Mn(ii) betadiketonates: structural diversity from deceptively minor alterations to synthetic protocols
Ibrahim, Mukaila A.; Boeré, René T.; Preuss, Kathryn E.; RSC Advances 15 (2025) 32299–32308; doi:10.1039/D5RA03587B

data_7250840
_publ_section_title
;
 Mn(ii) betadiketonates: structural diversity from deceptively minor
 alterations to synthetic protocols
;
_journal_issue                   39
_journal_name_full               'RSC Advances'
_journal_page_first              32299
_journal_page_last               32308
_journal_paper_doi               10.1039/D5RA03587B
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C10 H12 F6 Mn O6, H2 O'
_chemical_formula_sum            'C10 H14 F6 Mn O7'
_chemical_formula_weight         415.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-06
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-07-07 deposited with the CCDC.	2025-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.495(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9445(8)
_cell_length_b                   6.9902(5)
_cell_length_c                   21.9193(19)
_cell_measurement_reflns_used    4991
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.7770
_cell_measurement_theta_min      4.1150
_cell_volume                     1637.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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   -105.00 -35.00   0.50    8.00    --  -38.50 -38.00-180.00  140
  2  \w   -105.00 -35.00   0.50    8.00    --  -38.50 -38.00  90.00  140
  3  \w    -62.00  26.00   0.50    8.00    --  -38.50  77.00-150.00  176
  4  \w   -101.00 -25.00   0.50    8.00    --  -38.50 -61.00-105.45  152
  5  \w    -42.00  28.00   0.50    8.00    --  -38.50  38.00 -90.00  140
  6  \w     34.00 104.00   0.50    8.00    --   47.06-136.00 173.00  140
  7  \w    107.00 178.00   0.50   16.00    --  111.00  25.00  60.00  142
  8  \w    105.00 175.00   0.50   16.00    --  111.00  50.00 120.00  140
  9  \w     47.00 117.00   0.50   16.00    --  111.00 -50.00 -60.00  140
 10  \w    105.00 175.00   0.50   16.00    --  111.00  50.00 120.00  140
 11  \w     47.00 117.00   0.50   16.00    --  111.00 -50.00 -30.00  140
 12  \w     42.00 115.00   0.50   16.00    --  111.00 -25.00 120.00  146
 13  \w     43.00 115.00   0.50   16.00    --  111.00 -28.00  -4.22  144
 14  \w     43.00 119.00   0.50   16.00    --  111.00 -16.00 172.00  152
 15  \w    108.00 177.00   0.50   16.00    --  111.00  38.00 -90.00  138
 16  \w    108.00 177.00   0.50   16.00    --  111.00  38.00 -90.00  138
 17  \w    108.00 177.00   0.50   16.00    --  111.00  38.00 150.00  138
 18  \w     42.00 115.00   0.50   16.00    --  111.00 -25.00 -90.00  146
 19  \w     42.00 115.00   0.50   16.00    --  111.00 -25.00-150.00  146
 20  \w     61.00 146.00   0.50   16.00    --  111.00 178.00   0.00  170
 21  \w     46.00 109.00   0.50   16.00    --  111.00-111.00-150.00  126
 22  \w     47.00 117.00   0.50   16.00    --  111.00 -50.00  60.00  140
 23  \w     47.00 117.00   0.50   16.00    --  111.00 -50.00 120.00  140
 24  \w     53.00  84.00   0.50   16.00    --  111.00 -50.00  30.00   62
 25  \w     48.00  78.00   0.50   16.00    --  111.00 -50.00  90.00   60
 26  \w     42.00  68.00   0.50   16.00    --  111.00  -5.00-111.85   52
 27  \w     77.00 105.00   0.50   16.00    --  111.00  -5.00-111.85   56
 28  \w    113.00 138.00   0.50   16.00    --  111.00  -5.00-111.85   50
 29  \w     52.00 102.00   0.50   16.00    --  111.00 -38.00-150.00  100
 30  \w    130.00 174.00   0.50   16.00    --  111.00  77.00-120.00   88
 31  \w     42.00  68.00   0.50   16.00    --  111.00 -12.00  30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0146945000
_diffrn_orient_matrix_UB_12      0.0649735000
_diffrn_orient_matrix_UB_13      0.0650931000
_diffrn_orient_matrix_UB_21      0.1072875000
_diffrn_orient_matrix_UB_22      -0.1341676000
_diffrn_orient_matrix_UB_23      0.0304430000
_diffrn_orient_matrix_UB_31      0.0954037000
_diffrn_orient_matrix_UB_32      0.1625537000
_diffrn_orient_matrix_UB_33      -0.0006496000
_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  0.1096
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13112
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.745
_diffrn_reflns_theta_min         4.132
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.482
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_description       plate
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.453
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.596
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         2937
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0891
_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^)+(0.1602P)^2^+4.5236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2354
_refine_ls_wR_factor_ref         0.2524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2246
_reflns_number_total             2937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra03587b2.cif
_cod_data_source_block           rb24064-rev2b
_cod_database_code               7250840
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C10H14F6MnO7
_chemical_oxdiff_usercomment
'One ugly needle from an aggreage of mostly plates.'
_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, All O(H,H) groups
2. Restrained distances
 O1S-H1SB = O1S-H1SA = O5-H5A = O5-H5B
 0.84 with sigma of 0.02
 O6-H6A = O6-H6B
 0.84 with sigma of 0.02
 Mn1-H6A \\sim Mn1-H6B
 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7)
3.b Idealised Me refined as rotating group:
 C5(H5C,H5D,H5E), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              36173
_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 2.875
_oxdiff_exptl_absorpt_empirical_full_min 0.383