Dual deoxygenation in an α-ketoimine chelated rhenium(III) complex: structural and mechanistic interpretations.
Sinha, Ankita; Banerjee, Suparna; Sen, Suphal; Ghosh, Aniruddha; Dey, Arindam; Naskar, Tilak; Singh, Tejender; Gangopadhyay, Jaydip; Dalton transactions (Cambridge, England : 2003) 54 (2025) 17137–17150; doi:10.1039/d5dt01782c

data_7719690
_publ_section_title
;
 Dual deoxygenation in an &#x3b1;-ketoimine chelated rhenium(III) complex:
 structural and mechanistic interpretations.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17137
_journal_page_last               17150
_journal_paper_doi               10.1039/d5dt01782c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C38 H29 Cl3 N2 O2 P Re, [+ solvents]1[CH2Cl2]'
_chemical_formula_sum            'C39 H31 Cl5 N2 O2 P Re'
_chemical_formula_weight         954.08
_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
_audit_creation_date             2025-10-10
_audit_creation_method
;
Olex2 1.5
(compiled 2025.02.27 svn.r83f5de26 for OlexSys, GUI svn.r7172)
;
_audit_update_record
;
2025-10-10 deposited with the CCDC.	2025-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                75.994(2)
_cell_angle_beta                 76.868(2)
_cell_angle_gamma                80.556(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0316(9)
_cell_length_b                   13.7471(12)
_cell_length_c                   15.4809(13)
_cell_measurement_reflns_used    9124
_cell_measurement_temperature    297.00
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.30
_cell_volume                     2203.5(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker APEX3'
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      297.00
_diffrn_measured_fraction_theta_full 0.998
_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  0.0364
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49025
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_min         1.908
_exptl_absorpt_coefficient_mu    3.129
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brownish
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       plate
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.136
_refine_diff_density_min         -1.497
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         7989
_refine_ls_number_restraints     366
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0371
_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^)+9.5778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7152
_reflns_number_total             7989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01782c2.cif
_cod_data_source_block           ccdc_2394052
_cod_depositor_comments
'Adding full bibliography for 7719689--7719690.cif.'
_cod_database_code               7719690
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.745
_shelx_estimated_absorpt_t_min   0.573
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
C2 \\sim C7 \\sim C6 \\sim C5 \\sim C4 \\sim C3 \\sim C2A \\sim C3A \\sim C4A
\\sim C5A \\sim C6A \\sim C7A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C9 \\sim C14 \\sim C10 \\sim C13 \\sim C11 \\sim C12 \\sim C9A \\sim C10A \\sim
C11A \\sim C12A \\sim C13A \\sim C14A: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
2. Others
 Sof(C9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=
 Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=1-FVAR(1)
 Sof(C9)=Sof(C14)=Sof(H14)=Sof(C13)=Sof(H13)=Sof(C12)=Sof(H12)=Sof(C11)=
 Sof(H11)=Sof(C10)=Sof(H10)=FVAR(1)
 Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=
 Sof(H6A)=Sof(C7A)=Sof(H7A)=1-FVAR(2)
 Sof(C2)=Sof(C7)=Sof(H7)=Sof(C6)=Sof(H6)=Sof(C5)=Sof(H5)=Sof(C4)=Sof(H4)=
 Sof(C3)=Sof(H3)=FVAR(2)
3.a Aromatic/amide H refined with riding coordinates:
 C38(H38), C26(H26), C20(H20), C37(H37), C34(H34), C16(H16), C19(H19),
 C35(H35), C18(H18), C28(H28), C22(H22), C25(H25), C24(H24), C32(H32), C29(H29),
  C17(H17), C30(H30), C23(H23), C31(H31), C14(H14), C13(H13), C12(H12),
 C11(H11), C10(H10), C10A(H10A), C11A(H11A), C12A(H12A), C13A(H13A), C14A(H14A),
  C7(H7), C6(H6), C5(H5), C4(H4), C3(H3), C3A(H3A), C4A(H4A), C5A(H5A),
 C6A(H6A), C7A(H7A)
3.b Fitted hexagon refined as free rotating group:
 C9(C14,C13,C12,C11,C10), C9A(C10A,C11A,C12A,C13A,C14A), C2(C7,C6,C5,C4,C3),
 C2A(C3A,C4A,C5A,C6A,C7A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              96412
_shelx_hkl_checksum              78583
_shelx_fab_checksum              37888
_olex2_submission_special_instructions 'No special instructions were received'