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_1571973
_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         'C52 H39 Fe4 O10 P3'
_chemical_formula_sum            'C52 H39 Fe4 O10 P3'
_chemical_formula_weight         1140.14
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-19
_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                 104.582(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2347(3)
_cell_length_b                   24.9460(6)
_cell_length_c                   19.6152(6)
_cell_measurement_reflns_used    9672
_cell_measurement_temperature    100.02(12)
_cell_measurement_theta_max      73.1950
_cell_measurement_theta_min      4.3910
_cell_volume                     4846.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_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      100.02(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.938
_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   -112.00 -12.00   1.00   30.00    --  -39.84 -57.00-150.00  100
  2  \w    -72.00  36.00   1.00   30.00    --  -39.84  77.00   0.00  108
  3  \w     34.00 133.00   1.00   37.50    --  107.09 -45.00 -60.00   99
  4  \w     79.00 178.00   1.00   37.50    --  107.09  30.00 120.00   99
  5  \w     24.00 107.00   1.00   37.50    --  107.09 -94.00 -90.00   83
  6  \w     34.00 112.00   1.00   37.50    --  107.09-125.00-120.00   78
  7  \w    103.00 178.00   1.00   37.50    --  107.09  77.00 -60.00   75
  8  \w     97.00 178.00   1.00   37.50    --  107.09 125.00-120.00   81
  9  \w   -112.00 -12.00   1.00   30.00    --  -39.84 -57.00  30.00  100
 10  \w   -112.00 -12.00   1.00   30.00    --  -39.84 -57.00 -60.00  100
 11  \w     79.00 178.00   1.00   37.50    --  107.09  30.00  30.00   99
 12  \w     54.00  85.00   1.00   37.50    --  107.09  15.00-120.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1488611000
_diffrn_orient_matrix_UB_12      -0.0151295000
_diffrn_orient_matrix_UB_13      0.0314302000
_diffrn_orient_matrix_UB_21      -0.0408285000
_diffrn_orient_matrix_UB_22      -0.0591841000
_diffrn_orient_matrix_UB_23      0.0033601000
_diffrn_orient_matrix_UB_31      0.0182461000
_diffrn_orient_matrix_UB_32      -0.0089636000
_diffrn_orient_matrix_UB_33      -0.0748392000
_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  0.0892
_diffrn_reflns_av_unetI/netI     0.0820
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24734
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.500
_diffrn_reflns_theta_min         2.925
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.843
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic greenish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_preparation       'From the reaction of 2 with Triphos in MeCN.'
_exptl_crystal_recrystallization_method
'Slow evaporation from a solution of 8 in diethyl ether.'
_exptl_crystal_size_max          0.426
_exptl_crystal_size_mid          0.227
_exptl_crystal_size_min          0.141
_refine_diff_density_max         1.616
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         9172
_refine_ls_number_restraints     414
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_gt           0.0804
_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^)+(0.1259P)^2^+13.9167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2005
_refine_ls_wR_factor_ref         0.2307
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6227
_reflns_number_total             9172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01370k3.cif
_cod_data_source_block           compound8
_cod_depositor_comments
'Adding full bibliography for 1571968--1571976.cif.'
_cod_database_code               1571973
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C108 H108 N108 O108 P108 Fe108 '
_chemical_oxdiff_usercomment     'black crystal, block'
_reflns_odcompleteness_completeness 95.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H00L(0.034) H00A(0.023) H00B(0.023) H00O(0.037) H00C(0.028)
 H00D(0.028) H00E(0.028) H00F(0.028) H00T(0.034) H00U(0.038) H00V(0.034)
 H00X(0.036) H00G(0.039) H00H(0.039) H00I(0.039) H00Z(0.028) H012(0.033)
 H016(0.039) H017(0.039) H018(0.043) H01B(0.045) H01C(0.037) H01F(0.045)
 H2(0.041) H01I(0.042) H01J(0.044) H01K(0.044) H01L(0.044) H01M(0.042)
 H01N(0.041) H01O(0.048) H01P(0.046) H01Q(0.047) H01S(0.054) H01T(0.064)
 H01U(0.06) H01V(0.049) H01W(0.054) H01X(0.053)
 Fixed X: H00L(0.910169) H00A(0.778159) H00B(0.708292) H00O(0.774155)
 H00C(0.636786) H00D(0.734787) H00E(0.496747) H00F(0.420893) H00T(0.658508)
 H00U(0.314576) H00V(1.311278) H00X(1.111261) H00G(0.555024) H00H(0.455259)
 H00I(0.440691) H00Z(1.111836) H012(0.953947) H016(0.905743) H017(1.313712)
 H018(0.807757) H01B(0.666595) H01C(0.377983) H01F(0.916419) H2(0.17656)
 H01I(0.994996) H01J(0.35317) H01K(0.163475) H01L(0.53927) H01M(0.616983)
 H01N(0.556331) H01O(0.465533) H01P(0.158205) H01Q(0.384766) H01S(0.186166)
 H01T(0.995456) H01U(0.804863) H01V(1.047114) H01W(0.377278) H01X(0.345327)
 Fixed Y: H00L(0.700249) H00A(0.710292) H00B(0.746465) H00O(0.553367)
 H00C(0.606886) H00D(0.652172) H00E(0.684024) H00F(0.648408) H00T(0.485955)
 H00U(0.640472) H00V(0.615003) H00X(0.734033) H00G(0.715214) H00H(0.668422)
 H00I(0.724003) H00Z(0.582942) H012(0.509801) H016(0.786885) H017(0.690243)
 H018(0.467541) H01B(0.885937) H01C(0.78204) H01F(0.404114) H2(0.819805)
 H01I(0.425364) H01J(0.874182) H01K(0.863918) H01L(0.510952) H01M(0.418472)
 H01N(0.837666) H01O(0.43186) H01P(0.6125) H01Q(0.578663) H01S(0.533566)
 H01T(0.943202) H01U(0.957228) H01V(0.858274) H01W(0.482088) H01X(0.510523)
 Fixed Z: H00L(0.933899) H00A(0.81825) H00B(0.863044) H00O(0.959539)
 H00C(0.882764) H00D(0.919854) H00E(0.721925) H00F(0.76515) H00T(0.755069)
 H00U(0.639682) H00V(0.934423) H00X(1.001536) H00G(0.914496) H00H(0.88383)
 H00I(0.845353) H00Z(0.863723) H012(0.807401) H016(0.857751) H017(1.003049)
 H018(1.005022) H01B(0.720565) H01C(0.656803) H01F(0.955946) H2(0.665449)
 H01I(0.858036) H01J(0.856745) H01K(0.765781) H01L(0.626723) H01M(0.826429)
 H01N(0.849589) H01O(0.894335) H01P(0.537858) H01Q(0.812984) H01S(0.483681)
 H01T(0.856745) H01U(0.766403) H01V(0.901222) H01W(0.52673) H01X(0.884857)
;
_shelx_res_checksum              43290
_olex2_date_sample_data_collection 2021-07-10
_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 3.678
_oxdiff_exptl_absorpt_empirical_full_min 0.415