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_7250838
_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         'C12 H7 F12 Mn N O5'
_chemical_formula_sum            'C12 H7 F12 Mn N O5'
_chemical_formula_weight         528.13
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-05-07
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-05-20 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                   9.1029(3)
_cell_length_b                   21.7344(6)
_cell_length_c                   9.0051(3)
_cell_measurement_reflns_used    4080
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      74.0410
_cell_measurement_theta_min      4.0340
_cell_volume                     1781.62(10)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.941
_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    2.20    --  -38.50 -38.00  90.00  140
  2  \w   -108.00 -33.00   0.50    2.20    --  -38.50 -19.00   0.00  150
  3  \w   -108.00 -33.00   0.50    2.20    --  -38.50 -19.00 -90.00  150
  4  \w    104.00 166.00   0.50    8.79    --  100.13 111.00   0.00  124
  5  \w    104.00 166.00   0.50    8.79    --  100.13 111.00-120.00  124
  6  \w    104.00 166.00   0.50    8.79    --  100.13 111.00 150.00  124
  7  \w     38.00 113.00   0.50    8.79    --  100.13 -61.00   0.00  150
  8  \w    104.00 166.00   0.50    8.79    --  100.13 111.00  30.00  124
  9  \w     92.00 169.00   0.50    8.79    --  100.13  15.00 150.00  154
 10  \w    104.00 166.00   0.50    8.79    --  100.13 111.00  90.00  124
 11  \w    104.00 166.00   0.50    8.79    --  100.13 111.00   0.00  124
 12  \w   -105.00 -35.00   0.50    2.20    --  -38.50 -38.00-150.00  140
 13  \w   -105.00 -35.00   0.50    2.20    --  -38.50 -38.00 150.00  140
 14  \w     34.00 109.00   0.50    2.20    --   45.81  57.00  30.00  150
 15  \w     96.00 121.00   0.50    8.79    --  100.13  45.00 -30.00   50
;
_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      -0.0243029000
_diffrn_orient_matrix_UB_12      0.0698945000
_diffrn_orient_matrix_UB_13      0.0125907000
_diffrn_orient_matrix_UB_21      0.0886306000
_diffrn_orient_matrix_UB_22      0.0009768000
_diffrn_orient_matrix_UB_23      0.1460726000
_diffrn_orient_matrix_UB_31      0.1422775000
_diffrn_orient_matrix_UB_32      0.0113933000
_diffrn_orient_matrix_UB_33      -0.0885313000
_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  0.0406
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7617
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.916
_diffrn_reflns_theta_min         4.068
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.488
_exptl_absorpt_correction_T_max  0.618
_exptl_absorpt_correction_T_min  0.381
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_description       block
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.157
_refine_diff_density_max         1.134
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1770
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0766
_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^)+(0.0372P)^2^+21.6976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1783
_refine_ls_wR_factor_ref         0.1820
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1539
_reflns_number_total             1770
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra03587b2.cif
_cod_data_source_block           8-[Mn(hfac)2NCCH3(OH2)
_cod_database_code               7250838
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C12H7F12MnNO5
_chemical_oxdiff_usercomment
'Clear light yellow block from Sample Tube 10 - Ibrahim'
_shelx_estimated_absorpt_t_max   0.386
_shelx_estimated_absorpt_t_min   0.317
_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) groups
2. Restrained distances
 O3-H3
 0.84 with sigma of 0.02
3. Others
 Fixed Sof: H7A(0.5) H7B(0.5) H7C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2)
4.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              43212
_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 1.477
_oxdiff_exptl_absorpt_empirical_full_min 0.705