FeII complexes supported by an Iminophosphorane ligand: Synthesis and Reactivity
Tannoux, Thibault; Mazaud, Louis; Cheisson, Thibault; Casaretto, Nicolas; Auffrant, Audrey; Dalton Transactions  (2023) –; doi:10.1039/D3DT00950E

data_7713581
_publ_section_title
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 FeII complexes supported by an Iminophosphorane ligand: Synthesis and
 Reactivity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00950E
_journal_year                    2023
_chemical_formula_moiety         'C39 H32 F6 Fe N2 O6 P2 S2'
_chemical_formula_sum            'C39 H32 F6 Fe N2 O6 P2 S2'
_chemical_formula_weight         920.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-16 deposited with the CCDC.	2023-07-26 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 93.038(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8695(10)
_cell_length_b                   23.485(2)
_cell_length_c                   14.6125(12)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      26.562
_cell_measurement_theta_min      2.442
_cell_volume                     4067.6(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0505
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            87327
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.537
_diffrn_reflns_theta_min         2.430
_diffrn_source_current           31.0
_diffrn_source_power             1.705
_diffrn_source_voltage           55.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0671 before and 0.0546 after correction.
The Ratio of minimum to maximum transmission is 0.9478.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       needle
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.053
_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     560
_refine_ls_number_reflns         9356
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+2.5593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0850
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7697
_reflns_number_total             9356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00950e2.cif
_cod_data_source_block           '[LFe(OTf)2]'
_cod_database_code               7713581
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.787
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 S1-C39A \\sim S1-C39B
 with sigma of 0.02
 F6A-C39A \\sim F6B-C39B
 with sigma of 0.02
 F5A-F4A \\sim F5B-F4B
 with sigma of 0.04
 F5A-C39A \\sim F5B-C39B
 with sigma of 0.02
 F4A-C39A \\sim F4B-C39B
 with sigma of 0.02
 S1-F6A \\sim S1-F6B
 with sigma of 0.04
 S1-F5A \\sim S1-F5B
 with sigma of 0.04
 S1-F4A \\sim S1-F4B
 with sigma of 0.04
 F6A-F5A \\sim F6B-F5B
 with sigma of 0.04
 F6A-F4A \\sim F6B-F4B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
F4A \\sim F5A \\sim F6A \\sim C39A \\sim F4B \\sim F5B \\sim F6B \\sim C39B:
within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A
4. Others
 Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(C39B)=1-FVAR(1)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(C39A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
5.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C23(H23), C24(H24), C19(H19), C8(H8), C9(H9), C10(H10),
 C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C2(H2),
 C3(H3), C4(H4), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33),
 C34(H34), C35(H35), C36(H36), C37(H37)
;
_shelx_res_checksum              19662
_olex2_submission_special_instructions 'No special instructions were received'