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_7063909
_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 Cl Ir P'
_chemical_formula_sum            'C30 H40 B Cl Ir P'
_chemical_formula_weight         670.05
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-17
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-06-22 deposited with the CCDC.	2025-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                65.4390(10)
_cell_angle_beta                 75.5410(10)
_cell_angle_gamma                62.3010(10)
_cell_formula_units_Z            2
_cell_length_a                   10.9766(6)
_cell_length_b                   11.6327(7)
_cell_length_c                   12.9516(7)
_cell_measurement_reflns_used    9831
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.43
_cell_measurement_theta_min      2.82
_cell_volume                     1328.48(13)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2 v2013.10-0'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'PHOTON 2 CMOS detector'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'Triumph Monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24950
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.545
_diffrn_reflns_theta_min         2.816
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    5.204
_exptl_absorpt_correction_T_max  0.746070
_exptl_absorpt_correction_T_min  0.516703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1117 before and 0.0616 after correction.
 
For component 2:
 wR2(int) was 0.1125 before and 0.0634 after correction.
 The Ratio of minimum to maximum transmission is 0.69.

Final HKLF 4 output contains 67459 reflections, Rint = 0.0691
 (44484 with I > 3sig(I), Rint = 0.0549)
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             668
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane/pentane'
_exptl_crystal_size_max          0.478
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.089
_refine_diff_density_max         1.297
_refine_diff_density_min         -1.877
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       0.0028(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         24950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0377P)^2^+0.5856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22203
_reflns_number_total             24950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01429h2.cif
_cod_data_source_block           bp96_0m_5_a
_cod_depositor_comments
'Adding full bibliography for 7063906--7063912.cif.'
_cod_database_code               7063909
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.655
_shelx_estimated_absorpt_t_min   0.190
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5526(6)
 0.4474(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Ternary CH refined with riding coordinates:
 C15(H15), C19(H19), C23(H23), C24(H24), C27(H27), C28(H28)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C25(H25A,H25B), C26(H26A,H26B),
  C29(H29A,H29B), C30(H30A,H30B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14)
;
_shelx_res_checksum              46612
_olex2_submission_special_instructions 'No special instructions were received'