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_7719689
_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         'C32 H26 Cl3 N O2 P Re'
_chemical_formula_sum            'C32 H26 Cl3 N O2 P Re'
_chemical_formula_weight         780.06
_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   mixed
_audit_creation_date             2025-08-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-08-25 deposited with the CCDC.	2025-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.389(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5959(6)
_cell_length_b                   19.8922(10)
_cell_length_c                   14.4642(7)
_cell_measurement_reflns_used    14128
_cell_measurement_temperature    154.99
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.38
_cell_volume                     3048.6(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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      154.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0752
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26950
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         2.178
_exptl_absorpt_coefficient_mu    4.331
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.1005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1669 before and 0.0855 after correction.
The Ratio of minimum to maximum transmission is 0.1348.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.091
_refine_diff_density_min         -2.261
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+6.5982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4784
_reflns_number_total             5503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01782c2.cif
_cod_data_source_block           mo_tn151222_0m
_cod_depositor_comments
'Adding full bibliography for 7719689--7719690.cif.'
_cod_database_code               7719689
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C26(H26), C7(H7), C32(H32), C10(H10), C22(H22), C28(H28), C20(H20), C3(H3),
 C24(H24), C6(H6), C5(H5), C23(H23), C16(H16), C11(H11), C25(H25), C14(H14),
 C4(H4), C19(H19), C31(H31), C30(H30), C29(H29), C17(H17), C12(H12), C13(H13),
 C18(H18)
;
_shelx_res_checksum              71831
_shelx_hkl_checksum              48715
_olex2_submission_special_instructions 'No special instructions were received'