Manganese(III) complexes stabilized with N-heterocyclic carbene ligands for alcohol oxidation catalysis
Rigoni, Giacomo; Nylund, Pamela Viktoria Sofie; Albrecht, Martin; Dalton Transactions  (2023) –; doi:10.1039/D3DT01013A

data_7713056
_publ_section_title
;
 Manganese(III) complexes stabilized with N-heterocyclic carbene ligands
 for alcohol oxidation catalysis
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01013A
_journal_year                    2023
_chemical_formula_moiety         'C36 H49 Mn N2 O4'
_chemical_formula_sum            'C36 H49 Mn N2 O4'
_chemical_formula_weight         628.71
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-30
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-03-30 deposited with the CCDC.	2023-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                62.126(4)
_cell_angle_beta                 80.257(3)
_cell_angle_gamma                78.894(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2841(3)
_cell_length_b                   13.6750(5)
_cell_length_c                   14.2509(5)
_cell_measurement_reflns_used    11789
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      27.837
_cell_measurement_theta_min      2.01
_cell_volume                     1731.21(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0965
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -28.00 109.00   1.00   30.00    --   27.56  38.00 -30.00  137
  2  \w    -42.00  71.00   1.00   30.00    --   27.56 -77.00 -60.00  113
  3  \w    -10.00 104.00   1.00   30.00    --   27.56  57.00  60.00  114
  4  \w     39.00 122.00   1.00   30.00    --   27.56 178.00-120.00   83
  5  \w    -48.00  65.00   1.00   30.00    --   27.56 -57.00-180.00  113
  6  \w    -16.00  42.00   1.00   30.00    --   27.56  77.00-120.00   58
  7  \w    -10.00 104.00   1.00   30.00    --   27.56  57.00 150.00  114
  8  \w    -54.00  83.00   1.00   30.00    --   27.56 -38.00   0.00  137
  9  \w    -43.00  -7.00   1.00   30.00    --   27.56 127.00 -15.38   36
 10  \w    -67.00  42.00   1.00   30.00    --  -23.50  77.00 -90.00  109
 11  \w    -15.00  32.00   1.00   30.00    --  -23.50 -99.00  60.00   47
 12  \w     59.00 104.00   1.00   30.00    --   27.56  57.00-180.00   45
 13  \w    -42.00  71.00   1.00   30.00    --   27.56 -77.00-150.00  113
 14  \w    -15.00  83.00   1.00   30.00    --   27.56 -99.00 -30.00   98
 15  \w    -63.00 119.00   1.00   30.00    --   27.56   0.00-180.00  182
 16  \w    -16.00  42.00   1.00   30.00    --   27.56  77.00 -30.00   58
 17  \w    -63.00  16.00   1.00   30.00    --   27.56   0.00-150.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0320242
_diffrn_orient_matrix_UB_12      -0.0509425
_diffrn_orient_matrix_UB_13      0.037589
_diffrn_orient_matrix_UB_21      0.0204819
_diffrn_orient_matrix_UB_22      0.0289506
_diffrn_orient_matrix_UB_23      0.0241182
_diffrn_orient_matrix_UB_31      -0.0594699
_diffrn_orient_matrix_UB_32      -0.0083113
_diffrn_orient_matrix_UB_33      0.0346734
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.073
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            40807
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.364
_diffrn_reflns_theta_min         1.623
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.42
_exptl_absorpt_correction_T_max  0.9411
_exptl_absorpt_correction_T_min  0.9411
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
        Spherical absorption correction
        using equivalent radius and absorption coefficient.
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.133
_refine_diff_density_max         2.558
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.1
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         7068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0751
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1175P)^2^+2.6937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.205
_refine_ls_wR_factor_ref         0.2158
_reflns_Friedel_coverage         0
_reflns_number_gt                5880
_reflns_number_total             7068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01013a2.cif
_cod_data_source_block           20MA104_PN5150
_cod_original_cell_volume        1731.22(12)
_cod_database_code               7713056
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C23(H23), C9(H9), C3(H3), C2(H2), C7(H7), C33(H33)
1.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C17(H17A,H17B,
 H17C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C), C31(H31A,H31B,H31C), C12(H12A,
 H12B,H12C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C13(H13A,H13B,H13C),
 C35(H35A,H35B,H35C), C14(H14A,H14B,H14C), C36(H36A,H36B,H36C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              7746
_shelx_hkl_checksum              46289
_shelx_fab_checksum              71031
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.260
_oxdiff_exptl_absorpt_empirical_full_min 0.807