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_7713580
_publ_section_title
;
 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         'C52 H59 Fe N5 P2, 2(Cl), C H2 Cl2'
_chemical_formula_sum            'C53 H61 Cl4 Fe N5 P2'
_chemical_formula_weight         1027.65
_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             2022-11-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-12-16 deposited with the CCDC.	2023-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.507(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.298(5)
_cell_length_b                   17.214(5)
_cell_length_c                   25.028(10)
_cell_measurement_reflns_used    9311
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      24.119
_cell_measurement_theta_min      2.300
_cell_volume                     5547(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0745
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            154394
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.029
_diffrn_reflns_theta_min         1.594
_diffrn_source_current           31.0
_diffrn_source_power             1.705
_diffrn_source_voltage           55.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.7074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0887 before and 0.0615 after correction.
The Ratio of minimum to maximum transmission is 0.9491.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       prism
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.903
_refine_diff_density_min         -1.042
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         10914
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0669P)^2^+9.5819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1468
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8858
_reflns_number_total             10914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00950e2.cif
_cod_data_source_block           '[LFe(NCtBu)3](OTf)2'
_cod_original_cell_volume        5546(3)
_cod_database_code               7713580
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.896
_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. Restrained distances
 C20-C19 \\sim C20A-C19
 with sigma of 0.02
 C22-C19 \\sim C22A-C19
 with sigma of 0.02
 C21-C19 \\sim C21A-C19
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C20 \\sim C22 \\sim C19 \\sim C21: within 2A with sigma of 0.004 and sigma for
terminal atoms of 0.008 within 2A
C20 \\sim C22 \\sim C21 \\sim C19 \\sim C20A \\sim C22A \\sim C21A: within 2A
with sigma of 0.004 and sigma for terminal atoms of 0.008 within 2A
4. Others
 Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C6(H6A,H6B), C53(H53A,H53B)
5.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C48(H48), C2(H2), C4(H4), C24(H24), C39(H39), C44(H44), C3(H3),
 C49(H49), C37(H37), C25(H25), C40(H40), C45(H45), C43(H43), C33(H33), C38(H38),
  C50(H50), C32(H32), C34(H34), C30(H30), C31(H31), C52(H52), C51(H51),
 C46(H46), C42(H42), C26(H26), C28(H28), C27(H27)
5.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C12(H12A,H12B,
 H12C), C17(H17A,H17B,H17C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C18(H18A,
 H18B,H18C), C21(H21A,H21B,H21C), C20A(H20D,H20E,H20F), C22A(H22D,H22E,H22F),
 C21A(H21D,H21E,H21F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              68321
_shelx_fab_checksum              95540
_olex2_submission_special_instructions 'No special instructions were received'