The importance of understanding (pre)catalyst activation in versatile C-H bond functionalisations catalysed by [Mn<sub>2</sub>(CO)<sub>10</sub>].
Eastwood, Jonathan B.; Burden, Thomas J.; Hammarback, L. Anders; Horbaczewskyj, Chris; Tanner, Theo F. N.; Clark, Ian P.; Greetham, Gregory; Towrie, Michael; Fairlamb, Ian J. S.; Lynam, Jason M.; Chemical science 15 (2024) 9183–9191; doi:10.1039/d4sc01215a

data_1571534
_publ_section_title
;
 The importance of understanding (pre)catalyst activation in versatile C-H
 bond functionalisations catalysed by [Mn<sub>2</sub>(CO)<sub>10</sub>].
;
_journal_issue                   24
_journal_name_full               'Chemical science'
_journal_page_first              9183
_journal_page_last               9191
_journal_paper_doi               10.1039/d4sc01215a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C24 H15 Mn2 N O11'
_chemical_formula_sum            'C24 H15 Mn2 N O11'
_chemical_formula_weight         603.25
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-20 deposited with the CCDC.	2024-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                110.200(6)
_cell_angle_beta                 94.410(5)
_cell_angle_gamma                92.531(5)
_cell_formula_units_Z            2
_cell_length_a                   9.0789(5)
_cell_length_b                   11.2974(8)
_cell_length_c                   12.7130(8)
_cell_measurement_reflns_used    3682
_cell_measurement_temperature    110.00(14)
_cell_measurement_theta_max      28.9660
_cell_measurement_theta_min      3.5260
_cell_volume                     1216.63(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.854
_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     58.00  87.00   1.00    1.73    --   18.24  57.00-120.00   29
  2  \w    -51.00  38.00   1.00    1.73    --   18.24 -57.00  90.00   89
  3  \w     39.00  66.00   1.00    1.73    --   18.24 178.00  90.00   27
  4  \w    -15.00  56.00   1.00    1.73    --   18.24 -99.00-150.00   71
  5  \w    -48.00  36.00   1.00    1.73    --   18.24 -57.00 -30.00   84
  6  \w    -27.00  11.00   1.00    1.73    --  -18.55 -77.00   0.00   38
  7  \w    -36.00  -2.00   1.00    1.73    --  -18.55 -77.00 -90.00   34
  8  \w    -15.00  12.00   1.00    1.73    --  -18.55 -77.00-150.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0078022000
_diffrn_orient_matrix_UB_12      -0.0536894000
_diffrn_orient_matrix_UB_13      0.0164841000
_diffrn_orient_matrix_UB_21      -0.0290794000
_diffrn_orient_matrix_UB_22      -0.0372486000
_diffrn_orient_matrix_UB_23      -0.0556454000
_diffrn_orient_matrix_UB_31      0.0725863000
_diffrn_orient_matrix_UB_32      -0.0152052000
_diffrn_orient_matrix_UB_33      -0.0141648000
_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  0.0248
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9897
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.023
_diffrn_reflns_theta_min         3.557
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_recrystallization_method Hexane
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.292
_exptl_crystal_size_min          0.224
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+0.5942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4629
_reflns_number_total             5548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01215a2.cif
_cod_data_source_block           jml21009
_cod_depositor_comments          'Adding full bibliography for 1571534.cif.'
_cod_database_code               1571534
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     'Jonny Eastwood Jbe-5-385'
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.661
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C4(H4), C3(H3), C14(H14), C11(H11), C10(H10), C13(H13), C6(H6), C7(H7)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              96974
_olex2_date_sample_data_collection 2021-06-11
_olex2_exptl_crystal_mounting_method 'Oil on 200um mount'
_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 1.159
_oxdiff_exptl_absorpt_empirical_full_min 0.844