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_7134132
_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         'C50 H70 Cl Fe Ir P4'
_chemical_formula_sum            'C50 H70 Cl Fe Ir P4'
_chemical_formula_weight         1078.44
_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
_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                 101.275(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.555(4)
_cell_length_b                   24.575(7)
_cell_length_c                   15.940(5)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    110
_cell_measurement_theta_max      32.27
_cell_measurement_theta_min      2.52
_cell_volume                     4823(3)
_computing_cell_refinement       SAINT
_computing_data_collection       Apex3
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0856
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            221640
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.090
_diffrn_reflns_theta_min         2.987
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.278
_exptl_absorpt_correction_T_max  0.518
_exptl_absorpt_correction_T_min  0.4004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       prism
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.514
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.249
_refine_diff_density_max         1.910
_refine_diff_density_min         -2.227
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         24558
_refine_ls_number_restraints     585
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0252P)^2^+3.6246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0707
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18932
_reflns_number_total             24558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06176d3.cif
_cod_data_source_block           Complex_7
_cod_depositor_comments
'Adding full bibliography for 7134131--7134135.cif.'
_cod_original_cell_volume        4823(2)
_cod_database_code               7134132
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.496
_shelx_estimated_absorpt_t_min   0.284
_olex2_refinement_description
;
1. Shared sites
{P1, P1'}
{P2, P2'}
{C15, C15'}
{C22, C22'}
{C23, C23'}
2. Restrained distances
 P1-C11 = P1'-C11' = P2-C12 = P2'-C12'
 1.85 with sigma of 0.008
3. Uiso/Uaniso restraints and constraints
Uanis(P1) = Uanis(P1')
Uanis(P2) = Uanis(P2')
Uanis(C15) = Uanis(C15')
Uanis(C22) = Uanis(C22')
Uanis(C23) = Uanis(C23')
Uanis(C11) = Uanis(C11')
Uanis(C12) = Uanis(C12')
Uanis(C13) = Uanis(C13')
Uanis(C14) = Uanis(C14')
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C22, C23, C24} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C22', C23', C24'}
{C11, C12, C13, C14, C15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C11', C12', C13', C14', C15'}
6. Others
 Sof(P1')=Sof(P2')=Sof(C11')=Sof(H11C)=Sof(H11D)=Sof(C12')=Sof(H12C)=Sof(H12D)=
 Sof(C13')=Sof(H13C)=Sof(H13D)=Sof(C14')=Sof(H14C)=Sof(H14D)=Sof(C15')=
 Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(P1)=Sof(P2)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=FVAR(1)
 Sof(C22')=Sof(H22C)=Sof(H22D)=Sof(C23')=Sof(H23C)=Sof(H23D)=Sof(C24')=
 Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(2)
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=
 Sof(H24B)=Sof(H24C)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C11'(H11C,H11D), C12'(H12C,H12D), C13'(H13C,H13D), C14'(H14C,H14D), C16(H16A,
 H16B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B), C22(H22A,H22B),
 C23(H23A,H23B), C22'(H22C,H22D), C23'(H23C,H23D), C25(H25A,H25B), C26(H26A,
 H26B)
7.b Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C15'(H15D,H15E,H15F), C24(H24A,H24B,H24C), C24'(H24D,
 H24E,H24F)
7.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
  C46(H46), C47(H47), C48(H48), C49(H49), C50(H50)
7.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C18(H18A,H18B,H18C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              18432
_shelx_hkl_checksum              87292
_olex2_submission_special_instructions 'No special instructions were received'