Catalytic dehydrocoupling of methylamine borane using Yamashita's [Ir(PBP)] boryl complex – characterisation of a novel highly fluxional Ir tetrahydride
Decker, David; Drexler, Hans-Joachim; Baumann, Wolfgang; Reiß, Fabian; Beweries, Torsten; New Journal of Chemistry 46 (2022) 22314–22321; doi:10.1039/D2NJ04914G

data_7062044
_publ_section_title
;
 Catalytic dehydrocoupling of methylamine borane using Yamashita's
 [Ir(PBP)] boryl complex -- characterisation of a novel highly fluxional
 Ir tetrahydride
;
_journal_issue                   46
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              22314
_journal_page_last               22321
_journal_paper_doi               10.1039/D2NJ04914G
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C25 H46 B Ir N2 O P2, C4 H8 O'
_chemical_formula_sum            'C29 H54 B Ir N2 O2 P2'
_chemical_formula_weight         727.69
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-09-01 deposited with the CCDC.	2022-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_c                   34.2767(13)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.70
_cell_measurement_theta_min      2.72
_cell_volume                     6452.1(4)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
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_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
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_diffrn_measured_fraction_theta_max 1.000
_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  0.0437
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
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_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            103504
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
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_diffrn_source                   'fine-focus sealed tube'
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_exptl_absorpt_correction_T_min  0.6717
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            red
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_exptl_crystal_F_000             2960
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         6333
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_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0129P)^2^+16.1269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0453
_refine_ls_wR_factor_ref         0.0483
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5497
_reflns_number_total             6333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04914g3.cif
_cod_data_source_block           ax2223absa
_cod_depositor_comments
'Adding full bibliography for 7062043--7062044.cif.'
_cod_database_code               7062044
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_shelx_estimated_absorpt_t_min   0.567
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_shelx_res_checksum              67365