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_7135257
_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         'C33 H68 Al Mg N5 Si4'
_chemical_formula_sum            'C33 H68 Al Mg N5 Si4'
_chemical_formula_weight         698.57
_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   mixed
_audit_creation_date             2025-01-30
_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                 100.0930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.95580(10)
_cell_length_b                   17.06120(10)
_cell_length_c                   24.83840(10)
_cell_measurement_reflns_used    40123
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      68.1630
_cell_measurement_theta_min      2.5660
_cell_volume                     4153.71(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.119a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.119a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.119a (Rigaku OD, 2024)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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    -22.00  69.00   0.50    0.50    --   40.58 -81.00-138.00  182
  2  \w   -152.00 -78.00   0.50    3.00    --  -82.50 -81.00-138.00  148
  3  \w   -152.00 -78.00   0.50    3.00    --  -82.50 -81.00-138.00  148
  4  \w   -111.00 -13.00   0.50    3.00    --  -82.50  81.00 -16.00  196
  5  \w     28.00 125.00   0.50    3.00    --   96.67 -81.00-138.00  194
  6  \w    100.00 166.00   0.50    3.00    --   96.67  81.00 -16.00  132
  7  \w   -109.00 -63.00   0.50    0.50    --  -40.58-139.00   0.00   92
  8  \w   -108.00 -27.00   0.50    0.50    --  -40.58 -32.00  30.00  162
  9  \w    -24.00  35.00   0.50    0.50    --  -40.58  11.00-120.00  118
 10  \w   -109.00 -63.00   0.50    0.50    --  -40.58-139.00  30.00   92
 11  \w   -109.00 -63.00   0.50    0.50    --  -40.58-139.00 150.00   92
 12  \w    -69.00  29.00   0.50    0.50    --  -40.58  81.00 -16.00  196
 13  \w    -48.00  27.00   0.50    0.50    --  -40.58  43.00-120.00  150
 14  \w   -109.00 -63.00   0.50    0.50    --  -40.58-139.00-120.00   92
 15  \w    -69.00  29.00   0.50    0.50    --  -40.58  81.00 -16.00  196
 16  \w    -35.00  24.00   0.50    0.50    --   40.58 -11.00-150.00  118
 17  \w    -31.00  28.00   0.50    0.50    --   40.58 -21.00 -90.00  118
 18  \w    -31.00  28.00   0.50    0.50    --   40.58 -21.00  60.00  118
 19  \w    -47.00 -15.00   0.50    3.00    --  -82.50  42.00  90.00   64
 20  \w   -156.00 -83.00   0.50    3.00    --  -82.50 -96.00 -60.00  146
 21  \w    -47.00 -15.00   0.50    3.00    --  -82.50  42.00-150.00   64
 22  \w     29.00  83.00   0.50    3.00    --   96.67 -68.00-120.00  108
 23  \w    105.00 170.00   0.50    3.00    --   96.67  96.00  30.00  130
 24  \w     70.00 165.00   0.50    3.00    --   96.67  77.00 -30.00  190
 25  \w     82.00 167.00   0.50    3.00    --   96.67  25.00 -60.00  170
 26  \w     70.00 165.00   0.50    3.00    --   96.67  77.00 -30.00  190
 27  \w     29.00  83.00   0.50    3.00    --   96.67 -68.00  30.00  108
 28  \w     83.00 164.00   0.50    3.00    --   96.67  33.00  90.00  162
 29  \w     29.00  68.00   0.50    3.00    --   96.67 -59.00-150.00   78
 30  \w     29.00  83.00   0.50    3.00    --   96.67 -68.00  60.00  108
 31  \w     30.00  57.00   0.50    3.00    --   96.67 -50.00 -30.00   54
 32  \w     33.00 109.00   0.50    3.00    --   96.67-117.00  60.00  152
 33  \w     29.00  68.00   0.50    3.00    --   96.67 -59.00 -90.00   78
 34  \w     30.00  57.00   0.50    3.00    --   96.67 -50.00-150.00   54
 35  \w     33.00 109.00   0.50    3.00    --   96.67-117.00-180.00  152
 36  \w     29.00  68.00   0.50    3.00    --   96.67 -59.00 -60.00   78
 37  \w     33.00 109.00   0.50    3.00    --   96.67-117.00-180.00  152
 38  \w     30.00  57.00   0.50    3.00    --   96.67 -50.00  60.00   54
 39  \w     99.00 161.00   0.50    3.00    --   96.67 117.00 -60.00  124
 40  \w   -109.00 -17.00   0.50    0.50    --  -40.58 -66.00  30.00  184
 41  \w   -109.00 -17.00   0.50    0.50    --  -40.58 -66.00 -30.00  184
 42  \w   -109.00 -17.00   0.50    0.50    --  -40.58 -66.00 150.00  184
 43  \w   -109.00 -17.00   0.50    0.50    --  -40.58 -66.00-120.00  184
 44  \w   -109.00 -14.00   0.50    0.50    --  -40.58 -77.00 -60.00  190
 45  \w     14.00 109.00   0.50    0.50    --   40.58  77.00-120.00  190
 46  \w     41.00 100.00   0.50    0.50    --   40.58-139.00-180.00  118
 47  \w     14.00 109.00   0.50    0.50    --   40.58  77.00  90.00  190
 48  \w     14.00 109.00   0.50    0.50    --   40.58  77.00-180.00  190
 49  \w     17.00 109.00   0.50    0.50    --   40.58  66.00 150.00  184
 50  \w     75.00 124.00   0.50    3.00    --   96.67  59.00-120.00   98
 51  \w     78.00 163.00   0.50    3.00    --   96.67  50.00  30.00  170
 52  \w     71.00 170.00   0.50    3.00    --   96.67  17.00-150.00  198
 53  \w     75.00 164.00   0.50    3.00    --   96.67  59.00 120.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            54018
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.272
_diffrn_reflns_theta_min         3.158
_exptl_absorpt_coefficient_mu    1.886
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.119a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brownish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.0121
_exptl_crystal_size_mid          0.0113
_exptl_crystal_size_min          0.0112
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         7569
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0423P)^2^+1.6879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6958
_reflns_number_total             7569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05693d2.cif
_cod_data_source_block           dm_cm_mgh_auto
_cod_database_code               7135257
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C1(H1)
1.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C16(H16A,H16B), C15(H15A,H15B), C20(H20A,H20B), C18(H18A,H18B)
1.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C4(H4), C3(H3), C2(H2)
1.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C8(H8A,H8B,H8C), C25(H25A,H25B,H25C), C27(H27A,H27B,
 H27C), C26(H26A,H26B,H26C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C),
 C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C13(H13A,H13B,H13C), C21(H21A,H21B,
 H21C), C28(H28A,H28B,H28C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              69542
_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
;