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_1575611
_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         'C44 H112 Li4 Mg2 N12'
_chemical_formula_sum            'C44 H112 Li4 Mg2 N12'
_chemical_formula_weight         885.83
_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             2025-07-18
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7308)
;
_audit_update_record
;
2025-07-21 deposited with the CCDC.	2025-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                103.3020(10)
_cell_angle_beta                 95.8980(10)
_cell_angle_gamma                98.2070(10)
_cell_formula_units_Z            2
_cell_length_a                   10.52080(10)
_cell_length_b                   16.6818(2)
_cell_length_c                   17.4957(2)
_cell_measurement_reflns_used    32654
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      78.8400
_cell_measurement_theta_min      4.2470
_cell_volume                     2928.16(6)
_computing_cell_refinement       'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.131a 64-bit (release 19-07-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.963
_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  58.00   0.50    2.00    --   50.88 -71.00 -91.00  144
  2  \w    -60.00  12.00   0.50    2.00    --  -52.88  71.00  39.00  144
  3  \w    -65.00 -14.00   0.50    2.00    --  -78.40  71.00  39.00  102
  4  \w   -143.00 -95.00   0.50    2.00    --  -78.40 -71.00 -91.00   96
  5  \w    117.00 169.00   0.50    2.00    --  103.80  71.00  39.00  104
  6  \w     39.00  65.00   0.50    2.00    --  103.80 -71.00 -91.00   52
  7  \w    -32.00  -2.00   0.50    2.00    --    2.00 114.00  89.38   60
  8  \w    -19.00   8.00   0.50    2.00    --    6.00  98.00-118.17   54
  9  \w     10.00  37.00   0.50    2.00    --   18.00  72.00  -7.40   54
 10  \w     16.00  42.00   0.50    2.00    --   22.00  69.00-165.11   52
 11  \w     25.00  51.00   0.50    2.00    --   30.00  66.00  37.91   52
 12  \w     25.00  51.00   0.50    2.00    --   30.00  66.00 -52.63   52
 13  \w     25.00  51.00   0.50    2.00    --   30.00  66.00-126.94   52
 14  \w     25.00  51.00   0.50    2.00    --   30.00  66.00 -99.85   52
 15  \w     25.00  51.00   0.50    2.00    --   30.00  66.00 125.97   52
 16  \w     25.00  51.00   0.50    2.00    --   30.00  66.00   1.23   52
 17  \w     25.00  51.00   0.50    2.00    --   30.00  66.00  84.60   52
 18  \w     31.00  58.00   0.50    2.00    --   34.00  62.00-169.20   54
 19  \w     33.00  59.00   0.50    2.00    --   34.00  58.00  -9.63   52
 20  \w     31.00  58.00   0.50    2.00    --   34.00  61.00 164.54   54
 21  \w     32.00  59.00   0.50    2.00    --   34.00  60.00 -66.78   54
 22  \w     31.00  58.00   0.50    2.00    --   34.00  61.00  93.77   54
 23  \w     31.00  58.00   0.50    2.00    --   34.00  62.00  19.16   54
 24  \w     31.00  58.00   0.50    2.00    --   34.00  62.00 124.58   54
 25  \w     31.00  58.00   0.50    2.00    --   34.00  62.00-141.73   54
 26  \w     46.00 116.00   0.50    2.00    --   46.00  54.00 -97.15  140
 27  \w     50.00 120.00   0.50    2.00    --   50.00  54.00 118.10  140
 28  \w     50.00 120.00   0.50    2.00    --   50.00  54.00 100.67  140
 29  \w     50.00 120.00   0.50    2.00    --   50.00  54.00  47.00  140
 30  \w     51.00 121.00   0.50    2.00    --   50.88  51.00 166.20  140
 31  \w     51.00 121.00   0.50    2.00    --   50.88  53.00  72.21  140
 32  \w     52.00 121.00   0.50    2.00    --   50.88  50.00 -24.02  138
 33  \w     51.00 121.00   0.50    2.00    --   50.88  52.00-147.16  140
 34  \w     51.00 121.00   0.50    2.00    --   50.88  52.00-175.56  140
 35  \w     51.00 121.00   0.50    2.00    --   50.88  52.00 141.51  140
 36  \w     51.00 121.00   0.50    2.00    --   50.88  52.00-116.24  140
 37  \w     51.00 121.00   0.50    2.00    --   50.88  52.00 -82.91  140
 38  \w     51.00 121.00   0.50    2.00    --   50.88  51.00 -54.29  140
 39  \w     51.00 121.00   0.50    2.00    --   50.88  52.00  11.22  140
 40  \w      8.00  89.00   0.50    2.00    --   70.00 -88.00 -61.80  162
 41  \w   -146.00 -79.00   0.50    2.00    --  -78.40 -61.00 -90.00  134
 42  \w   -146.00 -79.00   0.50    2.00    --  -78.40 -61.00  30.00  134
 43  \w    -51.00 -10.00   0.50    2.00    --  -78.40  61.00-180.00   82
 44  \w   -146.00 -79.00   0.50    2.00    --  -78.40 -61.00  60.00  134
 45  \w    -51.00 -10.00   0.50    2.00    --  -78.40  61.00  90.00   82
 46  \w   -146.00 -79.00   0.50    2.00    --  -78.40 -61.00 -30.00  134
 47  \w    -51.00 -10.00   0.50    2.00    --  -78.40  61.00   0.00   82
 48  \w   -146.00 -79.00   0.50    2.00    --  -78.40 -61.00 150.00  134
 49  \w   -149.00 -81.00   0.50    2.00    --  -78.40 -45.00  60.00  136
 50  \w   -149.00 -81.00   0.50    2.00    --  -78.40 -45.00-180.00  136
 51  \w   -104.00 -79.00   0.50    2.00    --  -78.40 -61.00-180.00   50
 52  \w   -140.00-114.00   0.50    2.00    --  -78.40 -61.00-150.00   52
 53  \w   -109.00 -79.00   0.50    2.00    --  -78.40 -61.00 -60.00   60
 54  \w    -57.00 -17.00   0.50    2.00    --  -78.40  77.00-150.00   80
 55  \w   -116.00 -84.00   0.50    2.00    --  -78.40 -45.00-120.00   64
 56  \w   -108.00 -81.00   0.50    2.00    --  -78.40 -45.00  90.00   54
 57  \w   -109.00 -79.00   0.50    2.00    --  -78.40 -61.00-150.00   60
 58  \w   -113.00 -87.00   0.50    2.00    --  -78.40 -45.00 -30.00   52
 59  \w   -107.00 -80.00   0.50    2.00    --  -78.40 -61.00 -30.00   54
 60  \w   -114.00 -83.00   0.50    2.00    --  -78.40 -45.00 -60.00   62
 61  \w   -111.00 -85.00   0.50    2.00    --  -78.40 -45.00 -90.00   52
 62  \w   -105.00 -79.00   0.50    2.00    --  -78.40 -61.00   0.00   52
 63  \w   -107.00 -79.00   0.50    2.00    --  -78.40 -61.00  90.00   56
 64  \w   -146.00-113.00   0.50    2.00    --  -78.40 -61.00  90.00   66
 65  \w   -132.00 -79.00   0.50    2.00    --  -78.40 -61.00-120.00  106
 66  \w   -109.00 -83.00   0.50    2.00    --  -78.40 -45.00 150.00   52
 67  \w   -141.00-115.00   0.50    2.00    --  -78.40 -61.00  60.00   52
 68  \w    -57.00 -17.00   0.50    2.00    --  -78.40  77.00 120.00   80
 69  \w   -113.00 -79.00   0.50    2.00    --  -78.40 -61.00 120.00   68
 70  \w   -144.00-119.00   0.50    2.00    --  -78.40 -61.00 -60.00   50
 71  \w    137.00 172.00   0.50    2.00    --  103.80  61.00  60.00   70
 72  \w    101.00 139.00   0.50    2.00    --  103.80  61.00 -90.00   76
 73  \w    147.00 172.00   0.50    2.00    --  103.80  61.00-120.00   50
 74  \w    101.00 131.00   0.50    2.00    --  103.80  61.00-120.00   60
 75  \w    102.00 128.00   0.50    2.00    --  103.80  61.00  60.00   52
 76  \w    121.00 150.00   0.50    2.00    --  103.80 125.00 120.00   58
 77  \w    144.00 170.00   0.50    2.00    --  103.80  61.00 -30.00   52
 78  \w    102.00 128.00   0.50    2.00    --  103.80  61.00 -30.00   52
 79  \w     43.00  92.00   0.50    2.00    --  103.80 -95.00 120.00   98
 80  \w    132.00 172.00   0.50    2.00    --  103.80  61.00 -60.00   80
 81  \w    101.00 126.00   0.50    2.00    --  103.80  61.00 -60.00   50
 82  \w    101.00 171.00   0.50    2.00    --  103.80  61.00 120.00  140
 83  \w    101.00 171.00   0.50    2.00    --  103.80  61.00  90.00  140
 84  \w    102.00 164.00   0.50    2.00    --  103.80  61.00  30.00  124
 85  \w    101.00 172.00   0.50    2.00    --  103.80  61.00-150.00  142
 86  \w    107.00 133.00   0.50    2.00    --  103.80  45.00 150.00   52
 87  \w     39.00 100.00   0.50    2.00    --  103.80-125.00-180.00  122
 88  \w    123.00 165.00   0.50    2.00    --  103.80 125.00   0.00   84
 89  \w    146.00 172.00   0.50    2.00    --  103.80  61.00   0.00   52
 90  \w    125.00 151.00   0.50    2.00    --  103.80 125.00-180.00   52
 91  \w    101.00 127.00   0.50    2.00    --  103.80  61.00   0.00   52
 92  \w    107.00 134.00   0.50    2.00    --  103.80  45.00  30.00   54
 93  \w    101.00 169.00   0.50    2.00    --  103.80  61.00 150.00  136
 94  \w    106.00 131.00   0.50    2.00    --  103.80  45.00 -90.00   50
 95  \w    106.00 145.00   0.50    2.00    --  103.80  45.00-180.00   78
 96  \w     41.00  92.00   0.50    2.00    --  103.80 -95.00-150.00  102
 97  \w    108.00 134.00   0.50    2.00    --  103.80  45.00 120.00   52
 98  \w     44.00  91.00   0.50    2.00    --  103.80 -95.00 -60.00   94
 99  \w    106.00 132.00   0.50    2.00    --  103.80  45.00  90.00   52
100  \w    107.00 132.00   0.50    2.00    --  103.80  45.00  60.00   50
101  \w    110.00 169.00   0.50    2.00    --  103.80  45.00   0.00  118
102  \w    107.00 165.00   0.50    2.00    --  103.80  45.00 -30.00  116
103  \w    123.00 152.00   0.50    2.00    --  103.80 125.00  90.00   58
104  \w     44.00  92.00   0.50    2.00    --  103.80 -95.00 -90.00   96
105  \w    106.00 150.00   0.50    2.00    --  103.80  45.00 -60.00   88
106  \w    109.00 168.00   0.50    2.00    --  103.80 125.00-120.00  118
107  \w    142.00 168.00   0.50    2.00    --  103.80  45.00-120.00   52
108  \w    108.00 134.00   0.50    2.00    --  103.80  45.00-120.00   52
109  \w     43.00  92.00   0.50    2.00    --  103.80 -95.00  30.00   98
110  \w    106.00 147.00   0.50    2.00    --  103.80  45.00-150.00   82
111  \w    119.00 159.00   0.50    2.00    --  103.80 125.00 150.00   80
112  \w    101.00 170.00   0.50    2.00    --  103.80  61.00-180.00  138
113  \w     43.00  92.00   0.50    2.00    --  103.80 -95.00  90.00   98
114  \w     44.00  92.00   0.50    2.00    --  103.80 -95.00  60.00   96
115  \w     46.00  93.00   0.50    2.00    --  107.75-102.00-174.58   94
116  \w     59.00  92.00   0.50    2.00    --  107.75 -98.00  84.61   66
117  \w     62.00  91.00   0.50    2.00    --  107.75 -97.00 155.82   58
118  \w     46.00  93.00   0.50    2.00    --  107.75-102.00-116.84   94
119  \w     45.00  92.00   0.50    2.00    --  107.75 -95.00 -39.46   94
120  \w     67.00  92.00   0.50    2.00    --  107.75 -89.00 -23.69   50
121  \w     68.00  93.00   0.50    2.00    --  107.75 -96.00   6.92   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0876645000
_diffrn_orient_matrix_UB_12      -0.0008535000
_diffrn_orient_matrix_UB_13      -0.0654027000
_diffrn_orient_matrix_UB_21      0.0472024000
_diffrn_orient_matrix_UB_22      0.0947661000
_diffrn_orient_matrix_UB_23      0.0325134000
_diffrn_orient_matrix_UB_31      0.1114338000
_diffrn_orient_matrix_UB_32      -0.0172648000
_diffrn_orient_matrix_UB_33      0.0549338000
_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  0.0463
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            117165
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.728
_diffrn_reflns_theta_min         2.621
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.130a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.005
_exptl_crystal_description       plank
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         20292
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0667P)^2^+0.3145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16502
_reflns_number_total             20292
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9799\% 
around [0.30 0.90 -0.30] (reciprocal) or [0.70 0.71 0.00] (direct)
;
_cod_data_source_file            d5cc04144a2.cif
_cod_data_source_block           y24mu11_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 1575607--1575611.cif.'
_cod_database_code               1575611
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Li2 Mg N8 C28 H50'
_diffrn_oxdiff_ac3_digest_hkl    41a21024062fbc69fc5758de912d0c1f801e33
_diffrn_oxdiff_digest_hkl
;
434511431de54874705f77839e18d08ecd6c07
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9108(3)
 0.0892(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N8-C27 \\sim N8-C27A
 with sigma of 0.02
 C28-C27 \\sim C28A-C27A
 with sigma of 0.02
 N8-C28 \\sim N8-C28A
 with sigma of 0.04
 C25-C26 \\sim C25-C26A
 with sigma of 0.02
4. Others
 Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C27)=Sof(H27A)=Sof(H27B)=FVAR(1)
 Sof(H25C)=Sof(H25D)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(2)
 Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C41(H41A,H41B), C7(H7A,H7B), C18(H18A,H18B), C17(H17A,H17B),
 C11(H11A,H11B), C1(H1A,H1B), C9(H9A,H9B), C33(H33A,H33B), C13(H13A,H13B),
 C31(H31A,H31B), C5(H5A,H5B), C3(H3A,H3B), C25(H25A,H25B), C25(H25C,H25D),
 C23(H23A,H23B), C15(H15A,H15B), C37(H37A,H37B), C29(H29A,H29B), C35(H35A,H35B),
  C27(H27A,H27B), C27A(H27C,H27D)
5.b Me refined with riding coordinates:
 C26(H26A,H26B,H26C), C26A(H26D,H26E,H26F)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C),
 C34(H34A,H34B,H34C), C2(H2A,H2B,H2C), C20(H20A,H20B,H20C), C6(H6A,H6B,H6C),
 C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C40(H40A,H40B,H40C), C22(H22A,H22B,
 H22C), C39(H39A,H39B,H39C), C32(H32A,H32B,H32C), C24(H24A,H24B,H24C), C38(H38A,
 H38B,H38C), C30(H30A,H30B,H30C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C),
 C21(H21A,H21B,H21C), C36(H36A,H36B,H36C), C16(H16A,H16B,H16C), C28(H28A,H28B,
 H28C), C28A(H28D,H28E,H28F)
;
_shelx_res_checksum              11776
_shelx_hkl_checksum              92258
_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 1.723
_oxdiff_exptl_absorpt_empirical_full_min 0.716
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2