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_1571970
_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         'C33 H15 Fe5 O14 P'
_chemical_formula_sum            'C33 H15 Fe5 O14 P'
_chemical_formula_weight         945.67
_chemical_name_systematic        Fe5(mu5-C)(CO)14(PPh3)
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
;
2023-06-02 deposited with the CCDC.	2024-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.663(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5978(2)
_cell_length_b                   11.8597(2)
_cell_length_c                   14.5875(3)
_cell_measurement_reflns_used    24703
_cell_measurement_temperature    100.0(8)
_cell_measurement_theta_max      75.8370
_cell_measurement_theta_min      3.0040
_cell_volume                     1660.34(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_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(8)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_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  24.00   0.50    4.00    --  -48.29  74.00-142.00  186
  2  \w   -119.00 -28.00   0.50    4.00    --  -48.29 -74.00  89.00  182
  3  \w    -23.00  69.00   0.50    4.00    --   48.29 -74.00  89.00  184
  4  \w   -102.00 -32.00   0.50   12.00    -- -104.52  74.00-142.00  140
  5  \w   -177.00 -84.00   0.50   12.00    -- -104.52 -74.00  89.00  186
  6  \w     32.00  96.00   0.50   12.00    --  104.52 -74.00  89.00  128
  7  \w   -119.00 -87.00   0.50    4.00    --  -48.29-125.00 -60.00   64
  8  \w    -45.00  24.00   0.50    4.00    --  -48.29  38.00  30.00  138
  9  \w    -25.00  20.00   0.50    4.00    --   48.29 -19.00 150.00   90
 10  \w    -25.00  20.00   0.50    4.00    --   48.29 -19.00 120.00   90
 11  \w    -25.00  20.00   0.50    4.00    --   48.29 -19.00  90.00   90
 12  \w     28.00 120.00   0.50    4.00    --   48.29  74.00-142.00  184
 13  \w   -177.00-100.00   0.50   12.00    -- -104.52 -77.00-120.00  154
 14  \w   -106.00 -32.00   0.50   12.00    -- -104.52  93.00  24.77  148
 15  \w   -107.00 -32.00   0.50   12.00    -- -104.52 103.00 165.05  150
 16  \w   -177.00 -94.00   0.50   12.00    -- -104.52 -15.00-120.00  166
 17  \w   -177.00 -91.00   0.50   12.00    -- -104.52 -61.00-180.00  172
 18  \w    -75.00 -32.00   0.50   12.00    -- -104.52  61.00  60.00   86
 19  \w    100.00 177.00   0.50   12.00    --  104.52  77.00 -60.00  154
 20  \w     32.00  69.00   0.50   12.00    --  104.52 -61.00  90.00   74
 21  \w     32.00 105.00   0.50   12.00    --  104.52 -95.00 -60.00  146
 22  \w     32.00 105.00   0.50   12.00    --  104.52 -95.00   0.00  146
 23  \w     32.00 105.00   0.50   12.00    --  104.52 -95.00  60.00  146
 24  \w     84.00 177.00   0.50   12.00    --  104.52  74.00-142.00  186
 25  \w     32.00 105.00   0.50   12.00    --  104.52 -95.00-120.00  146
 26  \w     32.00 111.00   0.50   12.00    --  104.52-125.00  60.00  158
 27  \w     32.00  69.00   0.50   12.00    --  104.52 -61.00-120.00   74
 28  \w     32.00 105.00   0.50   12.00    --  104.52 -95.00-150.00  146
 29  \w     32.00  69.00   0.50   12.00    --  104.52 -61.00 120.00   74
 30  \w     32.00  69.00   0.50   12.00    --  104.52 -61.00-150.00   74
 31  \w     32.00 105.00   0.50   12.00    --  104.52 -95.00  90.00  146
 32  \w    100.00 177.00   0.50   12.00    --  104.52  77.00  90.00  154
 33  \w     94.00 177.00   0.50   12.00    --  104.52  45.00 -60.00  166
 34  \w     35.00 120.00   0.50    4.00    --   48.29  55.00 158.41  170
 35  \w     35.00 120.00   0.50    4.00    --   48.29  54.00 -48.66  170
 36  \w     36.00 120.00   0.50    4.00    --   48.29  53.00  84.83  168
 37  \w     35.00 120.00   0.50    4.00    --   48.29  56.00  33.73  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_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0982688000
_diffrn_orient_matrix_UB_12      -0.0421286000
_diffrn_orient_matrix_UB_13      0.0768643000
_diffrn_orient_matrix_UB_21      0.1184715000
_diffrn_orient_matrix_UB_22      0.0730111000
_diffrn_orient_matrix_UB_23      -0.0386567000
_diffrn_orient_matrix_UB_31      -0.0459153000
_diffrn_orient_matrix_UB_32      0.0986672000
_diffrn_orient_matrix_UB_33      0.0613123000
_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  0.0541
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29237
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.819
_diffrn_reflns_theta_min         3.727
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.203
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_description       plate
_exptl_crystal_F_000             940
_exptl_crystal_preparation
'Reaction of Fe6^0 with 9 equivalents of triphenylphosphine'
_exptl_crystal_recrystallization_method
'grown by slow evaporation of a diethylether solution at -20 Celsius'
_exptl_crystal_size_max          1.145
_exptl_crystal_size_mid          0.688
_exptl_crystal_size_min          0.149
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Flack x determined using 2763 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         6522
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0722P)^2^+2.9775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1226
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_full    0.929
_reflns_Friedel_fraction_max     0.878
_reflns_number_gt                6306
_reflns_number_total             6522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01370k3.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 1571968--1571976.cif.'
_cod_database_code               1571970
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Fe C O  P '
_chemical_oxdiff_usercomment     'pentane wash elution 2 '
_shelx_estimated_absorpt_t_max   0.172
_shelx_estimated_absorpt_t_min   0.018
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C23(H23), C25(H25), C19(H19), C27(H27), C21(H21), C29(H29),
 C18(H18), C33(H33), C32(H32), C24(H24), C20(H20), C26(H26), C30(H30), C31(H31)
;
_shelx_res_checksum              80778
_olex2_exptl_crystal_mounting_method mounted
_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 2.121
_oxdiff_exptl_absorpt_empirical_full_min 0.589