Amidines: a deeper look at the archetypal pro-ligand.
de Vere-Tucker, Matthew; Squire, Imogen; Tritto, Michelangelo; Anandkar, Rohil; Syeda, Tayyibah; Uthayan, Divia; Aguila, Gabrielle; Silva de Moraes, Lygia; Bakewell, Clare; Dalton transactions (Cambridge, England : 2003) 55 (2026) 4977–4987; doi:10.1039/d6dt00276e

data_7720575
_publ_section_title
;
 Amidines: a deeper look at the archetypal pro-ligand.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4977
_journal_page_last               4987
_journal_paper_doi               10.1039/d6dt00276e
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C33 H45 Al N2'
_chemical_formula_sum            'C33 H45 Al N2'
_chemical_formula_weight         496.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-12-08
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-01-30 deposited with the CCDC.	2026-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                83.387(2)
_cell_angle_beta                 72.037(2)
_cell_angle_gamma                79.219(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5994(2)
_cell_length_b                   11.5430(3)
_cell_length_c                   14.6201(4)
_cell_measurement_reflns_used    23795
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      35.8220
_cell_measurement_theta_min      2.9190
_cell_volume                     1510.96(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.122a 64-bit (release 15-05-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_detector_type            'Eiger2 1M'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.933
_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    -33.00  51.00   0.50    6.12    --   25.88 -77.00-180.00  168
  2  \w     14.00  97.00   0.50    6.12    --   25.88  38.00-120.00  166
  3  \w    -29.00  52.00   0.50    6.12    --   25.88 -77.00 -60.00  162
  4  \w    -32.00  51.00   0.50    6.12    --   25.88 -77.00  90.00  166
  5  \w     14.00  98.00   0.50    6.12    --   25.88  38.00   0.00  168
  6  \w      5.00  87.00   0.50    6.12    --   25.88  77.00 150.00  164
  7  \w     11.00  86.00   0.50    6.12    --   25.88  57.00  90.00  150
  8  \w      3.00  87.00   0.50    6.12    --   25.88  77.00-120.00  168
  9  \w    -33.00  52.00   0.50    6.12    --   25.88 -77.00  60.00  170
 10  \w      0.00  87.00   0.50    6.12    --   25.88  77.00   0.00  174
 11  \w    -40.00  42.00   0.50    6.12    --   25.88 -57.00-150.00  164
 12  \w    -28.00  52.00   0.50    6.12    --   25.88 -77.00 -30.00  160
 13  \w    -29.00  15.00   0.50    6.12    --   25.88 -77.00 -90.00   88
 14  \w     25.00  52.00   0.50    6.12    --   25.88 -77.00 -90.00   54
 15  \w      1.00  86.00   0.50    6.12    --   25.88  77.00 120.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Eiger2 1M'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0782611000
_diffrn_orient_matrix_UB_12      -0.0161897000
_diffrn_orient_matrix_UB_13      -0.0158789000
_diffrn_orient_matrix_UB_21      -0.0044958000
_diffrn_orient_matrix_UB_22      -0.0467850000
_diffrn_orient_matrix_UB_23      0.0362528000
_diffrn_orient_matrix_UB_31      -0.0069167000
_diffrn_orient_matrix_UB_32      -0.0384286000
_diffrn_orient_matrix_UB_33      -0.0323208000
_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  0.0700
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            64695
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.249
_diffrn_reflns_theta_min         2.631
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.240
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (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            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         14592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0615P)^2^+0.1027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10175
_reflns_number_total             14592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00276e3.cif
_cod_data_source_block           dippAmoXylAlH2_10-Al
_cod_depositor_comments
'Adding full bibliography for 7720566--7720581.cif.'
_cod_database_code               7720575
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Al C30 N2 H80'
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.969
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C31(H31), C16(H16), C28(H28), C19(H19)
1.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C26(H26), C24(H24), C4(H4), C5(H5), C25(H25), C12(H12), C14(H14),
 C13(H13)
1.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C),
 C33(H33A,H33B,H33C), C20(H20A,H20B,H20C), C30(H30A,H30B,H30C), C18(H18A,H18B,
 H18C), C32(H32A,H32B,H32C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              39725
_shelx_hkl_checksum              47537
_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 1.340
_oxdiff_exptl_absorpt_empirical_full_min 0.741