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_1571974
_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 H27 Fe0.5 N P2, C11 H Fe3 O10, 0.5(C4 H10 O)'
_chemical_formula_sum            'C45 H33 Fe3.5 N O10.5 P2'
_chemical_formula_weight         1013.14
_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   mixed
_audit_creation_date             2023-01-18
_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                 94.5540(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.61041(12)
_cell_length_b                   15.93666(13)
_cell_length_c                   21.4660(2)
_cell_measurement_reflns_used    31980
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      76.9780
_cell_measurement_theta_min      3.4400
_cell_volume                     4300.36(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.25a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.25a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.25a (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)'
_diffrn_ambient_temperature      100.02(13)
_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 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            76437
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         3.458
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    10.529
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.42.25a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALES3 ABSPACK scaling algorithm.''
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       prism
_exptl_crystal_F_000             2060
_exptl_crystal_preparation
'From the reaction of 2 with 1,2-bis(diphenylphosphino)benzene in MeCN.'
_exptl_crystal_recrystallization_method
'Fractional distillation by repeated slow evaporation from diethyl ether at -20 degrees C.'
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         7871
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0361P)^2^+3.7934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7344
_reflns_number_total             7871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01370k3.cif
_cod_data_source_block           compound5
_cod_depositor_comments
'Adding full bibliography for 1571968--1571976.cif.'
_cod_original_formula_sum        'C45 H33 Fe3.50 N O10.50 P2'
_cod_database_code               1571974
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 C2A-C1A
 1.5 with sigma of 0.02
 C2A-C3A
 2.4 with sigma of 0.04
 O1A-C1A
 2.4 with sigma of 0.04
 C4A-C3A
 1.5 with sigma of 0.02
 O1A-C4A
 2.4 with sigma of 0.04
 O1A-C2A
 1.45 with sigma of 0.02
 O1A-C3A
 1.45 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C1A) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(C3A)
\\sim Ueq, Uanis(C4A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
3. Others
 Fixed Sof: O1A(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C2A(0.5) H2AA(0.5)
 H2AB(0.5) C3A(0.5) H3AA(0.5) H3AB(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5) H4AC(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C3A(H3AA,H3AB)
4.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22),
 C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
  C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40),
 C41(H41), C42(H42)
4.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C1A(H1AA,H1AB,H1AC), C4A(H4AA,H4AB,H4AC)
;
_shelx_res_checksum              15628
_olex2_submission_special_instructions 'No special instructions were received'