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_7714689
_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         'C26 H16 Mn2 N4 O6'
_chemical_formula_sum            'C26 H16 Mn2 N4 O6'
_chemical_formula_weight         590.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-14
_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                90
_cell_angle_beta                 96.032(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9780(4)
_cell_length_b                   10.8779(2)
_cell_length_c                   13.9502(3)
_cell_measurement_reflns_used    3427
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6590
_cell_measurement_theta_min      4.9050
_cell_volume                     2411.22(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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 2014/5 (Sheldrick, 2014)'
_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 1.000
_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    -14.00  26.00   1.00    5.00    --  -36.95  57.00 -90.00   40
  2  \w     31.00  67.00   1.00    5.00    --   36.95-125.00 -30.00   36
  3  \w     28.00  55.00   1.00    5.00    --   36.95-125.00 -60.00   27
  4  \w    -24.00  45.00   1.00    5.00    --   36.95 -57.00-150.00   69
  5  \w     22.00  63.00   1.00    5.00    --   36.95 -77.00  90.00   41
  6  \w     10.00  76.00   1.00    5.00    --   36.95 -99.00 -30.00   66
  7  \w      7.00  72.00   1.00    5.00    --   36.95 -99.00  90.00   65
  8  \w    -21.00  19.00   1.00    5.00    --   36.95 -77.00  90.00   40
  9  \w     32.00  85.00   1.00    5.00    --   36.95-125.00-120.00   53
 10  \w     43.00 104.00   1.00   20.00    --  111.00 -92.00-120.00   61
 11  \w     91.00 118.00   1.00   20.00    --  111.00 -12.00  60.00   27
 12  \w    106.00 132.00   1.00   20.00    --  111.00 -25.00 -90.00   26
 13  \w     46.00  73.00   1.00   20.00    --  111.00-111.00-180.00   27
 14  \w    105.00 136.00   1.00   20.00    --  111.00  38.00 -90.00   31
 15  \w     76.00 103.00   1.00   20.00    --  111.00-111.00  60.00   27
 16  \w     43.00 101.00   1.00   20.00    --  111.00 -92.00 -30.00   58
 17  \w    109.00 134.00   1.00   20.00    --  111.00  77.00  60.00   25
 18  \w     43.00 128.00   1.00   20.00    --  111.00 -38.00 -30.00   85
 19  \w     63.00 110.00   1.00   20.00    --  111.00 178.00  60.00   47
 20  \w     46.00 100.00   1.00   20.00    --  111.00 -25.00  90.00   54
 21  \w     44.00 110.00   1.00   20.00    --  111.00 -64.00   0.00   66
 22  \w     69.00 100.00   1.00   20.00    --  111.00 -25.00 -90.00   31
 23  \w     82.00 110.00   1.00   20.00    --  111.00 -59.00  92.00   28
 24  \w     50.00  82.00   1.00   20.00    --  111.00 -12.00  60.00   32
 25  \w     50.00  76.00   1.00   20.00    --  111.00 -59.00  92.00   26
 26  \w     46.00 134.00   1.00   20.00    --  111.00 -77.00  90.00   88
 27  \w     52.00  90.00   1.00   20.00    --  111.00 -92.00  60.00   38
 28  \w     92.00 141.00   1.00   20.00    --  111.00  64.00-150.00   49
 29  \w     73.00 145.00   1.00   20.00    --  111.00  12.00  60.00   72
;
_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      -0.0264204000
_diffrn_orient_matrix_UB_12      -0.0943274000
_diffrn_orient_matrix_UB_13      0.0735401000
_diffrn_orient_matrix_UB_21      -0.0931586000
_diffrn_orient_matrix_UB_22      0.0306344000
_diffrn_orient_matrix_UB_23      -0.0299449000
_diffrn_orient_matrix_UB_31      -0.0037326000
_diffrn_orient_matrix_UB_32      -0.1012721000
_diffrn_orient_matrix_UB_33      -0.0775834000
_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  0.0206
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7442
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.646
_diffrn_reflns_theta_min         4.927
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.969
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
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    1.626
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0569P)^2^+0.6466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2173
_reflns_number_total             2424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03709f2.cif
_cod_data_source_block           MeLMn2CO6
_cod_depositor_comments
'Adding full bibliography for 7714688--7714690.cif.'
_cod_database_code               7714689
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.716
_shelx_estimated_absorpt_t_min   0.346
_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:
 C8(H8), C4(H4), C3(H3), C9(H9), C10(H10)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              36737
_olex2_date_sample_data_collection 2021-10-01
_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 1.499
_oxdiff_exptl_absorpt_empirical_full_min 0.842