Oxidatively-induced C(sp<sup>3</sup>)-C(sp<sup>3</sup>) bond formation at a tucked-in iron(iii) complex.
Zurakowski, Joseph A.; Durfy, Connor S.; Stocek, Noah B.; Fanchini, Giovanni; Drover, Marcus W.; Chemical science 15 (2024) 10359–10365; doi:10.1039/d4sc03292f

data_1571896
_publ_section_title
;
 Oxidatively-induced C(sp<sup>3</sup>)-C(sp<sup>3</sup>) bond formation at
 a tucked-in iron(iii) complex.
;
_journal_issue                   27
_journal_name_full               'Chemical science'
_journal_page_first              10359
_journal_page_last               10365
_journal_paper_doi               10.1039/d4sc03292f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C48 Fe2 I2 P4, C6, 0.28[C6H6]'
_chemical_formula_sum            'C54 H98 Fe2 I2 P4'
_chemical_formula_weight         1236.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-03-20 deposited with the CCDC.	2024-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                69.02(3)
_cell_angle_beta                 75.24(3)
_cell_angle_gamma                75.18(3)
_cell_formula_units_Z            1
_cell_length_a                   8.878(5)
_cell_length_b                   11.878(8)
_cell_length_c                   15.700(8)
_cell_measurement_reflns_used    9796
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.41
_cell_volume                     1469.8(15)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            96963
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.404
_diffrn_reflns_theta_min         1.957
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.685
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1058 before and 0.0763 after correction.
The Ratio of minimum to maximum transmission is 0.9126.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear bluish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       plate
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.460
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         7331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0546P)^2^+3.1634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1192
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6298
_reflns_number_total             7331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03292f3.cif
_cod_data_source_block           final11
_cod_depositor_comments          'Adding full bibliography for 1571896.cif.'
_cod_original_cell_volume        1469.7(15)
_cod_database_code               1571896
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.850
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C1(H1A,H1B), C23(H23A,H23B), C16(H16A,H16B), C13(H13A,H13B),
 C19(H19A,H19B), C17(H17A,H17B), C11(H11A,H11B), C20(H20A,H20B), C12(H12A,H12B),
  C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C25(H25), C27(H27)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C24(H24A,H24B,H24C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C),
 C18(H18A,H18B,H18C), C8(H8A,H8B,H8C), C21(H21A,H21B,H21C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              95867
_shelx_hkl_checksum              96106
_olex2_submission_special_instructions 'No special instructions were received'