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_7713057
_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 H50 Mn N3 O4'
_chemical_formula_sum            'C36 H50 Mn N3 O4'
_chemical_formula_weight         643.73
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 98.1747(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.41996(13)
_cell_length_b                   11.69669(11)
_cell_length_c                   18.63705(16)
_cell_measurement_reflns_used    14091
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      27.909
_cell_measurement_theta_min      2.048
_cell_volume                     3543.05(5)
_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 1.3 (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      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 0.919
_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    -16.00  42.00   1.00   30.00    --   27.56  77.00-120.00   58
  2  \w    -16.00  42.00   1.00   30.00    --   27.56  77.00-180.00   58
  3  \w    -48.00  65.00   1.00   30.00    --   27.56 -57.00-120.00  113
  4  \w    -28.00 109.00   1.00   30.00    --   27.56  38.00  60.00  137
  5  \w    -48.00  58.00   1.00   30.00    --   27.56 -57.00 -30.00  106
  6  \w    -48.00  65.00   1.00   30.00    --   27.56 -57.00  60.00  113
;
_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      -0.0276199
_diffrn_orient_matrix_UB_12      0.0453612
_diffrn_orient_matrix_UB_13      -0.0110619
_diffrn_orient_matrix_UB_21      0.0031105
_diffrn_orient_matrix_UB_22      -0.0121536
_diffrn_orient_matrix_UB_23      -0.0368049
_diffrn_orient_matrix_UB_31      -0.0336348
_diffrn_orient_matrix_UB_32      -0.0383629
_diffrn_orient_matrix_UB_33      -0.0014068
_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  0.0286
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30799
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.154
_diffrn_reflns_theta_min         2.062
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.413
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.89153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.234
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.043
_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     412
_refine_ls_number_reflns         7983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+1.1770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0
_reflns_number_gt                6622
_reflns_number_total             7983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01013a2.cif
_cod_data_source_block           20MA105_PN5144
_cod_database_code               7713057
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.172
_oxdiff_exptl_absorpt_empirical_full_min 0.807
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              57784
_shelx_hkl_checksum              43038