On the nature and limits of alkaline earth-triel bonding.
Boronski, Josef T.; Griffin, Liam P.; Conder, Caroline; Crumpton, Agamemnon E.; Wales, Lewis L.; Aldridge, Simon; Chemical science 15 (2024) 15377–15384; doi:10.1039/d4sc03832k

data_1572469
_publ_section_title
;
 On the nature and limits of alkaline earth-triel bonding.
;
_journal_issue                   37
_journal_name_full               'Chemical science'
_journal_page_first              15377
_journal_page_last               15384
_journal_paper_doi               10.1039/d4sc03832k
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C47 H62 Al N2 O, C5 H5 Mg'
_chemical_formula_sum            'C52 H67 Al Mg N2 O'
_chemical_formula_weight         787.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-04-09 deposited with the CCDC.	2024-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.1377(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6415(2)
_cell_length_b                   19.3339(3)
_cell_length_c                   18.9730(3)
_cell_measurement_reflns_used    37113
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.0860
_cell_measurement_theta_min      4.1500
_cell_volume                     4727.45(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_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     12.00  44.00   0.50    5.00    --   56.98-101.00  49.00   64
  2  \w     75.00 102.00   0.50   10.00    --   84.18-101.00  49.00   54
  3  \w     47.00  72.00   0.50   10.00    --   84.18-101.00  49.00   50
  4  \w      9.00  37.00   0.50    5.00    --   56.98 -30.00 -90.00   56
  5  \w     14.00  39.00   0.50    5.00    --   56.98 -95.00 150.00   50
  6  \w     62.00  87.00   0.50    5.00    --   56.98  45.00-150.00   50
  7  \w      6.00  37.00   0.50    5.00    --   56.98 -30.00 150.00   62
  8  \w      7.00  36.00   0.50    5.00    --   56.98 -30.00-180.00   58
  9  \w     44.00  69.00   0.50    5.00    --   56.98 -95.00 150.00   50
 10  \w     20.00  65.00   0.50    5.00    --   56.98 -95.00   0.00   90
 11  \w      4.00  30.00   0.50    5.00    --   56.98 -30.00-150.00   52
 12  \w     83.00 121.00   0.50    5.00    --   69.93  45.00  90.00   76
 13  \w     21.00  46.00   0.50    5.00    --   69.93 -45.00 120.00   50
 14  \w     19.00  45.00   0.50    5.00    --   69.93 -45.00  90.00   52
 15  \w     30.00  80.00   0.50    5.00    --   69.93 -95.00 120.00  100
 16  \w     45.00  80.00   0.50    5.00    --   69.93-101.00  49.00   70
 17  \w     22.00  48.00   0.50    5.00    --   69.93 -45.00-120.00   52
 18  \w     44.00  81.00   0.50   10.00    --   84.18 -77.00  60.00   74
 19  \w     60.00  86.00   0.50   10.00    --   84.18 -77.00-150.00   52
 20  \w     44.00  72.00   0.50   10.00    --   84.18 -61.00-120.00   56
 21  \w     44.00  88.00   0.50   10.00    --   84.18 -77.00 120.00   88
 22  \w     89.00 127.00   0.50   10.00    --   84.18  45.00  30.00   76
 23  \w     89.00 135.00   0.50   10.00    --   84.18  45.00 -60.00   92
 24  \w     39.00  67.00   0.50   10.00    --   84.18 -61.00 -90.00   56
 25  \w     79.00 106.00   0.50   10.00    --   84.18-111.00 120.00   54
 26  \w     47.00  72.00   0.50   10.00    --   84.18 -61.00-150.00   50
 27  \w     43.00  69.00   0.50   10.00    --   84.18 -61.00 -60.00   52
 28  \w     46.00  98.00   0.50   10.00    --   84.18 -95.00  60.00  104
 29  \w     91.00 117.00   0.50   10.00    --   84.18 178.00 -90.00   52
 30  \w     92.00 118.00   0.50   10.00    --   84.18  45.00   0.00   52
 31  \w     40.00  65.00   0.50   10.00    --   84.18 -61.00  60.00   50
 32  \w     98.00 129.00   0.50   10.00    --   84.18  45.00-120.00   62
 33  \w     52.00  89.00   0.50   10.00    --   84.18 -95.00 120.00   74
 34  \w     56.00  82.00   0.50   10.00    --   84.18 178.00 -90.00   52
 35  \w     41.00  66.00   0.50   10.00    --   84.18 -61.00 -30.00   50
 36  \w    102.00 127.00   0.50   10.00    --   84.18  45.00  60.00   50
 37  \w     89.00 116.00   0.50   10.00    --   84.18   0.00-120.00   54
 38  \w     51.00  76.00   0.50   10.00    --   84.18   0.00-120.00   50
 39  \w     54.00  80.00   0.50   10.00    --   84.18 -77.00 -60.00   52
 40  \w     84.00 134.00   0.50   10.00    --   84.18  30.00   0.00  100
 41  \w     44.00  80.00   0.50   10.00    --   84.18 -77.00 150.00   72
 42  \w     46.00  72.00   0.50   10.00    --   84.18 -61.00-180.00   52
 43  \w     75.00 100.00   0.50   10.00    --   84.18 -95.00 150.00   50
 44  \w     89.00 125.00   0.50   10.00    --   84.18  45.00-150.00   72
 45  \w     67.00  93.00   0.50   10.00    --   84.18 178.00  30.00   52
 46  \w     95.00 127.00   0.50   10.00    --   84.18 178.00  30.00   64
 47  \w     58.00  83.00   0.50   10.00    --   84.18 178.00-120.00   50
 48  \w     94.00 131.00   0.50   10.00    --   84.18  45.00 120.00   74
 49  \w     33.00  58.00   0.50    5.00    --   69.93-101.00  49.00   50
 50  \w      6.00  46.00   0.50    5.00    --   56.98 -45.00  30.00   80
 51  \w      4.00  30.00   0.50    5.00    --   56.98 -30.00  30.00   52
 52  \w      5.00  32.00   0.50    5.00    --   56.98 -30.00 -60.00   54
 53  \w     19.00  44.00   0.50    5.00    --   69.93 -45.00   0.00   50
 54  \w     30.00  76.00   0.50    5.00    --   69.93 -95.00 -90.00   92
 55  \w     73.00 103.00   0.50    5.00    --   69.93-125.00-150.00   60
 56  \w     79.00 120.00   0.50    5.00    --   69.93  30.00 150.00   82
 57  \w     90.00 120.00   0.50    5.00    --   69.93  45.00 -90.00   60
 58  \w     87.00 122.00   0.50    5.00    --   69.93  30.00  30.00   70
 59  \w     35.00  83.00   0.50    5.00    --   69.93 -95.00 -30.00   96
 60  \w     41.00  70.00   0.50    5.00    --   69.93 -95.00-150.00   58
 61  \w     46.00  72.00   0.50   10.00    --   84.18-111.00 -60.00   52
 62  \w     86.00 125.00   0.50   10.00    --   84.18   0.00 -30.00   78
 63  \w     80.00 106.00   0.50   10.00    --   84.18-111.00 -60.00   52
 64  \w     53.00  97.00   0.50   10.00    --   84.18 178.00 120.00   88
 65  \w     69.00 136.00   0.50   10.00    --   84.18  15.00 120.00  134
 66  \w     40.00  67.00   0.50   10.00    --   84.18   0.00 -30.00   54
 67  \w     77.00 108.00   0.50   10.00    --   84.18-111.00  30.00   62
 68  \w     74.00  99.00   0.50   10.00    --   84.18 -95.00-180.00   50
 69  \w     82.00 108.00   0.50   10.00    --   84.18-111.00 120.00   52
 70  \w     82.00 108.00   0.50   10.00    --   84.18-111.00 150.00   52
 71  \w     52.00  78.00   0.50   10.00    --   84.18 -77.00-120.00   52
 72  \w     89.00 131.00   0.50   10.00    --   84.18  30.00 150.00   84
 73  \w     83.00 108.00   0.50   10.00    --   84.18-111.00   0.00   50
 74  \w     55.00  85.00   0.50   10.00    --   84.18-111.00-180.00   60
 75  \w     84.00 134.00   0.50   10.00    --   84.18  30.00-150.00  100
 76  \w     46.00  72.00   0.50   10.00    --   84.18 -95.00-150.00   52
 77  \w     47.00  73.00   0.50   10.00    --   84.18 -95.00 -60.00   52
 78  \w     38.00  64.00   0.50   10.00    --   84.18-111.00   0.00   52
 79  \w     81.00 107.00   0.50   10.00    --   84.18-111.00  90.00   52
 80  \w    100.00 127.00   0.50   10.00    --   84.18  15.00 -90.00   54
 81  \w     68.00 107.00   0.50   10.00    --   84.18-111.00-150.00   78
 82  \w     92.00 118.00   0.50   10.00    --   84.18  45.00  90.00   52
 83  \w    103.00 136.00   0.50   10.00    --   84.18  30.00 -90.00   66
 84  \w     55.00  81.00   0.50   10.00    --   84.18 -95.00   0.00   52
 85  \w    107.00 132.00   0.50   10.00    --   84.18  45.00 -90.00   50
 86  \w     74.00 105.00   0.50   10.00    --   84.18-111.00-120.00   62
 87  \w     78.00 105.00   0.50   10.00    --   84.18-111.00 -30.00   54
 88  \w     85.00 134.00   0.50   10.00    --   84.18  30.00-180.00   98
 89  \w    107.00 133.00   0.50   10.00    --   84.18  30.00  30.00   52
 90  \w     80.00 115.00   0.50   10.00    --   84.18  30.00  90.00   70
 91  \w     75.00 100.00   0.50   10.00    --   84.18 -95.00 -30.00   50
 92  \w     93.00 118.00   0.50   10.00    --   84.18   0.00-150.00   50
 93  \w     82.00 107.00   0.50   10.00    --   86.75-104.00-101.12   50
 94  \w     58.00 107.00   0.50   10.00    --   86.75-105.00  40.65   98
 95  \w     50.00  76.00   0.50   10.00    --   86.75-104.00-101.12   52
 96  \w     33.00  58.00   0.50    5.00    --   69.93-101.00  49.00   50
 97  \w     -1.00  25.00   0.50    5.00    --   -6.75  61.00 120.00   52
 98  \w    -43.00 -15.00   0.50    5.00    --   -6.75 -61.00 -30.00   56
 99  \w      0.00  29.00   0.50    5.00    --   -6.75  61.00  60.00   58
100  \w     -5.00  38.00   0.50    5.00    --   -6.75  30.00   0.00   86
101  \w     -9.00  16.00   0.50    5.00    --   10.00 101.00 147.88   50
102  \w     -8.00  19.00   0.50    5.00    --   10.00 100.00 -49.65   54
103  \w     -1.00  24.00   0.50    5.00    --   14.00  95.00  68.06   50
104  \w     15.00  42.00   0.50    5.00    --   26.00  89.00 -76.20   54
105  \w     15.00  40.00   0.50    5.00    --   26.00  89.00-142.78   50
106  \w     17.00  42.00   0.50    5.00    --   26.00  86.00 162.26   50
107  \w     13.00  38.00   0.50    5.00    --   26.00  92.00  80.10   50
108  \w     13.00  38.00   0.50    5.00    --   26.00  92.00   0.81   50
109  \w     27.00  52.00   0.50    5.00    --   30.00  77.00  66.13   50
110  \w     31.00  56.00   0.50    5.00    --   34.00  76.00  95.11   50
111  \w     31.00  58.00   0.50    5.00    --   34.00  77.00-152.23   54
112  \w     32.00  57.00   0.50    5.00    --   34.00  75.00 -52.52   50
113  \w     35.00  60.00   0.50    5.00    --   38.00  77.00  22.38   50
114  \w     37.00  62.00   0.50    5.00    --   38.00  73.00  69.79   50
115  \w     35.00  60.00   0.50    5.00    --   38.00  77.00 175.78   50
116  \w     35.00  60.00   0.50    5.00    --   38.00  77.00 -30.59   50
117  \w     39.00  64.00   0.50    5.00    --   42.00  77.00 156.11   50
118  \w     39.00  64.00   0.50    5.00    --   42.00  77.00  -7.42   50
119  \w     39.00  64.00   0.50    5.00    --   42.00  76.00 -99.31   50
120  \w     40.00  65.00   0.50    5.00    --   42.00  74.00  89.42   50
121  \w     40.00  65.00   0.50    5.00    --   42.00  75.00 110.87   50
122  \w     39.00  64.00   0.50    5.00    --   42.00  77.00 132.82   50
123  \w     43.00  68.00   0.50    5.00    --   46.00  77.00 -73.20   50
124  \w     43.00  68.00   0.50    5.00    --   46.00  77.00  -5.20   50
125  \w     43.00  68.00   0.50    5.00    --   46.00  77.00-129.38   50
126  \w     43.00  68.00   0.50    5.00    --   46.00  77.00-146.47   50
127  \w     47.00  72.00   0.50    5.00    --   50.00  77.00  59.91   50
128  \w     47.00  72.00   0.50    5.00    --   50.00  77.00  20.20   50
129  \w     47.00  72.00   0.50    5.00    --   50.00  77.00 109.25   50
130  \w     51.00  76.00   0.50    5.00    --   54.00  77.00-173.68   50
131  \w     51.00  76.00   0.50    5.00    --   54.00  77.00-117.97   50
132  \w     53.00  78.00   0.50    5.00    --   54.00  73.00 137.34   50
133  \w     51.00  63.50   0.50    5.00    --   54.00  77.00 -48.45   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1170389000
_diffrn_orient_matrix_UB_12      -0.0160991000
_diffrn_orient_matrix_UB_13      0.0281957000
_diffrn_orient_matrix_UB_21      0.0227215000
_diffrn_orient_matrix_UB_22      0.0742837000
_diffrn_orient_matrix_UB_23      0.0303460000
_diffrn_orient_matrix_UB_31      -0.0083018000
_diffrn_orient_matrix_UB_32      -0.0239021000
_diffrn_orient_matrix_UB_33      0.0753200000
_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  0.0908
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            136512
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.559
_diffrn_reflns_theta_min         3.362
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.61a (Rigaku Oxford Diffraction, 2022)
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    1.106
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         9689
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0661
_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^)+(0.1094P)^2^+2.9015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1834
_refine_ls_wR_factor_ref         0.2016
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7166
_reflns_number_total             9689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03832k2.cif
_cod_data_source_block           073craec22_auto
_cod_depositor_comments
'Adding full bibliography for 1572469--1572472.cif.'
_cod_database_code               1572469
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C25 H25 Al2 Mg2 N2'
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.829
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma
for terminal atoms of 0.06 within 1A
3. Rigid body (RIGU) restrains
 C39, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C47, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C38, C37, C39
 with sigma for 1-2 distances of 0.04 and sigma for 1-3 distances of 0.04
4.a Ternary CH refined with riding coordinates:
 C49(H49), C34(H34), C46(H46), C37(H37)
4.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C52(H52), C19(H19), C8(H8), C42(H42), C32(H32), C44(H44), C31(H31),
 C43(H43), C30(H30), C1(H1), C5(H5), C4(H4), C2(H2), C3(H3)
4.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C51(H51A,H51B,H51C), C13(H13A,H13B,
 H13C), C50(H50A,H50B,H50C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C36(H36A,
 H36B,H36C), C24(H24A,H24B,H24C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C35(H35A,H35B,H35C), C48(H48A,H48B,H48C), C47(H47A,H47B,H47C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              25868
_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 3.204
_oxdiff_exptl_absorpt_empirical_full_min 0.323