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_7063907
_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         'C30 H40 B Ir N3 P'
_chemical_formula_sum            'C30 H40 B Ir N3 P'
_chemical_formula_weight         676.63
_chemical_name_systematic
'[(1,2,5,6-\h)-cycloocta-1,5-diene]-(3-{9-[2-(diphenylphosphanyl)ethyl]-9\l5-borabicyclo[3.3.1]nonan-9-yl}triaza-1,2-dien-2-ium-1-ide)-iridium'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_audit_creation_date             2025-06-12
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-06-22 deposited with the CCDC.	2025-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.6544(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0583(5)
_cell_length_b                   14.1410(5)
_cell_length_c                   16.6581(6)
_cell_measurement_reflns_used    9841
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.5419
_cell_measurement_theta_min      3.0899
_cell_volume                     2781.92(18)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 v2013.10-0'
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker AXS D8 Venture fixed chi'
_diffrn_measurement_method       'omega scan, PHOTON 100 CMOS'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20403
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.247
_diffrn_reflns_theta_min         3.090
_exptl_absorpt_coefficient_mu    4.881
_exptl_absorpt_correction_T_max  0.36
_exptl_absorpt_correction_T_min  0.18
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'light orange'
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1352
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane/Pentane'
_exptl_crystal_size_max          0.553
_exptl_crystal_size_mid          0.422
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.640
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0046P)^2^+9.9830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0611
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4459
_reflns_number_total             4980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01429h2.cif
_cod_data_source_block           bp4cms
_cod_depositor_comments
'Adding full bibliography for 7063906--7063912.cif.'
_cod_database_code               7063907
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.363
_shelx_estimated_absorpt_t_min   0.173
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3), C7(H7), C23(H23), C24(H24), C27(H27), C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C25(H25A,H25B), C26(H26A,H26B), C29(H29A,H29B),
 C30(H30A,H30B)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22)
;
_shelx_res_checksum              7588
_olex2_submission_special_instructions 'No special instructions were received'