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_7135258
_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         'C33 H66 Al Ca N5 Si4'
_chemical_formula_sum            'C33 H66 Al Ca N5 Si4'
_chemical_formula_weight         712.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-08-20
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6499(12)
_cell_length_b                   15.8975(17)
_cell_length_c                   20.806(2)
_cell_measurement_reflns_used    9781
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.669
_cell_measurement_theta_min      2.340
_cell_volume                     4184.1(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      100.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1044
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            76575
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         2.057
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.7373
_exptl_absorpt_correction_T_min  0.5783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1400 before and 0.1150 after correction.
The Ratio of minimum to maximum transmission is 0.7843.
The \l/2 correction factor is Not present.
;
_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    1.131
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.0128
_exptl_crystal_size_mid          0.0124
_exptl_crystal_size_min          0.0122
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 3194 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.013(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         7352
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0700P)^2^+0.3821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1140
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                6853
_reflns_number_total             7352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05693d2.cif
_cod_data_source_block           dmcmdca01_0ma
_cod_database_code               7135258
_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:
 C16(H16B,H16A), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C15(H15), C3(H3), C13(H13), C4(H4), C2(H2)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C28(H28A,H28B,H28C), C10(H10A,H10B,H10C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C26(H26A,
 H26B,H26C), C14(H14A,H14B,H14C), C30(H30A,H30B,H30C), C21(H21A,H21B,H21C),
 C25(H25A,H25B,H25C), C19(H19A,H19B,H19C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              76619
_olex2_submission_special_instructions 'No special instructions were received'