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_1572471
_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 Ga N2 O'
_chemical_formula_sum            'C52 H67 Ga N2 O'
_chemical_formula_weight         805.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-03
_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                 103.2039(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.3033(2)
_cell_length_b                   17.3028(2)
_cell_length_c                   27.4999(4)
_cell_measurement_reflns_used    64441
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      40.1500
_cell_measurement_theta_min      1.6110
_cell_volume                     8942.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.83a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.83a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.83a (Rigaku OD, 2023)'
_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      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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -11.00  15.00   0.50   25.00    --   -0.16 -17.00 161.00   52
  2  \w    -49.00 -21.00   0.50   25.00    --   -0.16 -17.00 161.00   56
  3  \w     16.00  50.00   0.50   25.00    --   -0.16  17.00 -29.00   68
  4  \w    -11.00  34.00   0.50   25.00    --   -0.16  93.00-132.54   90
  5  \w     -6.00  22.00   0.50   25.00    --   -0.16  99.00 139.16   56
  6  \w     -3.00  30.00   0.50   25.00    --   -0.16  95.00 116.82   66
  7  \w    -14.00  13.00   0.50   25.00    --   -0.16 102.00  29.01   54
  8  \w    -49.00 -24.00   0.50   25.00    --   -0.16 -47.00 -44.61   50
  9  \w    -16.00   9.00   0.50   25.00    --   -0.16 100.00 -17.27   50
 10  \w    -12.00  22.00   0.50   25.00    --   -0.16  93.00 -10.40   68
 11  \w    -31.00  12.00   0.50   25.00    --   20.00 -35.00  -6.82   86
 12  \w    -28.00  -1.00   0.50   25.00    --   20.00 -49.00  97.24   54
 13  \w     -1.00  47.00   0.50   25.00    --   -0.16  31.00 151.35   96
 14  \w    -46.00 -20.00   0.50   25.00    --    4.00 -22.00 -88.94   52
 15  \w    -11.00  30.00   0.50   25.00    --    4.00 -22.00 -88.94   82
 16  \w    -14.00  30.00   0.50   25.00    --   12.00 -25.00 162.93   88
 17  \w     -6.00  22.00   0.50   25.00    --   12.00 -27.00  71.66   56
 18  \w      1.00  32.00   0.50   25.00    --   12.00 -24.00  30.05   62
 19  \w    -38.00  29.00   0.50   25.00    --   12.00 -25.00  -3.29  134
 20  \w    -15.00  27.00   0.50   25.00    --   20.00 -28.00  35.58   84
 21  \w    -31.00  29.00   0.50   25.00    --   20.00 -27.00-102.77  120
 22  \w    -13.00  34.00   0.50   25.00    --   20.00 -26.00-173.74   94
 23  \w     25.00  51.00   0.50   25.00    --   20.00-125.00  32.75   52
 24  \w     16.00  42.00   0.50   25.00    --   20.00-110.00-178.28   52
 25  \w     17.00  42.00   0.50   25.00    --   20.00-109.00 -58.94   50
 26  \w      5.00  34.00   0.50   25.00    --   20.00 -26.00 122.92   58
 27  \w    -32.00  -6.00   0.50   25.00    --   20.00 -26.00 122.92   52
 28  \w      4.00  11.00   0.50   25.00    --   20.00 -26.00  72.31   14
;
_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      -0.0113743000
_diffrn_orient_matrix_UB_12      0.0027508000
_diffrn_orient_matrix_UB_13      -0.0263452000
_diffrn_orient_matrix_UB_21      -0.0350686000
_diffrn_orient_matrix_UB_22      0.0082924000
_diffrn_orient_matrix_UB_23      0.0023534000
_diffrn_orient_matrix_UB_31      0.0080362000
_diffrn_orient_matrix_UB_32      0.0400540000
_diffrn_orient_matrix_UB_33      0.0013340000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            142875
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.212
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.456
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.83a (Rigaku Oxford Diffraction, 2023)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       block
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         10241
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+39.4598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1618
_refine_ls_wR_factor_ref         0.1667
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8760
_reflns_number_total             10241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03832k2.cif
_cod_data_source_block           187ccaec23_2)077cut
_cod_depositor_comments
'Adding full bibliography for 1572469--1572472.cif.'
_cod_original_cell_volume        8942.17(19)
_cod_database_code               1572471
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C25 H25 Ga2 N2 O2'
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.813
_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. Restrained distances
 C21-C24 \\sim C21-C24A
 with sigma of 0.02
 C21-C22 \\sim C21-C22A
 with sigma of 0.02
 C21-C23 \\sim C21-C23A
 with sigma of 0.02
3. Others
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(1)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C8(H8), C43(H43), C15(H15), C50(H50)
4.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C19(H19), C25(H25), C37(H37), C13(H13), C12(H12), C46(H46),
 C48(H48), C11(H11), C47(H47), C4(H4), C3(H3), C5(H5), C2(H2)
4.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C10(H10A,H10B,H10C), C44(H44A,H44B,
 H44C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C9(H9A,H9B,H9C), C35(H35A,
 H35B,H35C), C45(H45A,H45B,H45C), C36(H36A,H36B,H36C), C34(H34A,H34B,H34C),
 C52(H52A,H52B,H52C), C51(H51A,H51B,H51C), C24(H24A,H24B,H24C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24A(H24D,H24E,H24F), C22A(H22D,H22E,H22F),
 C23A(H23D,H23E,H23F)
;
_shelx_res_checksum              77747
_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 1.195
_oxdiff_exptl_absorpt_empirical_full_min 0.745