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_1575607
_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 Mg N8'
_chemical_formula_sum            'C32 H72 Li2 Mg N8'
_chemical_formula_weight         607.16
_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             2025-01-14
_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                 103.329(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9078(2)
_cell_length_b                   17.4149(3)
_cell_length_c                   20.8490(5)
_cell_measurement_reflns_used    29145
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      79.0870
_cell_measurement_theta_min      3.3010
_cell_volume                     3853.75(14)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_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 0.989
_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     19.00  81.00   0.50    2.00    --   50.88-106.00  57.00  124
  2  \w    -67.00   3.00   0.50    2.00    --  -52.88 106.00 157.00  140
  3  \w    -67.00 -16.00   0.50    2.00    --  -78.40 106.00 157.00  102
  4  \w     42.00  93.00   0.50    2.00    --  103.80-106.00  57.00  102
  5  \w    120.00 166.00   0.50    2.00    --  103.80 106.00 157.00   92
  6  \w     -3.00  23.00   0.50    2.00    --   10.00  80.00-136.22   52
  7  \w     -2.00  25.00   0.50    2.00    --   10.00  78.00-100.93   54
  8  \w      0.00  28.00   0.50    2.00    --   10.00  75.00  66.75   56
  9  \w    -38.00 -12.00   0.50    2.00    --  -14.00 -60.00  27.93   52
 10  \w   -116.00 -48.00   0.50    2.00    --  -46.00 -47.00 -27.03  136
 11  \w   -129.00 -62.00   0.50    2.00    --  -58.00 -41.00 165.54  134
 12  \w   -131.00 -62.00   0.50    2.00    --  -62.00 -54.00  22.66  138
 13  \w   -136.00 -67.00   0.50    2.00    --  -66.00 -48.00 -44.07  138
 14  \w     12.00  93.00   0.50    2.00    --   74.00 -92.00-143.15  162
 15  \w    -51.00 -10.00   0.50    2.00    --  -78.40  61.00 -60.00   82
 16  \w    -66.00 -16.00   0.50    2.00    --  -78.40  77.00 -90.00  100
 17  \w   -136.00 -78.00   0.50    2.00    --  -78.40 -15.00-150.00  116
 18  \w    -75.00 -14.00   0.50    2.00    --  -78.40 125.00  60.00  122
 19  \w    -66.00 -16.00   0.50    2.00    --  -78.40  77.00  90.00  100
 20  \w    -66.00 -17.00   0.50    2.00    --  -78.40  77.00 150.00   98
 21  \w    -66.00 -41.00   0.50    2.00    --  -78.40  77.00  30.00   50
 22  \w   -153.00-117.00   0.50    2.00    --  -86.25 -60.00 136.21   72
 23  \w    103.00 130.00   0.50    2.00    --  103.80  15.00 -90.00   54
 24  \w    103.00 134.00   0.50    2.00    --  103.80  15.00-180.00   62
 25  \w    103.00 135.00   0.50    2.00    --  103.80  15.00-150.00   64
 26  \w    136.00 161.00   0.50    2.00    --  103.80  77.00  30.00   50
 27  \w     48.00  92.00   0.50    2.00    --  103.80 -95.00  30.00   88
 28  \w    103.00 136.00   0.50    2.00    --  103.80  15.00 -30.00   66
 29  \w    135.00 162.00   0.50    2.00    --  103.80  77.00 120.00   54
 30  \w    103.00 131.00   0.50    2.00    --  103.80  15.00  90.00   56
 31  \w    122.00 150.00   0.50    2.00    --  103.80  77.00 -30.00   56
 32  \w     52.00  91.00   0.50    2.00    --  103.80 -95.00 -90.00   78
 33  \w     54.00  80.00   0.50    2.00    --  103.80 -95.00  60.00   52
 34  \w    103.00 135.00   0.50    2.00    --  103.80  15.00  60.00   64
 35  \w     49.00  92.00   0.50    2.00    --  103.80 -95.00  90.00   86
 36  \w    133.00 165.00   0.50    2.00    --  103.80 125.00 -90.00   64
 37  \w    115.00 140.00   0.50    2.00    --  103.80  45.00  60.00   50
 38  \w     62.00  88.00   0.50    2.00    --  103.80 -95.00 -30.00   52
 39  \w    104.00 135.00   0.50    2.00    --  103.80  15.00  30.00   62
 40  \w    131.00 167.00   0.50    2.00    --  103.80 125.00  90.00   72
 41  \w    103.00 135.00   0.50    2.00    --  103.80  15.00-120.00   64
 42  \w    139.00 164.00   0.50    2.00    --  103.80  77.00-150.00   50
 43  \w     56.00  92.00   0.50    2.00    --  103.80-125.00 -30.00   72
 44  \w    104.00 135.00   0.50    2.00    --  103.80  15.00 -60.00   62
 45  \w     48.00  74.00   0.50    2.00    --  103.80 -77.00   0.00   52
 46  \w    104.00 135.00   0.50    2.00    --  103.80  15.00 150.00   62
 47  \w     48.00  75.00   0.50    2.00    --  103.80 -95.00   0.00   54
 48  \w    124.00 168.00   0.50    2.00    --  103.80 125.00 -30.00   88
 49  \w    110.00 136.00   0.50    2.00    --  103.80  15.00 120.00   52
 50  \w     41.00  91.00   0.50    2.00    --  103.80 -95.00 150.00  100
 51  \w     48.00  74.00   0.50    2.00    --  103.80-125.00 150.00   52
 52  \w     75.00 100.00   0.50    2.00    --  103.80-125.00 150.00   50
 53  \w     42.00  67.00   0.50    2.00    --  103.80 -77.00-120.00   50
 54  \w     46.00  91.00   0.50    2.00    --  103.80 -95.00-180.00   90
 55  \w     42.00  67.00   0.50    2.00    --  103.80 -77.00  90.00   50
 56  \w    119.00 157.00   0.50    2.00    --  103.80  30.00 -30.00   76
 57  \w     59.00  90.00   0.50    2.00    --  107.75 -93.00 -59.59   62
 58  \w     67.00  93.00   0.50    2.00    --  107.75 -94.00  54.38   52
 59  \w     58.00  91.00   0.50    2.00    --  107.75 -94.00-133.80   66
 60  \w     48.00  93.00   0.50    2.00    --  107.75 -94.00   6.96   90
 61  \w     50.00  89.00   0.50    2.00    --  107.75 -87.00  66.64   78
 62  \w     67.00  93.00   0.50    2.00    --  107.75-100.00  -7.25   52
 63  \w     46.00  92.00   0.50    2.00    --  107.75 -99.00  56.76   92
 64  \w     46.00  93.00   0.50    2.00    --  107.75-102.00 139.48   94
 65  \w     46.00  93.00   0.50    2.00    --  107.75 -96.00-165.57   94
 66  \w     45.00  70.00   0.50    2.00    --  107.75 -93.00  15.28   50
 67  \w     64.00  90.00   0.50    2.00    --  107.75-102.00 -14.23   52
 68  \w     66.00  92.00   0.50    2.00    --  107.75 -97.00  -1.50   52
 69  \w     46.00  71.00   0.50    2.00    --  107.75-102.00 -70.06   50
 70  \w     46.00  93.00   0.50    2.00    --  107.75-100.00-106.21   94
 71  \w     45.00  92.00   0.50    2.00    --  107.75 -94.00 -38.64   94
 72  \w     67.00  92.00   0.50    2.00    --  107.75 -98.00-141.64   50
 73  \w     64.00  92.00   0.50    2.00    --  107.75 -95.00 -75.33   56
 74  \w     66.00  92.00   0.50    2.00    --  107.75 -98.00 172.30   52
;
_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      -0.0391493000
_diffrn_orient_matrix_UB_12      0.0789375000
_diffrn_orient_matrix_UB_13      0.0221760000
_diffrn_orient_matrix_UB_21      -0.0804680000
_diffrn_orient_matrix_UB_22      0.0145763000
_diffrn_orient_matrix_UB_23      -0.0699799000
_diffrn_orient_matrix_UB_31      -0.1141884000
_diffrn_orient_matrix_UB_32      -0.0372623000
_diffrn_orient_matrix_UB_33      0.0195085000
_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  0.0423
_diffrn_reflns_av_unetI/netI     0.0062
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            59582
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.072
_diffrn_reflns_theta_min         3.345
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66646
_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    1.046
_exptl_crystal_description       plate
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         15283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0708P)^2^+0.4733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1220
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14070
_reflns_number_total             15283
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9605\% 
around [0.92 -0.00 -0.40] (reciprocal) or [1.00 -0.00 -0.00] (direct)
;
_cod_data_source_file            d5cc04144a2.cif
_cod_data_source_block           y24mu09_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 1575607--1575611.cif.'
_cod_database_code               1575607
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Li2 Mg N8 C32 H68'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8510(5)
 0.1490(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C1(H1A,H1B), C5(H5A,H5B), C6(H6A,H6B), C9(H9A,H9B), C16(H16A,
 H16B), C20(H20A,H20B), C7(H7A,H7B), C2(H2A,H2B), C22(H22A,H22B), C21(H21A,
 H21B), C8(H8A,H8B), C11(H11A,H11B), C15(H15A,H15B), C4(H4A,H4B), C17(H17A,
 H17B), C19(H19A,H19B), C12(H12A,H12B), C18(H18A,H18B), C13(H13A,H13B), C3(H3A,
 H3B), C14(H14A,H14B), C28(H28A,H28B), C27(H27A,H27B)
3.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C31(H31A,H31B,H31C), C23(H23A,H23B,
 H23C), C32(H32A,H32B,H32C), C24(H24A,H24B,H24C), C30(H30A,H30B,H30C), C29(H29A,
 H29B,H29C)
;
_shelx_res_checksum              16512
_shelx_hkl_checksum              74136
_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 1.650
_oxdiff_exptl_absorpt_empirical_full_min 0.703
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2