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_1570995
_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_absolute_configuration ad
_chemical_formula_moiety         'C32 H30 Mn N4 O7, C F3 O3 S'
_chemical_formula_sum            'C33 H30 F3 Mn N4 O10 S'
_chemical_formula_weight         786.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-07 deposited with the CCDC.	2024-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 123.873(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9009(7)
_cell_length_b                   15.2585(3)
_cell_length_c                   13.0302(4)
_cell_measurement_reflns_used    18443
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      77.5760
_cell_measurement_theta_min      3.7680
_cell_volume                     3450.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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     38.75 158.75   0.80   10.00    --   67.99  59.25  69.92  150
  2  \w    151.31 275.31   0.80   16.00    -- -112.99 -59.25 -19.92  155
  3  \w    151.31 275.31   0.80   16.00    -- -112.99 -59.25-147.92  155
  4  \w    245.71 320.11   0.80   16.00    -- -112.99  94.56-142.84   93
  5  \f   -339.92  20.08   0.80   14.00 -68.94 -97.99 -59.25    --   450
  6  \w     -7.26  88.74   0.80    8.00    --   42.50 -89.85  72.66  120
  7  \w    151.31 275.31   0.80   16.00    -- -112.99 -59.25  52.08  155
  8  \w    151.31 275.31   0.80   16.00    -- -112.99 -59.25 -83.92  155
  9  \w    151.31 275.31   0.80   16.00    -- -112.99 -59.25 148.08  155
 10  \w     -1.74 118.26   0.80    8.00    --   27.50  59.25 -20.08  150
 11  \w     13.26 133.26   0.80    8.00    --   42.50  59.25-140.08  150
 12  \w    200.08 326.48   0.80   16.00    -- -112.99  89.85 127.34  158
 13  \w    166.31 290.31   0.80   14.00    --  -97.99 -59.25 110.08  155
 14  \w     -1.74 118.26   0.80    8.00    --   27.50  59.25 159.92  150
 15  \w    200.08 326.48   0.80   16.00    -- -112.99  89.85  31.33  158
 16  \w     38.75 158.75   0.80   10.00    --   67.99  59.25 -20.08  150
 17  \w    151.31 275.31   0.80   16.00    -- -112.99 -59.25-179.92  155
 18  \w    151.31 275.31   0.80   16.00    -- -112.99 -59.25  84.08  155
 19  \w     -7.26  88.74   0.80    8.00    --   42.50 -89.85  32.66  120
 20  \w    151.31 275.31   0.80   16.00    -- -112.99 -59.25  20.08  155
 21  \w    151.31 275.31   0.80   16.00    -- -112.99 -59.25 -51.92  155
 22  \f   -339.92  20.08   0.80   12.00 -53.94 -82.99 -59.25    --   450
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0704256234
_diffrn_orient_matrix_UB_12      -0.0574788528
_diffrn_orient_matrix_UB_13      -0.0880703418
_diffrn_orient_matrix_UB_21      0.0393545091
_diffrn_orient_matrix_UB_22      -0.0788272457
_diffrn_orient_matrix_UB_23      0.0870690290
_diffrn_orient_matrix_UB_31      -0.0369878611
_diffrn_orient_matrix_UB_32      0.0257555859
_diffrn_orient_matrix_UB_33      0.0702826401
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            33427
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.058
_diffrn_reflns_theta_min         3.858
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.380
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellowish
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       prism
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 2761 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         6449
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0323P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0703
_reflns_Friedel_coverage         0.964
_reflns_Friedel_fraction_full    0.972
_reflns_Friedel_fraction_max     0.965
_reflns_number_gt                6164
_reflns_number_total             6449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05326a2.cif
_cod_data_source_block           cu_c1_dmap_rd
_cod_depositor_comments
'Adding full bibliography for 1570994--1570996.cif.'
_cod_original_cell_volume        3450.2(2)
_cod_database_code               1570995
_shelx_shelxl_version_number     2019/1
_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:
 C00H(H00H), C00J(H00J), C00K(H00K), C00M(H00M), C00R(H00R), C00V(H00V),
 C00X(H00X), C00Z(H00Z), C011(H011), C013(H013), C014(H014), C017(H017),
 C018(H018), C019(H019), C01B(H01D)
2.b Idealised Me refined as rotating group:
 C01A(H01A,H01B,H01C), C01C(H01E,H01F,H01G), C01D(H01H,H01I,H01J), C01E(H01K,
 H01L,H01M), C01G(H01N,H01O,H01P)
;
_shelx_res_checksum              83288
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.606
_oxdiff_exptl_absorpt_empirical_full_min 0.719