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_7713055
_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         'C40 H34 Mn2 N4 O8, 2(C2 H3 N)'
_chemical_formula_sum            'C44 H40 Mn2 N6 O8'
_chemical_formula_weight         890.7
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_update_record
;
2023-03-30 deposited with the CCDC.	2023-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                88.126(2)
_cell_angle_beta                 76.940(2)
_cell_angle_gamma                74.520(2)
_cell_formula_units_Z            1
_cell_length_a                   9.8533(2)
_cell_length_b                   10.0379(2)
_cell_length_c                   10.7928(3)
_cell_measurement_reflns_used    8057
_cell_measurement_temperature    23E1(8)
_cell_measurement_theta_max      78.526
_cell_measurement_theta_min      4.203
_cell_volume                     1001.71(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      23E1(8)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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    -50.00  32.00   0.50    3.50    --  -21.00  90.00 112.00  164
  2  \w     34.00  76.00   0.50    3.50    --   47.91 -90.00  -1.00   84
  3  \w    -18.00  27.00   0.50    3.50    --   47.91 -90.00  -1.00   90
  4  \w     43.00 103.00   0.50   12.00    --  112.86 -90.00  -1.00  120
  5  \w    -32.00  -6.00   0.50    3.50    --  -21.00 -57.00-180.00   52
  6  \w    -90.00 -40.00   0.50    3.50    --  -21.00 -57.00  30.00  100
  7  \w    -89.00 -64.00   0.50    3.50    --  -21.00 -57.00-180.00   50
  8  \w    -31.00  -6.00   0.50    3.50    --  -21.00 -57.00  30.00   50
  9  \w    -69.00 -13.00   0.50    3.50    --  -21.00 125.00   0.00  112
 10  \w      2.00  27.00   0.50    3.50    --   32.00  93.00  83.33   50
 11  \w     15.00  40.00   0.50    3.50    --   40.00  83.00 -81.93   50
 12  \w     15.00  40.00   0.50    3.50    --   44.00  90.00  81.00   50
 13  \w     15.00  40.00   0.50    3.50    --   44.00  90.00   3.51   50
 14  \w     15.00  40.00   0.50    3.50    --   44.00  91.00-160.41   50
 15  \w     17.00  42.00   0.50    3.50    --   44.00  87.00 -83.02   50
 16  \w     34.00  94.00   0.50    3.50    --   47.91-125.00 -30.00  120
 17  \w     93.00 125.00   0.50    3.50    --   52.00  77.00   6.50   64
 18  \w     33.00  61.00   0.50    3.50    --   52.00  77.00   6.50   56
 19  \w     34.00  75.00   0.50    3.50    --   56.00  76.00 127.08   82
 20  \w     38.00  88.00   0.50    3.50    --   60.00  76.00 -89.45  100
 21  \w     44.00  78.00   0.50    3.50    --   64.00  75.00  39.81   68
 22  \w     43.00  81.00   0.50    3.50    --   64.00  75.00 152.34   76
 23  \w     42.00  68.00   0.50    3.50    --   64.00  75.00  96.06   52
 24  \w     41.00  77.00   0.50    3.50    --   64.00  77.00-125.70   72
 25  \w     42.00  84.00   0.50    3.50    --   64.00  76.00-167.86   84
 26  \w    105.00 140.00   0.50    3.50    --   68.00  76.00 -68.21   70
 27  \w     88.00 114.00   0.50    3.50    --   68.00  68.00 105.31   52
 28  \w     46.00  86.00   0.50    3.50    --   68.00  76.00 -68.21   80
 29  \w     53.00 115.00   0.50    3.50    --   68.00  56.00 162.09  124
 30  \w     77.00 103.00   0.50    3.50    --   68.00  75.00 -35.22   52
 31  \w    101.00 139.00   0.50    3.50    --   68.00  76.00  48.53   76
 32  \w     45.00  73.00   0.50    3.50    --   68.00  77.00  -0.86   56
 33  \w     46.00  74.00   0.50    3.50    --   68.00  75.00 -35.22   56
 34  \w     51.00  78.00   0.50    3.50    --   68.00  68.00 105.31   54
 35  \w     47.00  93.00   0.50    3.50    --   68.00  76.00  48.53   92
 36  \w     67.00 104.00   0.50    3.50    --   72.00  35.00-104.38   74
 37  \w    126.00 177.00   0.50   12.00    --  104.00  70.00  69.60  102
 38  \w     84.00 122.00   0.50   12.00    --  104.00  70.00  69.60   76
 39  \w    101.00 147.00   0.50   12.00    --  112.86  61.00 -60.00   92
 40  \w    136.00 174.00   0.50   12.00    --  112.86  77.00-120.00   76
 41  \w     91.00 117.00   0.50   12.00    --  112.86  77.00-120.00   52
 42  \w     41.00 110.00   0.50   12.00    --  112.86-125.00 -60.00  138
 43  \w    131.00 158.00   0.50   12.00    --  112.86  61.00-180.00   54
 44  \w     41.00  66.00   0.50   12.00    --  112.86 -61.00-180.00   50
 45  \w    143.00 169.00   0.50   12.00    --  112.86  61.00-150.00   52
 46  \w    136.00 172.00   0.50   12.00    --  112.86  77.00 150.00   72
 47  \w     99.00 130.00   0.50   12.00    --  112.86  61.00-180.00   62
 48  \w     91.00 117.00   0.50   12.00    --  112.86  77.00  90.00   52
 49  \w     90.00 120.00   0.50   12.00    --  112.86  77.00 150.00   60
 50  \w     41.00  81.00   0.50   12.00    --  112.86 -77.00-150.00   80
 51  \w     41.00 102.00   0.50   12.00    --  112.86 -94.00  90.00  122
 52  \w    136.00 170.00   0.50   12.00    --  112.86  30.00 -90.00   68
 53  \w    102.00 127.00   0.50   12.00    --  112.86  30.00 -90.00   50
 54  \w     90.00 133.00   0.50   12.00    --  112.86  77.00 -30.00   86
 55  \w    144.00 175.00   0.50   12.00    --  112.86  77.00  90.00   62
 56  \w    102.00 132.50   0.50   12.00    --  112.86  61.00-150.00   61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0750002
_diffrn_orient_matrix_UB_12      -0.1033264
_diffrn_orient_matrix_UB_13      0.0759347
_diffrn_orient_matrix_UB_21      -0.0693605
_diffrn_orient_matrix_UB_22      0.107591
_diffrn_orient_matrix_UB_23      0.1103136
_diffrn_orient_matrix_UB_31      -0.1315091
_diffrn_orient_matrix_UB_32      0.0559537
_diffrn_orient_matrix_UB_33      -0.0596205
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12749
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        63.686
_diffrn_reflns_theta_max         63.686
_diffrn_reflns_theta_min         4.207
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.656
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.75307
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.2
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         3210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0399P)^2^+0.2307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0735
_reflns_Friedel_coverage         0
_reflns_number_gt                2939
_reflns_number_total             3210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01013a2.cif
_cod_data_source_block           21MA041_PN6078
_cod_database_code               7713055
_shelx_estimated_absorpt_t_min   0.501
_shelx_estimated_absorpt_t_max   0.707
_oxdiff_exptl_absorpt_empirical_details
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.407
_oxdiff_exptl_absorpt_empirical_full_min 0.676
_shelx_shelxl_version_number     2018/3
_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.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C9(H9), C8(H8), C14(H14), C2(H2), C12(H12), C13(H13), C17(H17),
 C3(H3), C5(H5), C4(H4)
        2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              84046
_shelx_hkl_checksum              41517