12.00    --  104.52-125.00 -30.00  158
 28  \w     32.00  69.00   0.50   12.00    --  104.52 -61.00 -60.00   74
 29  \w     32.00  69.00   0.50   12.00    --  104.52 -61.00-180.00   74
 30  \w     32.00 111.00   0.50   12.00    --  104.52-125.00 120.00  158
 31  \w    100.00 177.00   0.50   12.00    --  104.52  77.00-150.00  154
 32  \w     32.00  69.00   0.50   12.00    --  104.52 -61.00   0.00   74
 33  \w     32.00 105.00   0.50   12.00    --  104.52 -95.00 -60.00  146
 34  \w     32.00  69.00   0.50   12.00    --  104.52 -61.00-150.00   74
 35  \w     35.00 120.00   0.50    5.00    --   48.29  56.00 160.40  170
 36  \w     35.00 120.00   0.50    5.00    --   48.29  56.00-106.55  170
 37  \w     35.00 120.00   0.50    5.00    --   48.29  55.00   6.94  170
 38  \w     35.00 120.00   0.50    5.00    --   48.29  54.00  68.22  170
;
_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_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            88271
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.464
_diffrn_reflns_theta_min         3.195
_exptl_absorpt_coefficient_mu    8.770
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.545
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (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            'clear yellowish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       prism
_exptl_crystal_F_000             2148
_exptl_crystal_preparation
'From a solution of 8 in toluene for two months at -20 degrees C.'
_exptl_crystal_recrystallization_method
'From a crude solution in toluene at -20 degrees C.'
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         9727
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+3.4570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9255
_reflns_number_total             9727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01370k3.cif
_cod_data_source_block           compound10
_cod_depositor_comments
'Adding full bibliography for 1571968--1571976.cif.'
_cod_original_formula_sum        'C52.50 H43 Fe3 O7 P3'
_cod_database_code               1571971
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.673
_shelx_estimated_absorpt_t_min   0.245
_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. Restrained distances
 C55-C50
 1.39 with sigma of 0.02
 C51-C55
 2.4 with sigma of 0.03
 C55-C54
 1.39 with sigma of 0.02
 C54-C52
 2.4 with sigma of 0.03
 C54-C53
 1.39 with sigma of 0.02
 C55-C52
 2.8 with sigma of 0.03
 C53-C52
 1.39 with sigma of 0.02
 C55-C53
 2.4 with sigma of 0.03
 C52-C51
 1.39 with sigma of 0.02
 C53-C51
 2.4 with sigma of 0.03
 C51-C50
 1.39 with sigma of 0.02
 C50-C53
 2.8 with sigma of 0.03
 C56-C50
 1.52 with sigma of 0.02
 C51-C54
 2.8 with sigma of 0.03
 C50-C54
 2.4 with sigma of 0.03
 C50-C52
 2.4 with sigma of 0.03
 C51-C56 \\sim C55-C56
 with sigma of 0.02
3. Restrained planarity
 C53, C54, C55, C50, C51, C52, C56
 with sigma of 0.02
4. Others
 Fixed Sof: C50(0.5) C51(0.5) H51(0.5) C52(0.5) H52(0.5) C53(0.5) H53(0.5)
 C54(0.5) H54(0.5) C55(0.5) H55(0.5) C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B)
5.b Me refined with riding coordinates:
 C56(H56A,H56B,H56C)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), 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), C51(H51),
  C52(H52), C53(H53), C54(H54), C55(H55)
5.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_shelx_res_checksum              82606
_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
;