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_1571976
_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         'C32 H16 Fe5 O13 P, C8 H20 N'
_chemical_formula_sum            'C40 H36 Fe5 N O13 P'
_chemical_formula_weight         1048.92
_chemical_name_systematic        '[NEt4][Fe5(mu5-C)(CO)13(PPh3)]'
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-01-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-06-06 deposited with the CCDC.	2024-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.2791(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1733(3)
_cell_length_b                   12.1213(2)
_cell_length_c                   20.6329(3)
_cell_measurement_reflns_used    40338
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      75.958
_cell_measurement_theta_min      2.637
_cell_volume                     4180.16(12)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.974
_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   -119.00 -50.00   0.50    4.00    --  -48.29-160.00-124.00  138
  2  \w    -91.00  -8.00   0.50    4.00    --  -48.29 118.00 113.00  166
  3  \w     31.00 118.00   0.50    4.00    --   48.29-160.00-124.00  174
  4  \w      8.00  91.00   0.50    4.00    --   48.29-118.00  27.00  166
  5  \w     50.00 120.00   0.50    4.00    --   48.29 160.00 -94.00  140
  6  \w   -109.00 -32.00   0.50   16.00    -- -104.52 118.00 113.00  154
  7  \w   -135.00 -32.00   0.50   16.00    -- -104.52 160.00 -94.00  206
  8  \w   -177.00 -78.00   0.50   16.00    -- -104.52-118.00  27.00  198
  9  \w   -158.00 -50.00   0.50   16.00    -- -104.52-160.00-124.00  216
 10  \w     32.00 110.00   0.50   16.00    --  104.52-118.00  27.00  156
 11  \w     78.00 177.00   0.50   16.00    --  104.52 118.00 113.00  198
 12  \w     50.00 158.00   0.50   16.00    --  104.52 160.00 -94.00  216
 13  \w   -119.00 -82.00   0.50    4.00    --  -48.29 -57.00 -60.00   74
 14  \w   -119.00 -87.00   0.50    4.00    --  -48.29-125.00-120.00   64
 15  \w   -119.00 -82.00   0.50    4.00    --  -48.29 -57.00  30.00   74
 16  \w   -119.00 -82.00   0.50    4.00    --  -48.29 -57.00-120.00   74
 17  \w   -119.00 -82.00   0.50    4.00    --  -48.29 -57.00 -90.00   74
 18  \w     82.00 120.00   0.50    4.00    --   48.29  57.00 120.00   76
 19  \w    -75.00 -32.00   0.50   16.00    -- -104.52  61.00 120.00   86
 20  \w   -177.00 -91.00   0.50   16.00    -- -104.52 -61.00 -60.00  172
 21  \w     94.00 177.00   0.50   16.00    --  104.52  45.00 -90.00  166
 22  \w     32.00 105.00   0.50   16.00    --  104.52 -95.00  60.00  146
 23  \w     94.00 178.00   0.50   16.00    --  104.52  15.00 -60.00  168
 24  \w     32.00 105.00   0.50   16.00    --  104.52 -95.00  30.00  146
 25  \w     32.00  69.00   0.50   16.00    --  104.52 -61.00 -60.00   74
 26  \w     32.00 105.00   0.50   16.00    --  104.52 -95.00-150.00  146
 27  \w     32.00  69.00   0.50   16.00    --  104.52 -61.00 -90.00   74
 28  \w     32.00  69.00   0.50   16.00    --  104.52 -61.00-180.00   74
 29  \w     38.00 121.00   0.50    4.00    --   48.29  38.00   0.00  166
 30  \w     38.00 121.00   0.50    4.00    --   48.29  38.00-180.00  166
 31  \w     38.00 107.00   0.50    4.00    --   48.29  38.00 -90.00  138
 32  \w     38.00 121.00   0.50    4.00    --   48.29  38.00  90.00  166
;
_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      -0.0841739000
_diffrn_orient_matrix_UB_12      -0.0423285000
_diffrn_orient_matrix_UB_13      -0.0336879000
_diffrn_orient_matrix_UB_21      0.0261144000
_diffrn_orient_matrix_UB_22      -0.1187681000
_diffrn_orient_matrix_UB_23      0.0213658000
_diffrn_orient_matrix_UB_31      -0.0268210000
_diffrn_orient_matrix_UB_32      0.0166038000
_diffrn_orient_matrix_UB_33      0.0655736000
_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  0.0709
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            63765
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.490
_diffrn_reflns_theta_min         2.644
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.509
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.090
_exptl_absorpt_correction_type   'gaussian and multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       plate
_exptl_crystal_F_000             2128
_exptl_crystal_preparation       'reaction of Fe6^0 with PPh3'
_exptl_crystal_recrystallization_method
'grown from vapor diffusion of diethylether into fluorobenzene'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         8562
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0947P)^2^+2.0813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7910
_reflns_number_total             8562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01370k3.cif
_cod_data_source_block           compound4
_cod_depositor_comments
'Adding full bibliography for 1571968--1571976.cif.'
_cod_original_cell_volume        4180.17(13)
_cod_database_code               1571976
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.502
_shelx_estimated_absorpt_t_min   0.090
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
2.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C35(H35A,H35B), C37(H37A,H37B), C39(H39A,H39B)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
2.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C40(H40A,H40B,
 H40C)
;
_shelx_res_checksum              41043
_olex2_exptl_crystal_mounting_method mounted
_olex2_submission_special_instructions 'No special instructions were received'