A direct comparison of lithium tetra(<i>n</i>-butyl) manganate(II) and magnesiate: structural insights and catalytic hydroamination of styrenes.
Jones, Rebecca S.; Krämer, Tobias; Nichol, Gary S.; Mahon, Mary F.; Kragskow, Jon G. C.; Uzelac, Marina; Chemical communications (Cambridge, England) 61 (2025) 15834–15837; doi:10.1039/d5cc04144a

data_1575609
_publ_section_title
;
 A direct comparison of lithium tetra(<i>n</i>-butyl) manganate(II) and
 magnesiate: structural insights and catalytic hydroamination of styrenes.
;
_journal_issue                   81
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              15834
_journal_page_last               15837
_journal_paper_doi               10.1039/d5cc04144a
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C28 H68 Li2 Mn N4'
_chemical_formula_sum            'C28 H68 Li2 Mn N4'
_chemical_formula_weight         529.68
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-22
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2025-07-21 deposited with the CCDC.	2025-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.4300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4247(2)
_cell_length_b                   15.0569(2)
_cell_length_c                   16.6544(2)
_cell_measurement_reflns_used    22918
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.1060
_cell_measurement_theta_min      4.5630
_cell_volume                     3532.40(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (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 n/a (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_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    -66.00 -22.00   1.00    1.00    --    0.00 -57.00  60.00   44
  2  \w    -27.00  11.00   1.00    1.00    --    0.00  77.00-150.00   38
  3  \w     13.00  40.00   1.00    1.00    --    0.00  77.00-150.00   27
  4  \w    -18.00  17.00   1.00    1.00    --    0.00 -57.00  60.00   35
  5  \w     17.00  42.00   1.00    1.00    --    0.00  77.00-120.00   25
  6  \w   -123.00 -37.00   1.00    4.00    --  -55.50 -37.00  90.00   86
  7  \w    -76.00 -43.00   1.00    4.00    --  -55.50  19.00 -90.00   33
  8  \w   -125.00 -78.00   1.00    4.00    --  -55.50-125.00 -90.00   47
  9  \w   -113.00 -81.00   1.00    4.00    --  -55.50-125.00-150.00   32
 10  \w    -79.00 -47.00   1.00    4.00    --  -55.50 125.00-180.00   32
 11  \w   -123.00 -98.00   1.00    4.00    --  -55.50-125.00  30.00   25
 12  \w    -72.00  13.00   1.00    4.00    --  -55.50  37.00 -90.00   85
 13  \w   -117.00 -88.00   1.00    4.00    --  -55.50-125.00 150.00   29
 14  \w    -80.00 -39.00   1.00    4.00    --  -55.50 125.00  60.00   41
 15  \w     20.00  89.00   1.00    4.00    --   55.50 -99.00 -30.00   69
 16  \w     51.00  86.00   1.00   15.00    --  111.00 -91.00  30.00   35
 17  \w     82.00 108.00   1.00   15.00    --  111.00-111.00-150.00   26
 18  \w     87.00 125.00   1.00   15.00    --  111.00 -77.00  60.00   38
 19  \w     42.00  97.00   1.00   15.00    --  111.00-111.00 -30.00   55
 20  \w     49.00  75.00   1.00   15.00    --  111.00 -91.00  60.00   26
 21  \w     54.00 129.00   1.00   15.00    --  111.00 -37.00 -90.00   75
 22  \w     43.00  68.00   1.00   15.00    --  111.00 -37.00-180.00   25
 23  \w     93.00 120.00   1.00   15.00    --  111.00  25.00  60.00   27
 24  \w     49.00  99.00   1.00   15.00    --  111.00-111.00 120.00   50
 25  \w    102.00 144.00   1.00   15.00    --  111.00 178.00 -90.00   42
 26  \w     48.00  74.00   1.00   15.00    --  111.00 -77.00  60.00   26
 27  \w     74.00 107.00   1.00   15.00    --  111.00-111.00   0.00   33
 28  \w     41.00  98.00   1.00   15.00    --  111.00 -25.00  60.00   57
 29  \w    109.00 135.00   1.00   15.00    --  111.00 111.00 -30.00   26
 30  \w     45.00 104.00   1.00   15.00    --  111.00 -63.00 150.00   59
 31  \w     43.00 109.00   1.00   15.00    --  111.00-111.00  30.00   66
 32  \w     96.00 148.00   1.00   15.00    --  111.00  50.00-150.00   52
 33  \w     96.00 121.00   1.00   15.00    --  111.00  37.00-120.00   25
 34  \w    135.00 161.00   1.00   15.00    --  111.00  50.00-120.00   26
 35  \w    109.00 135.00   1.00   15.00    --  111.00  25.00 -60.00   26
 36  \w     49.00  86.00   1.00   15.00    --  111.00 -91.00-120.00   37
 37  \w     80.00 105.00   1.00   15.00    --  111.00-111.00-180.00   25
 38  \w     56.00 109.00   1.00   15.00    --  111.00-111.00-120.00   53
 39  \w     47.00  92.00   1.00   15.00    --  111.00 -91.00 -60.00   45
 40  \w    101.00 126.00   1.00   15.00    --  111.00  50.00-120.00   25
 41  \w    115.00 145.00   1.00   15.00    --  111.00  77.00  30.00   30
 42  \w     84.00 109.00   1.00   15.00    --  111.00-111.00  60.00   25
 43  \w     77.00 103.00   1.00   15.00    --  111.00 -63.00  60.00   26
 44  \w     53.00  96.00   1.00   15.00    --  111.00 -77.00-120.00   43
 45  \w     84.00 119.00   1.00   15.00    --  111.00 -50.00-120.00   35
 46  \w     82.00 126.00   1.00   15.00    --  111.00 -50.00  30.00   44
 47  \w    104.00 159.00   1.00   15.00    --  111.00  37.00 -90.00   55
 48  \w     65.00  91.00   1.00   15.00    --  111.00 -63.00 120.00   26
 49  \w     84.00 109.00   1.00   15.00    --  111.00-111.00 -60.00   25
 50  \w     84.00 109.00   1.00   15.00    --  111.00-111.00 150.00   25
 51  \w    145.00 173.00   1.00   15.00    --  111.00  25.00   0.00   28
 52  \w     93.00 141.00   1.00   15.00    --  111.00  37.00 -60.00   48
 53  \w     92.00 129.00   1.00   15.00    --  111.00  25.00 120.00   37
 54  \w    138.00 171.00   1.00   15.00    --  111.00  25.00 120.00   33
 55  \w     90.00 126.00   1.00   15.00    --  111.00  25.00   0.00   36
 56  \w    104.00 130.00   1.00   15.00    --  111.00  63.00 150.00   26
 57  \w     81.00 109.00   1.00   15.00    --  111.00-111.00  90.00   28
 58  \w    124.00 150.00   1.00   15.00    --  111.00 111.00 -90.00   26
 59  \w     49.00  78.00   1.00   15.00    --  111.00 -50.00-150.00   29
 60  \w     94.00 128.00   1.00   15.00    --  111.00  50.00-180.00   34
 61  \w     64.00 102.00   1.00   15.00    --  111.00 178.00  60.00   38
 62  \w     76.00 102.00   1.00   15.00    --  111.00 178.00 120.00   26
 63  \w     63.00  89.00   1.00   15.00    --  111.00 -91.00 -30.00   26
 64  \w     80.00 130.00   1.00   15.00    --  111.00 -37.00-180.00   50
 65  \w     99.00 125.00   1.00   15.00    --  111.00 -63.00-150.00   26
 66  \w     76.00 119.00   1.00   15.00    --  111.00 -63.00 -60.00   43
 67  \w     43.00 113.00   1.00   15.00    --  111.00 -37.00   0.00   70
 68  \w    109.00 141.00   1.00   15.00    --  111.00  77.00 -30.00   32
;
_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      0.0687569000
_diffrn_orient_matrix_UB_12      0.0685520000
_diffrn_orient_matrix_UB_13      -0.0237379000
_diffrn_orient_matrix_UB_21      -0.0130511000
_diffrn_orient_matrix_UB_22      -0.0428443000
_diffrn_orient_matrix_UB_23      -0.0856846000
_diffrn_orient_matrix_UB_31      -0.0840489000
_diffrn_orient_matrix_UB_32      0.0627335000
_diffrn_orient_matrix_UB_33      -0.0326020000
_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  0.0306
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42840
_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         73.340
_diffrn_reflns_theta_min         3.682
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.155
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    0.996
_exptl_crystal_description       block
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         7083
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+0.8780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6753
_reflns_number_total             7083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04144a2.cif
_cod_data_source_block           s23mu05
_cod_depositor_comments
'Adding full bibliography for 1575607--1575611.cif.'
_cod_database_code               1575609
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Mn1 Li2 N4 C28 H68'
_shelx_estimated_absorpt_t_max   0.723
_shelx_estimated_absorpt_t_min   0.441
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13-H13b = C13-H13a = C1-H1b = C1-H1a
 0.98 with sigma of 0.005
 C9-H9a = C9-H9b = C5-H5a = C5-H5b
 0.98 with sigma of 0.005
3.a Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C3(H3a,H3b), C6(H6a,H6b), C7(H7a,H7b), C10(H10a,H10b), C11(H11a,
 H11b), C14(H14a,H14b), C15(H15a,H15b), C17(H17a,H17b), C18(H18a,H18b),
 C23(H23a,H23b), C24(H24a,H24b)
3.b Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C8(H8a,H8b,H8c), C12(H12a,H12b,H12c), C16(H16a,H16b,H16c),
 C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C21(H21a,H21b,H21c), C22(H22a,H22b,
 H22c), C25(H25a,H25b,H25c), C26(H26a,H26b,H26c), C27(H27a,H27b,H27c), C28(H28a,
 H28b,H28c)
;
_shelx_res_checksum              52057
_shelx_hkl_checksum              30682
_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 1.710
_oxdiff_exptl_absorpt_empirical_full_min 0.643