Discovery of antibacterial manganese(i) tricarbonyl complexes through combinatorial chemistry.
Scaccaglia, Mirco; Birbaumer, Michael P.; Pinelli, Silvana; Pelosi, Giorgio; Frei, Angelo; Chemical science 15 (2024) 3907–3919; doi:10.1039/d3sc05326a

data_1570994
_publ_section_title
;
 Discovery of antibacterial manganese(i) tricarbonyl complexes through
 combinatorial chemistry.
;
_journal_issue                   11
_journal_name_full               'Chemical science'
_journal_page_first              3907
_journal_page_last               3919
_journal_paper_doi               10.1039/d3sc05326a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C23 H15 Br2 F Mn N4 O3, C F3 O3 S, C4 H8 O'
_chemical_formula_sum            'C28 H23 Br2 F4 Mn N4 O7 S'
_chemical_formula_weight         850.322
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-02T08:01:04-00:00
_audit_update_record
;
2023-07-07 deposited with the CCDC.	2024-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                86.216(2)
_cell_angle_beta                 86.692(2)
_cell_angle_gamma                77.039(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6506(3)
_cell_length_b                   13.0241(4)
_cell_length_c                   13.9603(4)
_cell_measurement_reflns_used    34343
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      29.06
_cell_measurement_theta_min      2.228
_cell_volume                     1704.58(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9993
_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    -24.00  94.00   0.50    5.50    --   13.07  25.00 119.00  236
  2  \w    -68.00  32.00   0.50    5.50    --   13.07 -25.00 -44.00  200
  3  \w    -29.00  68.00   0.50    5.50    --  -13.54  25.00 119.00  194
  4  \w    -95.00  24.00   0.50    5.50    --  -13.54 -25.00 -44.00  238
  5  \w     -8.00  90.00   0.50    5.50    --   13.07  57.00-120.00  196
  6  \w    -16.00  83.00   0.50    5.50    --   13.07  77.00 -30.00  198
  7  \w     -7.00  94.00   0.50    5.50    --   13.07  38.00-180.00  202
  8  \w    -19.00  29.00   0.50    5.50    --  -13.54 -99.00 -60.00   96
  9  \w    -78.00 -20.00   0.50    5.50    --  -13.54 136.00  63.32  116
 10  \w    -80.00 -21.00   0.50    5.50    --  -13.54 139.00 -44.52  118
 11  \w    -80.00 -21.00   0.50    5.50    --  -13.54 139.00-173.32  118
 12  \w    -83.00 -24.00   0.50    5.50    --  -13.54 144.00-104.62  118
 13  \w    -84.00 -25.00   0.50    5.50    --  -13.54 146.00  16.61  118
 14  \w    -87.00 -42.00   0.50    5.50    --  -13.54-178.00  30.00   90
 15  \w    -78.00 -20.00   0.50    5.50    --  -13.54 136.00 107.61  116
 16  \w    -19.00  29.00   0.50    5.50    --  -13.54 -99.00-120.00   96
 17  \w    -74.00 -17.00   0.50    5.50    --  -13.54 130.00  47.80  114
 18  \w    -75.00 -18.00   0.50    5.50    --  -13.54 132.00 158.48  114
 19  \w    -74.00 -17.00   0.50    5.50    --  -13.54 131.00-139.04  114
 20  \w    -74.00 -17.00   0.50    5.50    --  -13.54 130.00 140.22  114
 21  \w    -62.00  88.00   0.50    5.50    --   13.07   0.00-180.00  300
 22  \w    -62.00 -31.00   0.50    5.50    --   13.07   0.00-150.00   62
 23  \w    -18.00  54.00   0.50    5.50    --   13.07 -99.00 -30.00  144
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0639201
_diffrn_orient_matrix_UB_12      -0.0360006
_diffrn_orient_matrix_UB_13      -0.0132479
_diffrn_orient_matrix_UB_21      0.0339889
_diffrn_orient_matrix_UB_22      0.0426711
_diffrn_orient_matrix_UB_23      -0.0103803
_diffrn_orient_matrix_UB_31      0.021406
_diffrn_orient_matrix_UB_32      -0.0039396
_diffrn_orient_matrix_UB_33      0.0481099
_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  0.0768
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.9992
_diffrn_reflns_Laue_measured_fraction_max 0.9993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            102681
_diffrn_reflns_point_group_measured_fraction_full 0.9992
_diffrn_reflns_point_group_measured_fraction_max 0.9993
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.11
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.856
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.575
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.42.94a (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            red
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       needle
_exptl_crystal_F_000             842.00
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.765
_refine_diff_density_min         -0.8249
_refine_diff_density_rms         0.1247
_refine_ls_goodness_of_fit_ref   1.0344
_refine_ls_matrix_type           full
_refine_ls_number_constraints    40
_refine_ls_number_parameters     500
_refine_ls_number_reflns         6959
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.0306
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          -0.0005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+2.9335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.139
_reflns_Friedel_coverage         0
_reflns_number_gt                5753
_reflns_number_total             6959
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc05326a2.cif
_cod_data_source_block           23AF001_MnG9MeBeim
_cod_depositor_comments
'Adding full bibliography for 1570994--1570996.cif.'
_cod_original_cell_volume        1704.58(8)
_cod_original_formula_sum        'C28 H23 Br2 F4 Mn1 N4 O7 S1'
_cod_database_code               1570994
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 5.874
_oxdiff_exptl_absorpt_empirical_full_min 0.450
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
3. Rigid bond restraints
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4. Uiso/Uaniso restraints and constraints
: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(O5a) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(S1)
\\sim Ueq, Uanis(F4a) \\sim Ueq, Uanis(F6a) \\sim Ueq, Uanis(O3a) \\sim Ueq,
Uanis(O8) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.004
: with sigma of 0.01 and sigma for terminal atoms of 0.005
5. Rigid body (RIGU) restrains
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Uiso: F4(0.225549) C1a(0.054809) F5(0.050411) F2(0.053294) S6(0.153757)
 O4(0.034088) O6(0.12345) O9(0.073258)
7.a Secondary CH2 refined with riding coordinates:
 C28(H28a,H28b), C25(H25a,H25b), C27(H27a,H27b), C26(H26a,H26b)
7.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C22(H22), C23(H23), C19(H19), C20(H20), C1(H1), C4(H4), C24(H24),
 C5(H5), C7(H7), C14(H14), C13(H13)
7.c Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2