Primary and secondary coordination sphere Lewis acid interactions in β-phosphinoethylborane-ligated rhodium and iridium complexes
Nichols, Brian R.; Petersen, Jeffrey L.; Dolinar, Brian S.; Popp, Brian V.; New Journal of Chemistry 49 (2025) 14073–14081; doi:10.1039/D5NJ01429H

data_7063910
_publ_section_title
;
 Primary and secondary coordination sphere Lewis acid interactions in
 \b-phosphinoethylborane-ligated rhodium and iridium complexes
;
_journal_issue                   32
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14073
_journal_page_last               14081
_journal_paper_doi               10.1039/D5NJ01429H
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C32 H43 B Cl Ir N P'
_chemical_formula_sum            'C32 H43 B Cl Ir N P'
_chemical_formula_weight         711.10
_chemical_name_systematic
chloro-[(1,2,5,6-\h)-cycloocta-1,5-diene]-[{9-[2-(diphenylphosphanyl)ethyl]-9\l5-borabicyclo[3.3.1]nonan-9-yl}(ethylidyne)-\l5-azane]-iridium
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Air-sensitive,Moisture-sensitive
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2025-06-22 deposited with the CCDC.	2025-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                114.412(2)
_cell_angle_beta                 93.805(2)
_cell_angle_gamma                92.019(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8906(9)
_cell_length_b                   12.8325(13)
_cell_length_c                   13.1400(13)
_cell_measurement_reflns_used    7813
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.56
_cell_volume                     1511.7(3)
_computing_cell_refinement       'SMART (version 5.6)'
_computing_data_collection       'SMART (version 5.6)'
_computing_data_reduction        'SAINT (version 5/6.0)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Siemens P4, CCD detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10597
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    4.579
_exptl_absorpt_correction_T_max  0.803
_exptl_absorpt_correction_T_min  0.305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             712
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.206
_refine_diff_density_min         -1.346
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+0.3738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                5858
_reflns_number_total             6729
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d5nj01429h2.cif
_cod_data_source_block           bp16ccd
_cod_depositor_comments
'Adding full bibliography for 7063906--7063912.cif.'
_cod_database_code               7063910
_shelx_res_checksum              1661