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_7062043
_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         'C24 H48 B Ir N2 P2, C7 H8'
_chemical_formula_sum            'C31 H56 B Ir N2 P2'
_chemical_formula_weight         721.72
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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_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                 106.885(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1126(7)
_cell_length_b                   15.5043(6)
_cell_length_c                   11.6052(4)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      69.74
_cell_measurement_theta_min      2.42
_cell_volume                     3290.7(2)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'CELL_NOW (Sheldrick, 2008) and SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         microfocus
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0855
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5445
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        64.042
_diffrn_reflns_theta_max         64.042
_diffrn_reflns_theta_min         2.416
_exptl_absorpt_coefficient_mu    8.919
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       plate
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.201
_refine_diff_density_min         -1.491
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5445
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+14.0672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1519
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4370
_reflns_number_total             5445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04914g3.cif
_cod_data_source_block           ax2387twin4neu
_cod_depositor_comments
'Adding full bibliography for 7062043--7062044.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7062043
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.297
_shelx_estimated_absorpt_t_max   0.617
_shelx_res_checksum              84933