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_7063912
_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         'C88 H112 B4 Cl2 P4 Rh2'
_chemical_formula_sum            'C88 H112 B4 Cl2 P4 Rh2'
_chemical_formula_weight         1613.61
_chemical_name_systematic
Dichlorotetrakis{2-[9-borabicyclo[3.3.1]nonan-9-yl]ethyl}(diphenyl)phosphine)}dirhodium
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2025-06-22 deposited with the CCDC.	2025-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                96.1831(12)
_cell_angle_beta                 100.4360(11)
_cell_angle_gamma                114.9881(11)
_cell_formula_units_Z            2
_cell_length_a                   12.2787(5)
_cell_length_b                   14.2439(6)
_cell_length_c                   25.4195(10)
_cell_measurement_reflns_used    9675
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      30.0779
_cell_measurement_theta_min      2.9919
_cell_volume                     3877.4(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 V2014.1-7'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker AXS D8 Venture fixed-chi'
_diffrn_measurement_method       'omega scan, PHOTON 100 CMOS'
_diffrn_radiation_monochromator  Triumph
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            88431
_diffrn_reflns_theta_full        30.10
_diffrn_reflns_theta_max         30.10
_diffrn_reflns_theta_min         2.99
_diffrn_source_type              fine-focus
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/3 (Bruker AXS Inc.)'
_exptl_crystal_colour            'light orange'
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             1688
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane/pentane'
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.146
_refine_diff_density_max         1.913
_refine_diff_density_min         -0.717
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         22711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0342P)^2^+5.7918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                18876
_reflns_number_total             22711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01429h2.cif
_cod_data_source_block           bp35cms
_cod_depositor_comments
'Adding full bibliography for 7063906--7063912.cif.'
_cod_database_code               7063912
_shelx_res_checksum              16910