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_1571972
_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         'C18 Fe6 O17'
_chemical_formula_sum            'C18 Fe6 O17'
_chemical_formula_weight         823.28
_chemical_name_systematic        Fe6C(CO)17
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_audit_creation_date             2024-05-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-05-25 deposited with the CCDC.	2024-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.433(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9478(3)
_cell_length_b                   8.96230(10)
_cell_length_c                   17.1515(3)
_cell_measurement_reflns_used    7441
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      76.3210
_cell_measurement_theta_min      4.9430
_cell_volume                     2352.69(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (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 0.994
_diffrn_measured_fraction_theta_max 0.950
_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   -115.00 -34.00   0.50    1.44    -- -105.11  77.00 -30.00  162
  2  \w    -75.00 -33.00   0.50    1.44    -- -105.11  61.00 -30.00   84
  3  \w   -132.00 -58.00   0.50    1.44    -- -105.11  88.00 128.00  148
  4  \w    -70.00  24.00   0.50    0.40    --  -48.33  88.00 128.00  188
  5  \w     82.00 120.00   0.50    0.40    --   48.33  57.00 -60.00   76
  6  \w     84.00 117.00   0.50    0.40    --   48.33  57.00-150.00   66
  7  \w     85.00 121.00   0.50    0.40    --   48.33  57.00  90.00   72
  8  \w     79.00 176.00   0.50    1.44    --  105.11  88.00 128.00  194
  9  \w     34.00  69.00   0.50    1.44    --  105.11 -61.00  60.00   70
 10  \w     38.00  69.00   0.50    1.44    --  105.11 -61.00 150.00   62
 11  \w     33.00  69.00   0.50    1.44    --  105.11 -61.00  30.00   72
 12  \w     35.00  62.00   0.50    1.44    --  105.11 -61.00-120.00   54
 13  \w    -23.00   2.00   0.50    0.40    --   48.33 -88.00  12.00   50
 14  \w     58.00  83.00   0.50    1.44    --  105.11 -88.00  12.00   50
 15  \w     10.00  74.00   0.50    0.40    --   48.33 -88.00  12.00  128
 16  \w   -119.00 -82.00   0.50    0.40    --  -48.33 -57.00 120.00   74
 17  \w   -176.00-135.00   0.50    1.44    -- -105.11 -88.00  12.00   82
 18  \w   -177.00 -95.00   0.50    1.44    -- -105.11 -15.00  90.00  164
;
_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  0.0384
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15524
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.809
_diffrn_reflns_theta_min         2.887
_exptl_absorpt_coefficient_mu    29.717
_exptl_absorpt_correction_T_max  0.407
_exptl_absorpt_correction_T_min  0.133
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
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    2.324
_exptl_crystal_description       prism
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         4728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0436P)^2^+3.4308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4141
_reflns_number_total             4728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01370k3.cif
_cod_data_source_block           abscor_fe6cco17
_cod_depositor_comments
;
Adding full bibliography for 1571968--1571976.cif.

2025-07-10
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C36 Fe12 O34'
_cod_original_formula_weight         1646.56
_cod_original_formula_moiety         '2(C18 Fe6 O17)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        2352.69(7)
_cod_database_code               1571972
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.230
_shelx_estimated_absorpt_t_min   0.095
_olex2_refinement_description
;
;
_shelx_res_checksum              9724
_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
;