Intriguing Metal-Ligand Interplays Leading to Diverse Al-H-M (M = Mg, Ca) Heterobimetallic Hydrides on a Picolyl-Based 3N Ligand
Mandal, Chhotan; Kundu, Abhishek; Panda, Sourav; Mukherjee, Debabrata; Chemical Communications  (2025) –; doi:10.1039/D5CC05693D

data_7135256
_publ_section_title
;
 Intriguing Metal-Ligand Interplays Leading to Diverse Al-H-M (M = Mg, Ca)
 Heterobimetallic Hydrides on a Picolyl-Based 3N Ligand
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D5CC05693D
_journal_year                    2025
_chemical_formula_moiety         'C21 H32 Al N3'
_chemical_formula_sum            'C21 H32 Al N3'
_chemical_formula_weight         353.47
_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   mixed
_audit_creation_date             2025-08-18
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-08-21 deposited with the CCDC.	2025-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.464(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.931(3)
_cell_length_b                   9.974(3)
_cell_length_c                   19.421(5)
_cell_measurement_reflns_used    3760
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.124
_cell_measurement_theta_min      2.115
_cell_volume                     2116.7(10)
_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)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1652
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            51775
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.124
_diffrn_reflns_theta_max         25.124
_diffrn_reflns_theta_min         2.115
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.013
_exptl_crystal_size_mid          0.0126
_exptl_crystal_size_min          0.0122
_exptl_transmission_factor_max   0.999
_exptl_transmission_factor_min   0.999
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0437P)^2^+1.7618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2572
_reflns_number_total             3760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05693d2.cif
_cod_data_source_block           mesalh2_a
_cod_original_cell_volume        2116.6(10)
_cod_database_code               7135256
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C10(H10A,H10B), C11(H11A,H11B), C20(H20A,H20B), C21(H21A,H21B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C13(H13), C17(H17), C18(H18), C19(H19)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C)
;
_shelx_res_checksum              42508
_olex2_submission_special_instructions 'No special instructions were received'