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_7714690
_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         'C40 H32 Cl4 Mn2 N8, 2(C H2 Cl2)'
_chemical_formula_sum            'C42 H36 Cl8 Mn2 N8'
_chemical_formula_weight         1046.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-31
_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                 91.1170(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.89580(10)
_cell_length_b                   17.77790(10)
_cell_length_c                   25.6158(2)
_cell_measurement_reflns_used    32086
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      77.8840
_cell_measurement_theta_min      4.2340
_cell_volume                     4505.64(6)
_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_temperature      150.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_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     -8.00  29.00   0.50    0.68    --  -46.45  19.00 120.00   74
  2  \w     -6.00  30.00   0.50    0.68    --  -46.45  19.00 -90.00   72
  3  \w     -7.00  25.00   0.50    0.68    --  -46.45  19.00 150.00   64
  4  \w     -5.00  27.00   0.50    0.68    --  -46.45  19.00-120.00   64
  5  \w    -77.00  26.00   0.50    0.68    --  -46.45   0.00  90.00  206
  6  \w    -42.00 -16.00   0.50    0.68    --  -46.45  57.00   0.00   52
  7  \w    -22.00  17.00   0.50    0.68    --  -46.45  38.00-180.00   78
  8  \w     -7.00  26.00   0.50    0.68    --  -46.45  57.00   0.00   66
  9  \w    -22.00  18.00   0.50    0.68    --  -46.45  38.00 -60.00   80
 10  \w   -113.00 -87.00   0.50    0.68    --  -46.45   0.00  90.00   52
 11  \w     57.00  86.00   0.50    0.68    --   46.45-125.00   0.00   58
 12  \w     36.00  91.00   0.50    0.68    --   46.45-125.00  90.00  110
 13  \w     49.00  85.00   0.50    0.68    --   46.45-125.00-150.00   72
 14  \w     40.00  66.00   0.50    2.73    --  107.75 -45.00 -90.00   52
 15  \w     41.00  72.00   0.50    2.73    --  107.75 -45.00  60.00   62
 16  \w     32.00  58.00   0.50    2.73    --  107.75 -30.00  60.00   52
 17  \w     83.00 108.00   0.50    2.73    --  107.75-111.00 152.55   50
 18  \w     33.00  59.00   0.50    2.73    --  107.75 -30.00 120.00   52
 19  \w     32.00  59.00   0.50    2.73    --  107.75 -30.00   0.00   54
 20  \w     42.00 108.00   0.50    2.73    --  107.75-104.00 -88.03  132
 21  \w     56.00  82.00   0.50    2.73    --  107.75 -61.00 120.00   52
 22  \w     38.00  78.00   0.50    2.73    --  107.75 -61.00-180.00   80
 23  \w     41.00  66.00   0.50    2.73    --  107.75 -95.00 -60.00   50
 24  \w     38.00  78.00   0.50    2.73    --  107.75-111.00 152.55   80
 25  \w    103.00 134.00   0.50    2.73    --  107.75 125.00-150.00   62
 26  \w     35.00  60.00   0.50    2.73    --  107.75 -45.00-180.00   50
 27  \w     35.00  73.00   0.50    2.73    --  107.75 -45.00 -60.00   76
 28  \w     94.00 137.00   0.50    2.73    --  107.75  45.00  30.00   86
 29  \w    145.00 176.00   0.50    2.73    --  107.75  45.00  30.00   62
 30  \w     42.00  76.00   0.50    2.73    --  107.75 -95.00 -30.00   68
 31  \w     32.00  58.00   0.50    2.73    --  107.75 -30.00 150.00   52
 32  \w    107.00 160.00   0.50    2.73    --  107.75  45.00 150.00  106
 33  \w     75.00 106.00   0.50    2.73    --  107.75 -95.00   0.00   62
 34  \w     37.00  79.00   0.50    2.73    --  107.75 -77.00 -90.00   84
 35  \w     75.00 106.00   0.50    2.73    --  107.75 -95.00  30.00   62
 36  \w    100.00 174.00   0.50    2.73    --  107.75  15.00 -60.00  148
 37  \w     61.00  86.00   0.50    2.73    --  107.75 -61.00  90.00   50
 38  \w     81.00 106.00   0.50    2.73    --  107.75 -95.00  90.00   50
 39  \w     80.00 107.00   0.50    2.73    --  107.75-125.00 -90.00   54
 40  \w     41.00  68.00   0.50    2.73    --  107.75 -95.00  90.00   54
 41  \w     93.00 138.00   0.50    2.73    --  107.75  15.00  30.00   90
 42  \w    141.00 170.00   0.50    2.73    --  107.75  15.00  30.00   58
 43  \w     45.00  71.00   0.50    2.73    --  107.75 -95.00 -90.00   52
 44  \w     81.00 106.00   0.50    2.73    --  107.75 -95.00 -90.00   50
 45  \w     75.00 104.00   0.50    2.73    --  107.75 -95.00  60.00   58
 46  \w     58.00 104.00   0.50    2.73    --  107.75 -95.00-150.00   92
 47  \w    100.00 164.00   0.50    2.73    --  107.75  15.00 -30.00  128
 48  \w     78.00 106.00   0.50    2.73    --  107.75 -95.00 -60.00   56
 49  \w    120.00 160.00   0.50    2.73    --  107.75  45.00  60.00   80
 50  \w     34.00  69.00   0.50    2.73    --  107.75 -61.00  30.00   70
 51  \w     81.00 106.00   0.50    2.73    --  107.75 -95.00 -30.00   50
 52  \w    140.00 167.00   0.50    2.73    --  107.75 125.00-150.00   54
 53  \w     33.00  58.00   0.50    2.73    --  107.75 -30.00-180.00   50
 54  \w    101.00 126.00   0.50    2.73    --  107.75-143.00-114.59   50
 55  \w     55.00  87.00   0.50    2.73    --  107.75 -61.00 -60.00   64
 56  \w     51.00 106.00   0.50    2.73    --  107.75 -95.00-180.00  110
 57  \w     37.00  86.00   0.50    2.73    --  107.75-125.00  60.00   98
 58  \w     44.00  70.00   0.50    2.73    --  107.75-143.00-114.59   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0782118000
_diffrn_orient_matrix_UB_12      0.0735505000
_diffrn_orient_matrix_UB_13      -0.0105284000
_diffrn_orient_matrix_UB_21      -0.0185259000
_diffrn_orient_matrix_UB_22      0.0105687000
_diffrn_orient_matrix_UB_23      0.0591214000
_diffrn_orient_matrix_UB_31      0.1333397000
_diffrn_orient_matrix_UB_32      0.0446113000
_diffrn_orient_matrix_UB_33      0.0034394000
_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  0.0854
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            64904
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.045
_diffrn_reflns_theta_min         3.026
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.260
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11252
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       block
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.042
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         9584
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0682
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1193P)^2^+7.3158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1882
_refine_ls_wR_factor_ref         0.1919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8822
_reflns_number_total             9584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03709f2.cif
_cod_data_source_block           (MeL-MnCl2)2
_cod_depositor_comments
'Adding full bibliography for 7714688--7714690.cif.'
_cod_database_code               7714690
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.302
_shelx_estimated_absorpt_t_min   0.127
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl6-Cl7 \\sim Cl5-Cl8
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(Cl8) = Uanis(Cl5)
Uanis(Cl7) = Uanis(Cl6) = Uanis(C43)
4. Others
 Sof(H43A)=Sof(H43B)=Sof(Cl5)=Sof(Cl8)=1-FVAR(1)
 Sof(Cl6)=Sof(Cl7)=Sof(H43C)=Sof(H43D)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C43(H43C,H43D), C44(H44A,H44B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C23(H23), C11(H11), C4(H4), C5(H5), C24(H24), C9(H9), C33(H33),
 C27(H27), C10(H10), C6(H6), C26(H26), C31(H31), C36(H36), C15(H15), C32(H32),
 C38(H38), C17(H17), C39(H39), C16(H16)
5.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C35(H35A,H35B,H35C), C41(H41A,H41B,H41C), C19(H19A,H19B,
 H19C)
;
_shelx_res_checksum              7641
_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 4.428
_oxdiff_exptl_absorpt_empirical_full_min 0.391