Ring strain governs transmetalation behaviour at a tucked-in iron complex.
Durfy, Connor S.; Huang, Michelle; Zurakowski, Joseph A.; Boyle, Paul D.; Drover, Marcus W.; Chemical communications (Cambridge, England) 61 (2025) 3323–3326; doi:10.1039/d4cc06176d

data_7134134
_publ_section_title
;
 Ring strain governs transmetalation behaviour at a tucked-in iron
 complex.
;
_journal_issue                   16
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3323
_journal_page_last               3326
_journal_paper_doi               10.1039/d4cc06176d
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C32 H58 Cl Fe Ir P2'
_chemical_formula_sum            'C32 H58 Cl Fe Ir P2'
_chemical_formula_weight         788.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-08-30
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-30 deposited with the CCDC.	2025-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.854(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
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_cell_length_b                   11.404(4)
_cell_length_c                   18.851(6)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    110
_cell_measurement_theta_max      30.57
_cell_measurement_theta_min      2.80
_cell_volume                     6508(4)
_computing_cell_refinement       SAINT
_computing_data_collection       Apex3
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
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_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      110
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Bruker Apex2'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa Axis Apex2'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            152914
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.144
_diffrn_reflns_theta_min         1.345
_diffrn_source                   'sealed tube'
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_exptl_absorpt_correction_T_max  0.6591
_exptl_absorpt_correction_T_min  0.4085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       prism
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.708
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_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+3.1576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0656
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_reflns_number_gt                12715
_reflns_number_total             16668
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06176d3.cif
_cod_data_source_block           Complex_4
_cod_depositor_comments
'Adding full bibliography for 7134131--7134135.cif.'
_cod_database_code               7134134
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.718
_shelx_estimated_absorpt_t_min   0.263
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C11(H11), C12(H12), C15(H15), C16(H16)
1.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C13(H13A,H13B), C14(H14A,H14B), C17(H17A,H17B), C18(H18A,H18B),
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B),
  C25(H25A,H25B), C27(H27A,H27B), C28(H28A,H28B), C30(H30A,H30B), C31(H31A,H31B)
1.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C32(H32A,H32B,
 H32C)
;
_shelx_res_checksum              74141
_shelx_hkl_checksum              85199
_olex2_submission_special_instructions 'No special instructions were received'