A one-pot reduction route to bimetallic manganese 1,8-naphthyridine complexes.
Stevens, Michael A.; Lim, Li Feng; Pham, Le Nhan; Cox, Nicholas; Coote, Michelle L.; Colebatch, Annie L.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1284–1294; doi:10.1039/d3dt03709f

data_7714688
_publ_section_title
;
 A one-pot reduction route to bimetallic manganese 1,8-naphthyridine
 complexes.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1284
_journal_page_last               1294
_journal_paper_doi               10.1039/d3dt03709f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C23 H16 Br Mn N4 O3, C4 H8 O'
_chemical_formula_sum            'C27 H24 Br Mn N4 O4'
_chemical_formula_weight         603.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-24
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-05-31 deposited with the CCDC.	2023-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                78.587(7)
_cell_angle_beta                 84.102(7)
_cell_angle_gamma                81.662(6)
_cell_formula_units_Z            2
_cell_length_a                   9.0809(7)
_cell_length_b                   11.6416(8)
_cell_length_c                   12.6776(11)
_cell_measurement_reflns_used    2429
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      69.7330
_cell_measurement_theta_min      4.8090
_cell_volume                     1296.04(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.957
_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    -65.00  31.00   1.00    7.50    --  -35.78  19.00   0.00   96
  2  \w    -78.00  -8.00   1.00    7.50    --  -35.78 125.00 -30.00   70
  3  \w    -65.00  36.00   1.00    7.50    --  -35.78  19.00 -90.00  101
  4  \w    -15.00  63.00   1.00    7.50    --   35.78 -77.00  90.00   78
  5  \w     31.00  89.00   1.00    7.50    --   35.78-125.00 -60.00   58
  6  \w     43.00 123.00   1.00   30.00    --  106.41 -61.00  90.00   80
  7  \w     36.00 125.00   1.00   30.00    --  106.41 -30.00-180.00   89
  8  \w     87.00 157.00   1.00   30.00    --  106.41  30.00-180.00   70
  9  \w    126.00 173.00   1.00   30.00    --  106.41  61.00 120.00   47
 10  \w     91.00 122.00   1.00   30.00    --  106.41  61.00 120.00   31
 11  \w     90.00 170.00   1.00   30.00    --  106.41  61.00-150.00   80
 12  \w     65.00 123.00   1.00   30.00    --  106.41 178.00 120.00   58
 13  \w     44.00 109.00   1.00   30.00    --  106.41-111.00-150.00   65
 14  \w     39.00  66.00   1.00   30.00    --  106.41-111.00   0.00   27
 15  \w     39.00 109.00   1.00   30.00    --  106.41-111.00  90.00   70
 16  \w     40.00 121.00   1.00   30.00    --  106.41 -77.00-150.00   81
 17  \w     67.00 109.00   1.00   30.00    --  106.41-111.00   0.00   42
 18  \w    113.00 171.00   1.00   30.00    --  106.41  77.00-120.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0820495000
_diffrn_orient_matrix_UB_12      -0.0437615000
_diffrn_orient_matrix_UB_13      -0.0819704000
_diffrn_orient_matrix_UB_21      0.1446884000
_diffrn_orient_matrix_UB_22      -0.0066777000
_diffrn_orient_matrix_UB_23      -0.0747159000
_diffrn_orient_matrix_UB_31      0.0436401000
_diffrn_orient_matrix_UB_32      -0.1287191000
_diffrn_orient_matrix_UB_33      0.0561880000
_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  0.0425
_diffrn_reflns_av_unetI/netI     0.0826
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7410
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.529
_diffrn_reflns_theta_min         3.567
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.289
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.96a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_description       block
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.354
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         4839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0683
_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^)+(0.0989P)^2^+1.3827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1744
_refine_ls_wR_factor_ref         0.2031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3136
_reflns_number_total             4839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03709f2.cif
_cod_data_source_block           MeL-Mn(CO)5Br
_cod_depositor_comments
'Adding full bibliography for 7714688--7714690.cif.'
_cod_original_cell_volume        1296.05(18)
_cod_database_code               7714688
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.633
_shelx_estimated_absorpt_t_min   0.263
_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.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C23(H23A,H23B), C25(H25A,H25B), C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C15(H15), C4(H4), C3(H3), C11(H11), C16(H16), C9(H9),
 C10(H10), C17(H17)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              63315
_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 1.786
_oxdiff_exptl_absorpt_empirical_full_min 0.587