Electronic structure and magnetic properties of rhenium complexes with an iminoxolene ligand: experimental and computational studies.
Petrov, Pavel A.; Dmitriev, Alexey A.; Semikina, Anastasiia D.; Eltsov, Ilia V.; Sukhikh, Taisiya S.; Lavrov, Alexander N.; Gushchin, Artem L.; Sokolov, Maxim N.; Gritsan, Nina P.; Dalton transactions (Cambridge, England : 2003) 55 (2026) 3428–3441; doi:10.1039/d5dt02698a

data_7720303
_publ_section_title
;
 Electronic structure and magnetic properties of rhenium complexes with an
 iminoxolene ligand: experimental and computational studies.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3428
_journal_page_last               3441
_journal_paper_doi               10.1039/d5dt02698a
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C44 H52 Cl3 N O2 P Re, 4(C6 H6)'
_chemical_formula_sum            'C68 H76 Cl3 N O2 P Re'
_chemical_formula_weight         1262.81
_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             2023-07-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-03-18 deposited with the CCDC.	2026-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                79.9600(10)
_cell_angle_beta                 83.9670(10)
_cell_angle_gamma                79.2710(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5787(3)
_cell_length_b                   11.9253(3)
_cell_length_c                   23.4028(6)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.65
_cell_measurement_theta_min      2.60
_cell_volume                     3117.51(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            48882
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.706
_diffrn_reflns_theta_min         2.300
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.146
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0850 before and 0.0458 after correction.
The Ratio of minimum to maximum transmission is 0.9061.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       prism
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         15973
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+0.2439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0479
_refine_ls_wR_factor_ref         0.0495
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14394
_reflns_number_total             15973
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02698a2.cif
_cod_data_source_block           ads25c2
_cod_database_code               7720303
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.830
_shelx_estimated_absorpt_t_min   0.783
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6A-C1A = C2A-C1A = C3A-C2A = C4A-C3A = C5A-C4A = C6A-C5A = C3B-C2B = C2B-C1B
 = C6B-C1B = C6B-C5B = C5B-C4B = C4B-C3B = C2E-C1E = C2E-C3E = C3E-C4E = C4E-
 C5E = C5E-C6E = C1E-C6E = C2F-C1F = C2F-C3F = C4F-C3F = C5F-C4F = C6F-C5F =
 C6F-C1F
 1.39 with sigma of 0.02
 C9A-C7 = C8-C7 = C8A-C7 = C7-C10 = C7-C10A = C9-C7
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C7, C8, C9, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1E, C2E, C3E, C4E, C5E, C6E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1B, C2B, C3B, C4B, C5B, C6B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1A, C2A, C3A, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1F, C2F, C3F, C4F, C5F, C6F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C1E)=Sof(H1E)=Sof(C2E)=Sof(H2E)=Sof(C3E)=Sof(H3E)=Sof(C4E)=Sof(H4E)=
 Sof(C5E)=Sof(H5E)=Sof(C6E)=Sof(H6E)=1-FVAR(1)
 Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=
 Sof(C5B)=Sof(H5B)=Sof(C6B)=Sof(H6B)=FVAR(1)
 Sof(C1F)=Sof(H1F)=Sof(C2F)=Sof(H2F)=Sof(C3F)=Sof(H3F)=Sof(C4F)=Sof(H4F)=
 Sof(C5F)=Sof(H5F)=Sof(C6F)=Sof(H6F)=1-FVAR(2)
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=
 Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=FVAR(2)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=
 Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(3)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C21(H21), C24(H24)
6.b Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC), C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC),
 C10(H10A,H10B,H10C), C10A(H10D,H10E,H10F)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C18(H18), C19(H19), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40),
  C41(H41), C42(H42), C43(H43), C44(H44), C1A(H1A), C2A(H2A), C3A(H3A),
 C4A(H4A), C5A(H5A), C6A(H6A), C1B(H1B), C2B(H2B), C3B(H3B), C4B(H4B), C5B(H5B),
  C6B(H6B), C1C(H1C), C2C(H2C), C3C(H3C), C4C(H4C), C5C(H5C), C6C(H6C),
 C1D(H1D), C2D(H2D), C3D(H3D), C4D(H4D), C5D(H5D), C6D(H6D), C1E(H1E), C2E(H2E),
  C3E(H3E), C4E(H4E), C5E(H5E), C6E(H6E), C1F(H1F), C2F(H2F), C3F(H3F),
 C4F(H4F), C5F(H5F), C6F(H6F)
6.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              98620
_shelx_hkl_checksum              98585
_olex2_submission_special_instructions 'No special instructions were received'