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_1575608
_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         'C32 H72 Li2 Mn N8'
_chemical_formula_sum            'C32 H72 Li2 Mn N8'
_chemical_formula_weight         637.79
_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             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                90
_cell_angle_beta                 103.359(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9743(2)
_cell_length_b                   17.4237(3)
_cell_length_c                   20.8979(3)
_cell_measurement_reflns_used    38952
_cell_measurement_temperature    149.98(16)
_cell_measurement_theta_max      77.9560
_cell_measurement_theta_min      3.3010
_cell_volume                     3887.82(12)
_computing_cell_refinement       'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.144a 64-bit (release 23-01-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.43.143a (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.98(16)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.958
_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     40.00 123.00   0.50    1.00    --   47.16  28.00-162.00  166
  2  \w   -126.00 -42.00   0.50    1.00    --  -49.16 -28.00  35.00  168
  3  \w   -126.00 -42.00   0.50    1.00    --  -49.16 -28.00  35.00  168
  4  \w   -159.00 -74.00   0.50    4.00    --  -82.28 -28.00  35.00  170
  5  \w   -159.00 -74.00   0.50    4.00    --  -82.28 -28.00  35.00  170
  6  \w    101.00 164.00   0.50    4.00    --  109.02  28.00-162.00  126
  7  \w    -29.00   4.00   0.50    1.00    --    6.00 104.00-133.51   66
  8  \w    -25.00   4.00   0.50    1.00    --   10.00 104.00  69.50   58
  9  \w     -8.00  18.00   0.50    1.00    --   14.00  85.00 120.29   52
 10  \w    -10.00  16.00   0.50    1.00    --   14.00  87.00 -50.02   52
 11  \w     -8.00  18.00   0.50    1.00    --   14.00  85.00 101.31   52
 12  \w     -8.00  18.00   0.50    1.00    --   14.00  85.00 -27.42   52
 13  \w     32.00  58.00   0.50    1.00    --   42.00  62.00 143.47   52
 14  \w    -29.00   2.00   0.50    1.00    --   47.16 -28.00  35.00   62
 15  \w     -2.00  27.00   0.50    1.00    --  -49.16  28.00-162.00   58
 16  \w      8.00  92.00   0.50    1.00    --   66.00 -90.00 -66.06  168
 17  \w      6.00  90.00   0.50    1.00    --   66.00 -87.00  61.95  168
 18  \w      8.00  92.00   0.50    1.00    --   66.00 -90.00 -66.06  168
 19  \w      6.00  90.00   0.50    1.00    --   66.00 -87.00 -54.03  168
 20  \w      6.00  90.00   0.50    1.00    --   66.00 -87.00  61.95  168
 21  \w     66.00  92.00   0.50    1.00    --   66.00 -98.00-154.12   52
 22  \w     12.00  88.00   0.50    1.00    --   66.00 -84.00   5.31  152
 23  \w     21.00  48.00   0.50    1.00    --   70.00 -86.00-145.38   54
 24  \w     61.00  91.00   0.50    1.00    --   70.00 -86.00-145.38   60
 25  \w     63.00  93.00   0.50    1.00    --   70.00 -90.00 102.75   60
 26  \w     15.00  40.00   0.50    1.00    --   70.00 -90.00 102.75   50
 27  \w   -128.00-101.00   0.50    4.00    --  -82.28 -77.00-150.00   54
 28  \w    -42.00 -17.00   0.50    4.00    --  -82.28  61.00 150.00   50
 29  \w    -50.00 -24.00   0.50    4.00    --  -82.28  61.00 120.00   52
 30  \w   -127.00-101.00   0.50    4.00    --  -82.28 -77.00 -90.00   52
 31  \w    -48.00 -19.00   0.50    4.00    --  -82.28  61.00-180.00   58
 32  \w    -51.00 -26.00   0.50    4.00    --  -82.28  61.00 -90.00   50
 33  \w    -66.00 -17.00   0.50    4.00    --  -82.28  77.00-150.00   98
 34  \w   -148.00-101.00   0.50    4.00    --  -82.28 -77.00-180.00   94
 35  \w   -147.00-103.00   0.50    4.00    --  -82.28 -77.00 -30.00   88
 36  \w     54.00  92.00   0.50    4.00    --  109.02 -95.00-180.00   76
 37  \w     56.00 101.00   0.50    4.00    --  109.02-125.00 150.00   90
 38  \w    108.00 144.00   0.50    4.00    --  109.02 125.00 120.00   72
 39  \w    137.00 163.00   0.50    4.00    --  109.02  77.00 120.00   52
 40  \w     57.00 100.00   0.50    4.00    --  109.02-125.00-180.00   86
 41  \w     97.00 123.00   0.50    4.00    --  109.02  15.00 -60.00   52
 42  \w     66.00  92.00   0.50    4.00    --  109.02 -95.00   0.00   52
 43  \w    143.00 174.00   0.50    4.00    --  109.02  77.00-180.00   62
 44  \w     92.00 130.00   0.50    4.00    --  109.02  15.00-180.00   76
 45  \w    123.00 174.00   0.50    4.00    --  109.02  77.00  30.00  102
 46  \w    103.00 162.00   0.50    4.00    --  109.02  30.00-120.00  118
 47  \w     66.00  92.00   0.50    4.00    --  109.02 -95.00 150.00   52
 48  \w    121.00 160.00   0.50    4.00    --  109.02  30.00-150.00   78
 49  \w     43.00  68.00   0.50    4.00    --  109.02 -77.00 -30.00   50
 50  \w     43.00  68.00   0.50    4.00    --  109.02 -77.00-180.00   50
 51  \w     43.00  68.00   0.50    4.00    --  109.02 -77.00 150.00   50
 52  \w     43.00  69.00   0.50    4.00    --  109.02 -77.00 -60.00   52
 53  \w     92.00 135.00   0.50    4.00    --  109.02  15.00 -30.00   86
 54  \w     47.00  78.00   0.50    4.00    --  109.02 -95.00  30.00   62
 55  \w     95.00 125.00   0.50    4.00    --  109.02  15.00  60.00   60
 56  \w    100.00 126.00   0.50    4.00    --  109.02  15.00 150.00   52
 57  \w     46.00  73.00   0.50    4.00    --  109.02 -77.00  60.00   54
 58  \w     40.00  66.00   0.50    4.00    --  109.02-125.00 120.00   52
 59  \w    122.00 175.00   0.50    4.00    --  109.02  77.00  60.00  106
 60  \w    116.00 166.00   0.50    4.00    --  109.02  30.00 -30.00  100
 61  \w     58.00 101.00   0.50    4.00    --  109.02-125.00-120.00   86
 62  \w     49.00  92.00   0.50    4.00    --  109.02 -95.00 -30.00   86
 63  \w     75.00 101.00   0.50    4.00    --  109.02-125.00   0.00   52
 64  \w     61.00  87.00   0.50    4.00    --  109.02-125.00 -90.00   52
 65  \w     43.00  68.00   0.50    4.00    --  109.02 -77.00  90.00   50
 66  \w     48.00  93.00   0.50    4.00    --  111.75 -93.00  66.06   90
 67  \w     65.00  91.00   0.50    4.00    --  111.75 -94.00 -10.75   52
 68  \w     67.00  93.00   0.50    4.00    --  111.75 -93.00 -98.03   52
 69  \w     51.00  92.00   0.50    4.00    --  111.75 -92.00  13.12   82
 70  \w     65.00  92.00   0.50    4.00    --  111.75 -96.00 121.96   54
 71  \w     47.00  92.00   0.50    4.00    --  111.75 -96.00-105.11   90
 72  \w     48.00  93.00   0.50    4.00    --  111.75 -93.00  39.12   90
 73  \w     67.00  93.00   0.50    4.00    --  111.75 -91.00 170.70   52
 74  \w     51.00  92.00   0.50    4.00    --  111.75 -95.00-126.91   82
 75  \w     65.00  91.00   0.50    4.00    --  111.75 -94.00  91.73   52
 76  \w     57.00  92.00   0.50    4.00    --  111.75 -93.00-142.57   70
 77  \w     46.00  90.00   0.50    4.00    --  111.75 -94.00 -72.67   88
;
_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      0.0695482000
_diffrn_orient_matrix_UB_12      0.0773027000
_diffrn_orient_matrix_UB_13      0.0124401000
_diffrn_orient_matrix_UB_21      -0.1249113000
_diffrn_orient_matrix_UB_22      0.0428280000
_diffrn_orient_matrix_UB_23      -0.0245652000
_diffrn_orient_matrix_UB_31      -0.0197513000
_diffrn_orient_matrix_UB_32      0.0012570000
_diffrn_orient_matrix_UB_33      0.0706380000
_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  0.1038
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            78111
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         81.988
_diffrn_reflns_theta_min         3.340
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.975
_exptl_absorpt_correction_T_max  0.68520
_exptl_absorpt_correction_T_min  0.66356
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.143a (Rigaku Oxford Diffraction, 2024)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_description       plate
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_exptl_crystal_size_rad          0.092
_refine_diff_density_max         1.428
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         8255
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0789
_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^)+(0.0932P)^2^+9.3210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2259
_refine_ls_wR_factor_ref         0.2305
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7180
_reflns_number_total             8255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04144a2.cif
_cod_data_source_block           y25mu07_refinalized
_cod_depositor_comments
'Adding full bibliography for 1575607--1575611.cif.'
_cod_database_code               1575608
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C32 H72 Li2 Mn1 N8'
_shelx_estimated_absorpt_t_max   0.797
_shelx_estimated_absorpt_t_min   0.431
_diffrn_oxdiff_digest_hkl
;
431dae7cd5361ba8af0295d3900de85ed018bd
;
_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.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C1(H1A,H1B), C20(H20A,H20B), C6(H6A,H6B), C7(H7A,H7B), C17(H17A,
 H17B), C11(H11A,H11B), C21(H21A,H21B), C2(H2A,H2B), C10(H10A,H10B), C8(H8A,
 H8B), C19(H19A,H19B), C22(H22A,H22B), C4(H4A,H4B), C3(H3A,H3B), C15(H15A,H15B),
  C16(H16A,H16B), C18(H18A,H18B), C9(H9A,H9B), C14(H14A,H14B), C27(H27A,H27B),
 C12(H12A,H12B), C13(H13A,H13B), C28(H28A,H28B)
2.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C24(H24A,H24B,H24C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C26(H26A,H26B,H26C), C32(H32A,
 H32B,H32C)
;
_shelx_res_checksum              24223
_shelx_hkl_checksum              85744
_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 2.597
_oxdiff_exptl_absorpt_empirical_full_min 0.505