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_7135261
_publ_section_title
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 Intriguing Metal-Ligand Interplays Leading to Diverse Al-H-M (M = Mg, Ca)
 Heterobimetallic Hydrides on a Picolyl-Based 3N Ligand
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D5CC05693D
_journal_year                    2025
_chemical_formula_moiety         'C37 H76 Al Ca N5 O Si4'
_chemical_formula_sum            'C40.3 H83.7 Al Ca N5 O Si4'
_chemical_formula_weight         833.84
_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             2025-08-19
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
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2025-08-21 deposited with the CCDC.	2025-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.6140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.04900(10)
_cell_length_b                   19.6928(3)
_cell_length_c                   23.4848(3)
_cell_measurement_reflns_used    9166
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.511
_cell_measurement_theta_min      3.807
_cell_volume                     5052.32(11)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.985
_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  0.0664
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            78619
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.511
_diffrn_reflns_theta_min         3.807
_exptl_absorpt_coefficient_mu    2.395
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   multi-scan
_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    1.096
_exptl_crystal_description       block
_exptl_crystal_F_000             1830
_exptl_crystal_preparation       'solvent diffusion'
_exptl_crystal_size_max          0.0164
_exptl_crystal_size_mid          0.0134
_exptl_crystal_size_min          0.0125
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         9166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0674
_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^)+(0.0748P)^2^+6.8243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1679
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7825
_reflns_number_total             9166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05693d2.cif
_cod_data_source_block           dm_cm_alca12_auto
_cod_original_formula_sum        'C40.30 H83.70 Al Ca N5 O Si4'
_cod_database_code               7135261
_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 Ternary CH refined with riding coordinates:
 C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C20(H20A,H20B), C18(H18A,
 H18B), C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B), C36(H36A,H36B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C2(H2), C4(H4), C3(H3)
2.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C22(H22A,H22B,
 H22C), C25(H25A,H25B,H25C), C33(H33A,H33B,H33C), C32(H32A,H32B,H32C), C23(H23A,
 H23B,H23C), C27(H27A,H27B,H27C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C),
 C26(H26A,H26B,H26C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C29(H29A,H29B,H29C)
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_smtbx_masks_special_details
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A solvent mask was calculated and 102 electrons were 
found in a volume of 638\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.55[C6H14] per formula unit 
which account for 110 electrons 
per unit cell.
;
_shelx_res_checksum              7904
_shelx_fab_checksum              24591
_olex2_submission_special_instructions 'No special instructions were received'