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_1572470
_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         'C52 H67 Be In N2 O'
_chemical_formula_sum            'C52 H67 Be In N2 O'
_chemical_formula_weight         859.90
_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             2023-03-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-04-09 deposited with the CCDC.	2024-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.451(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9427(2)
_cell_length_b                   19.1025(3)
_cell_length_c                   18.6052(3)
_cell_measurement_reflns_used    19936
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      76.3500
_cell_measurement_theta_min      4.1450
_cell_volume                     4700.59(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_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      1.00  35.00   1.00    7.50    --  -41.65  19.00 -60.00   34
  2  \w    -16.00  31.00   1.00    7.50    --  -41.65  37.00  30.00   47
  3  \w    -11.00  30.00   1.00    7.50    --  -41.65  37.00-180.00   41
  4  \w     -5.00  20.00   1.00    7.50    --  -41.65  19.00   0.00   25
  5  \w      4.00  31.00   1.00    7.50    --  -41.65  19.00 -30.00   27
  6  \w     -3.00  29.00   1.00    7.50    --  -41.65  19.00-120.00   32
  7  \w     -5.00  35.00   1.00    7.50    --  -41.65  19.00  90.00   40
  8  \w     44.00  71.00   1.00   30.00    --  111.00 -45.00 -90.00   27
  9  \w    148.00 174.00   1.00   30.00    --  111.00  15.00-120.00   26
 10  \w     40.00  65.00   1.00   30.00    --  111.00 -45.00 -60.00   25
 11  \w     43.00  71.00   1.00   30.00    --  111.00 -45.00 120.00   28
 12  \w     45.00  72.00   1.00   30.00    --  111.00 -45.00  60.00   27
 13  \w     46.00  72.00   1.00   30.00    --  111.00-111.00-150.00   26
 14  \w     44.00  72.00   1.00   30.00    --  111.00 -45.00   0.00   28
 15  \w     42.00  68.00   1.00   30.00    --  111.00 -45.00-150.00   26
 16  \w    150.00 177.00   1.00   30.00    --  111.00  30.00 120.00   27
 17  \w     73.00  98.00   1.00   30.00    --  111.00  15.00-120.00   25
 18  \w     89.00 135.00   1.00   30.00    --  111.00  30.00 120.00   46
 19  \w    104.00 175.00   1.00   30.00    --  111.00 111.00 -30.00   71
 20  \w     46.00  72.00   1.00   30.00    --  111.00 -45.00-180.00   26
 21  \w     57.00 119.00   1.00   30.00    --  111.00 -77.00 -30.00   62
 22  \w    106.00 175.00   1.00   30.00    --  111.00  45.00 150.00   69
 23  \w     41.00  68.00   1.00   30.00    --  111.00 -45.00  30.00   27
 24  \w     83.00 108.00   1.00   30.00    --  111.00-111.00 -30.00   25
 25  \w     40.00  73.00   1.00   30.00    --  111.00-111.00 -30.00   33
 26  \w    129.00 164.00   1.00   30.00    --  111.00  77.00   0.00   35
 27  \w     66.00  91.00   1.00   30.00    --  111.00 -61.00  30.00   25
 28  \w     87.00 118.00   1.00   30.00    --  111.00  45.00 -60.00   31
 29  \w    -21.00   4.00   1.00    7.50    --  -41.65  37.00  30.00   25
 30  \w     -5.00  20.00   1.00    7.50    --  -41.65  19.00 -30.00   25
 31  \w   -114.00 -22.00   1.00    7.50    --  -41.65 -37.00 150.00   92
 32  \w      9.00  36.00   1.00    7.50    --  -41.65  19.00-150.00   27
 33  \w     -4.00  36.00   1.00    7.50    --  -41.65  19.00 -90.00   40
 34  \w    -21.00  13.00   1.00    7.50    --  -41.65  37.00  60.00   34
 35  \w     36.00  94.00   1.00    7.50    --   41.65-125.00 -30.00   58
 36  \w     92.00 163.00   1.00   30.00    --  111.00  61.00 120.00   71
 37  \w     43.00  98.00   1.00   30.00    --  111.00-111.00 -60.00   55
 38  \w    116.00 145.00   1.00   30.00    --  111.00 111.00 150.00   29
 39  \w     83.00 109.00   1.00   30.00    --  111.00  61.00-150.00   26
 40  \w     91.00 117.00   1.00   30.00    --  111.00  61.00 -30.00   26
 41  \w    136.00 150.00   1.00   30.00    --  111.00  61.00 -30.00   14
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0834471000
_diffrn_orient_matrix_UB_12      -0.0562957000
_diffrn_orient_matrix_UB_13      -0.0205853000
_diffrn_orient_matrix_UB_21      -0.0015725000
_diffrn_orient_matrix_UB_22      -0.0000105000
_diffrn_orient_matrix_UB_23      0.0823927000
_diffrn_orient_matrix_UB_31      -0.0814214000
_diffrn_orient_matrix_UB_32      0.0576722000
_diffrn_orient_matrix_UB_33      -0.0200948000
_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  0.0401
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41306
_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         76.358
_diffrn_reflns_theta_min         4.065
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.288
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.215
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         9754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+2.9147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8425
_reflns_number_total             9754
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03832k2.cif
_cod_data_source_block           noninbecp
_cod_depositor_comments
'Adding full bibliography for 1572469--1572472.cif.'
_cod_database_code               1572470
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Be1 In1 N2 O1 C50 H50'
_shelx_estimated_absorpt_t_max   0.792
_shelx_estimated_absorpt_t_min   0.632
_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.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C15(H15), C20(H20), C27(H27)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C13(H13), C14(H14), C23(H23), C24(H24), C25(H25), C31(H31),
 C37(H37), C47(H47), C48(H48)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C),
 C53(H53A,H53B,H53C)
;
_shelx_res_checksum              35544
_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 1.104
_oxdiff_exptl_absorpt_empirical_full_min 0.914