A picolinamide iridium catalyst immobilized on an aluminum-hydride anchor for the selective dehydrogenation of neat formic acid.
Alrais, Lujain; Dutta, Indranil; Hengne, Amol; Chakraborty, Priyanka; Abou-Hamad, Edy; Xi, Shibo; Rahman, Mohammad Misbahur; Zhang, Jia; Chen, Benjamin W. J.; Basset, Jean-Marie; Huang, Kuo-Wei; Dalton transactions (Cambridge, England : 2003) 54 (2025) 5119–5127; doi:10.1039/d4dt03521f

data_7718056
_publ_section_title
;
 A picolinamide iridium catalyst immobilized on an aluminum-hydride anchor
 for the selective dehydrogenation of neat formic acid.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5119
_journal_page_last               5127
_journal_paper_doi               10.1039/d4dt03521f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         '2(C20 H31 Cl Ir N4 O), C H2 Cl2, 2(F6 P)'
_chemical_formula_sum            'C41 H64 Cl4 F12 Ir2 N8 O2 P2'
_chemical_formula_weight         1517.14
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-12-22 deposited with the CCDC.	2025-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.759(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0034(11)
_cell_length_b                   12.3704(9)
_cell_length_c                   30.741(2)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      36.41
_cell_measurement_theta_min      2.20
_cell_volume                     5306.8(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.01
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0940
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            61501
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.449
_diffrn_reflns_theta_min         2.116
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.358
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.3341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_description       block
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         9.259
_refine_diff_density_min         -6.423
_refine_diff_density_rms         0.356
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.665
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         25497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.665
_refine_ls_R_factor_all          0.1501
_refine_ls_R_factor_gt           0.1065
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2784
_refine_ls_wR_factor_ref         0.2938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17524
_reflns_number_total             25497
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03521f2.cif
_cod_data_source_block           Ir
_cod_depositor_comments          'Adding full bibliography for 7718056.cif.'
_cod_original_cell_volume        5306.9(7)
_cod_database_code               7718056
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.446
_shelx_estimated_absorpt_t_min   0.385
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C29(H29A,H29B), C30(H30A,H30B), C40(H40A,H40B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C21(H21), C22(H22), C24(H24)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), N4(H4A,H4B,H4C),
  C01P(H01A,H01B,H01C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), N8(H8A,
 H8B,H8C)
;
_olex2_submission_special_instructions 'No special instructions were received'