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_7250837
_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         'C15 H12 F9 K Mn O6'
_chemical_formula_sum            'C15 H12 F9 K Mn O6'
_chemical_formula_weight         553.29
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-14
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-04-05 deposited with the CCDC.	2025-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4514(3)
_cell_length_b                   13.7819(3)
_cell_length_c                   10.8398(2)
_cell_measurement_reflns_used    7372
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      79.8440
_cell_measurement_theta_min      5.1900
_cell_volume                     2009.55(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.88a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.995
_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 -74.50   0.50    0.97    --  -38.50 -38.00 -60.00   61
  2  \w   -105.00 -35.00   0.50    0.97    --  -38.50 -38.00-180.00  140
  3  \w     28.00  97.00   0.50    0.97    --   47.81-125.00 -90.00  138
  4  \w     28.00  97.00   0.50    0.97    --   47.81-125.00   0.00  138
  5  \w     42.00 121.00   0.50    3.88    --  111.00 -12.00 120.00  158
  6  \w     46.00 109.00   0.50    3.88    --  111.00-111.00   0.00  126
  7  \w     42.00 115.00   0.50    3.88    --  111.00 -25.00 150.00  146
  8  \w     46.00 109.00   0.50    3.88    --  111.00-111.00 -30.00  126
  9  \w     42.00 115.00   0.50    3.88    --  111.00 -25.00-150.00  146
 10  \w     64.00 106.00   0.50    3.88    --  111.00 -91.00 120.00   84
 11  \w    110.00 136.00   0.50    3.88    --  111.00  77.00 -60.00   52
 12  \w     77.00 103.00   0.50    3.88    --  111.00 -63.00 -30.00   52
 13  \w    148.00 177.00   0.50    3.88    --  111.00  38.00 -60.00   58
 14  \w     61.00 109.00   0.50    3.88    --  111.00-111.00  30.00   96
 15  \w     80.00 110.00   0.50    3.88    --  111.00 -38.00 -60.00   60
 16  \w    141.00 175.00   0.50    3.88    --  111.00  38.00  30.00   68
 17  \w     45.00  84.00   0.50    3.88    --  111.00 -38.00 120.00   78
 18  \w     83.00 144.00   0.50    3.88    --  111.00 178.00-150.00  122
 19  \w     45.00  73.00   0.50    3.88    --  111.00 -38.00 -60.00   56
;
_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      0.0354436000
_diffrn_orient_matrix_UB_12      -0.1251690000
_diffrn_orient_matrix_UB_13      -0.0398717000
_diffrn_orient_matrix_UB_21      -0.1040046000
_diffrn_orient_matrix_UB_22      -0.0230214000
_diffrn_orient_matrix_UB_23      -0.0431749000
_diffrn_orient_matrix_UB_31      0.0325164000
_diffrn_orient_matrix_UB_32      0.0630379000
_diffrn_orient_matrix_UB_33      -0.0951055000
_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  0.0440
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10677
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.227
_diffrn_reflns_theta_min         5.191
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.293
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.467
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.88a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_description       needle
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2268
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0594P)^2^+1.7160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2153
_reflns_number_total             2268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra03587b2.cif
_cod_data_source_block           1_K[Mn(tfac)3]
_cod_database_code               7250837
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C15 H12 F9 O6 Mn'
_chemical_oxdiff_usercomment     'Yellow plates that are fibre bundles.'
_shelx_estimated_absorpt_t_max   0.771
_shelx_estimated_absorpt_t_min   0.218
_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. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O3) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(K1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: H10A(0.5) H10B(0.5) H10C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7)
4.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              35197
_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 1.885
_oxdiff_exptl_absorpt_empirical_full_min 0.751