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_1575610
_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 Mg N4'
_chemical_formula_sum            'C28 H68 Li2 Mg N4'
_chemical_formula_weight         499.05
_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             2024-10-31
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2025-07-21 deposited with the CCDC.	2025-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.5260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.46900(10)
_cell_length_b                   15.04860(10)
_cell_length_c                   16.64520(10)
_cell_measurement_reflns_used    37323
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      79.3600
_cell_measurement_theta_min      3.0950
_cell_volume                     3538.03(4)
_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-ac6-020 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-020 (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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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   -119.00 -58.00   0.50    1.00    --  -52.90 -38.00-150.00  122
  2  \w    -18.00   8.00   0.50    1.00    --  -52.90  77.00 -60.00   52
  3  \w    -60.00 -35.00   0.50    1.00    --  -52.90  77.00 -60.00   50
  4  \w    -26.00  10.00   0.50    1.00    --  -52.90  57.00 -60.00   72
  5  \w   -118.00 -62.00   0.50    1.00    --  -52.90 -38.00 150.00  112
  6  \w    -17.00  10.00   0.50    1.00    --  -52.90  38.00 150.00   54
  7  \w     12.00  93.00   0.50    1.00    --   74.00 -88.00  57.72  162
  8  \w    -42.00 -16.00   0.50    1.00    --  -78.39  61.00-180.00   52
  9  \w    -63.00 -29.00   0.50    1.00    --  -78.39  77.00 -90.00   68
 10  \w   -135.00 -80.00   0.50    1.00    --  -78.39 -15.00-120.00  110
 11  \w    -66.00 -41.00   0.50    1.00    --  -78.39  77.00-180.00   50
 12  \w    -51.00 -16.00   0.50    1.00    --  -78.39  61.00 120.00   70
 13  \w    -64.00 -26.00   0.50    1.00    --  -78.39  77.00   0.00   76
 14  \w    -51.00 -16.00   0.50    1.00    --  -78.39  61.00 150.00   70
 15  \w   -131.00 -84.00   0.50    1.00    --  -78.39 -15.00 -60.00   94
 16  \w   -144.00 -86.00   0.50    1.00    --  -78.39 -61.00-150.00  116
 17  \w   -135.00 -99.00   0.50    1.00    --  -78.39 -15.00  30.00   72
 18  \w    -44.00 -11.00   0.50    1.00    --  -78.39  61.00-120.00   66
 19  \w    -45.00 -16.00   0.50    1.00    --  -78.39  77.00 -60.00   58
 20  \w    103.00 135.00   0.50    2.00    --  103.79  15.00-120.00   64
 21  \w     66.00  92.00   0.50    2.00    --  103.79 -95.00 -90.00   52
 22  \w    131.00 157.00   0.50    2.00    --  103.79 125.00 150.00   52
 23  \w    103.00 134.00   0.50    2.00    --  103.79  15.00-150.00   62
 24  \w    131.00 165.00   0.50    2.00    --  103.79  77.00  60.00   68
 25  \w     39.00  96.00   0.50    2.00    --  103.79-125.00 -60.00  114
 26  \w    106.00 136.00   0.50    2.00    --  103.79  15.00  60.00   60
 27  \w    108.00 136.00   0.50    2.00    --  103.79  15.00   0.00   56
 28  \w     54.00  99.00   0.50    2.00    --  103.79-125.00-180.00   90
 29  \w     43.00  68.00   0.50    2.00    --  103.79 -77.00 150.00   50
 30  \w    103.00 134.00   0.50    2.00    --  103.79  15.00 -90.00   62
 31  \w     40.00  66.00   0.50    2.00    --  103.79-125.00 150.00   52
 32  \w    106.00 131.00   0.50    2.00    --  103.79  30.00 -30.00   50
 33  \w     49.00  90.00   0.50    2.00    --  103.79 -95.00-150.00   82
 34  \w     42.00  72.00   0.50    2.00    --  103.79 -77.00 120.00   60
 35  \w    137.00 163.00   0.50    2.00    --  103.79  77.00 150.00   52
 36  \w     42.00  90.00   0.50    2.00    --  103.79 -95.00  60.00   96
 37  \w    104.00 136.00   0.50    2.00    --  103.79  15.00 150.00   64
 38  \w     41.00  81.00   0.50    2.00    --  103.79 -95.00-180.00   80
 39  \w    103.00 128.00   0.50    2.00    --  103.79  15.00 -30.00   50
 40  \w    103.00 136.00   0.50    2.00    --  103.79  15.00  90.00   66
 41  \w    118.00 143.00   0.50    2.00    --  103.79 125.00  90.00   50
 42  \w     44.00  92.00   0.50    2.00    --  103.79 -95.00 -30.00   96
 43  \w    104.00 135.00   0.50    2.00    --  103.79  15.00-180.00   62
 44  \w     60.00  89.00   0.50    2.00    --  103.79 -95.00  30.00   58
 45  \w    103.00 128.00   0.50    2.00    --  103.79  15.00  30.00   50
 46  \w     52.00  98.00   0.50    2.00    --  103.79-125.00 120.00   92
 47  \w     66.00  91.00   0.50    2.00    --  103.79 -95.00 150.00   50
 48  \w    124.00 149.00   0.50    2.00    --  103.79 125.00-180.00   50
 49  \w     45.00  92.00   0.50    2.00    --  103.79 -95.00   0.00   94
 50  \w     43.00  69.00   0.50    2.00    --  103.79 -77.00   0.00   52
 51  \w    103.00 135.00   0.50    2.00    --  103.79  15.00 120.00   64
 52  \w     42.00  67.00   0.50    2.00    --  103.79 -77.00-120.00   50
 53  \w     46.00  71.00   0.50    2.00    --  103.79-125.00 -90.00   50
 54  \w    103.00 128.00   0.50    2.00    --  103.79  61.00-180.00   50
 55  \w     68.00  93.00   0.50    2.00    --  107.75 -94.00-102.68   50
 56  \w     51.00  92.00   0.50    2.00    --  107.75 -92.00 -61.52   82
 57  \w     65.00  91.00   0.50    2.00    --  107.75 -97.00-159.93   52
 58  \w     48.00  93.00   0.50    2.00    --  107.75-100.00 106.58   90
 59  \w     68.00  93.00   0.50    2.00    --  107.75 -96.00 120.33   50
 60  \w     65.00  92.00   0.50    2.00    --  107.75-101.00-177.51   54
 61  \w     68.00  93.00   0.50    2.00    --  107.75-100.00  53.68   50
 62  \w     46.00  93.00   0.50    2.00    --  107.75-100.00-128.52   94
 63  \w     68.00  93.00   0.50    2.00    --  107.75 -91.00-127.91   50
 64  \w     49.00  92.00   0.50    2.00    --  107.75 -95.00 -77.36   86
 65  \w     68.00  93.00   0.50    2.00    --  107.75 -94.00 -13.21   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      0.0071342000
_diffrn_orient_matrix_UB_12      0.0542776000
_diffrn_orient_matrix_UB_13      0.0796140000
_diffrn_orient_matrix_UB_21      0.0838521000
_diffrn_orient_matrix_UB_22      -0.0580520000
_diffrn_orient_matrix_UB_23      0.0432029000
_diffrn_orient_matrix_UB_31      0.0693740000
_diffrn_orient_matrix_UB_32      0.0644926000
_diffrn_orient_matrix_UB_33      -0.0280824000
_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  0.0250
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            59888
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.959
_diffrn_reflns_theta_min         3.674
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77842
_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    0.937
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         7593
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0663P)^2^+1.4610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6962
_reflns_number_total             7593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04144a2.cif
_cod_data_source_block           y24mu06
_cod_depositor_comments
'Adding full bibliography for 1575607--1575611.cif.'
_cod_database_code               1575610
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C28 H68 Li2 Mg N4'
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.857
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H,H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13-H13A = C13-H13B = C1-H1A = C1-H1B = C5-H5B = C5-H5A
 0.99 with sigma of 0.005
 C9-C10A \\sim C9-C10 \\sim C11-C10 \\sim C11A-C10A \\sim C12A-C11A \\sim
C12-C11
 with sigma of 0.005
 C12-C10 \\sim C12A-C10A \\sim C11A-C9
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C10 \\sim C11 \\sim C12 \\sim C10A \\sim C11A \\sim C12A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Fixed Sof: H9AA(0.9) H9AB(0.9) H9BC(0.1) H9BD(0.1) C10(0.9) H10A(0.9)
 H10B(0.9) C11(0.9) H11A(0.9) H11B(0.9) C12(0.9) H12A(0.9) H12B(0.9) H12C(0.9)
 C10A(0.1) H10C(0.1) H10D(0.1) C11A(0.1) H11C(0.1) H11D(0.1) C12A(0.1)
 H12D(0.1) H12E(0.1) H12F(0.1)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B), C9(H9AA,H9AB), C9(H9BC,
 H9BD), C14(H14A,H14B), C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B),
 C23(H23A,H23B), C24(H24A,H24B), C10(H10B,H10A), C11(H11B,H11A), C10A(H10C,
 H10D), C11A(H11D,H11C)
5.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), 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), C12(H12B,
 H12C,H12A), C12A(H12F,H12D,H12E)
;
_shelx_res_checksum              41997
_shelx_hkl_checksum              37390
_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 1.896
_oxdiff_exptl_absorpt_empirical_full_min 0.646