Facile Insertion of Rh and Ir into a Boron-Phenyl Bond, Leading to Boryl/Bis(phosphine) PBP Pincer Complexes.
Shih, Wei-Chun; Gu, Weixing; MacInnis, Morgan C.; Timpa, Samuel D.; Bhuvanesh, Nattamai; Zhou, Jia; Ozerov, Oleg V.; Journal of the American Chemical Society 138 (2016) 2086–2089; doi:10.1021/jacs.5b11706

data_4129906
_publ_section_title
;
 Facile Insertion of Rh and Ir into a Boron-Phenyl Bond, Leading to
 Boryl/Bis(phosphine) PBP Pincer Complexes.
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2086
_journal_page_last               2089
_journal_paper_doi               10.1021/jacs.5b11706
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C24 H36 B Cl2 Ir P2'
_chemical_formula_sum            'C24 H36 B Cl2 Ir P2'
_chemical_formula_weight         660.38
_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_creation_date             2015-06-01
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.10.22 svn.r3046 for OlexSys, GUI svn.r4928)
;
_cell_angle_alpha                98.450(2)
_cell_angle_beta                 100.388(2)
_cell_angle_gamma                104.851(2)
_cell_formula_units_Z            4
_cell_length_a                   9.3083(19)
_cell_length_b                   16.768(3)
_cell_length_c                   17.565(4)
_cell_measurement_reflns_used    6993
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      28.864
_cell_measurement_theta_min      2.325
_cell_volume                     2552.2(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16030
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.204
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.577
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.451
_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 0.0989 before and 0.0413 after correction.
 The Ratio of minimum to maximum transmission is 0.60.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1477 before and 0.0614 after correction.
 The Ratio of minimum to maximum transmission is 0.60.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 47006 reflections, Rint = 0.0460
 (28404 with I > 3sig(I), Rint = 0.0401)
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.19
_refine_diff_density_max         3.639
_refine_diff_density_min         -1.581
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         16030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0305P)^2^+6.3724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12945
_reflns_number_total             16030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b11706_si_002.cif
_cod_data_source_block           8-Ir
_cod_database_code               4129906
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.417
_shelx_estimated_absorpt_t_min   0.260
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8661(3) 0.1339(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C19(H19), C22(H22), C13B(H13B), C16B(H16B), C19B(H19B),
 C22B(H22B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C3B(H3B),
 C4B(H4B), C5B(H5B), C6B(H6B), C8B(H8B), C9B(H9B), C10B(H10B), C11B(H11B)
3.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C14B(H14D,H14E,H14F), C15B(H15D,H15E,H15F), C17B(H17D,H17E,H17F),
 C18B(H18D,H18E,H18F), C20B(H20D,H20E,H20F), C21B(H21D,H21E,H21F), C23B(H23D,
 H23E,H23F), C24B(H24D,H24E,H24F)
;
_shelx_res_checksum              97676
_shelx_hkl_checksum              59437
_olex2_submission_special_instructions 'No special instructions were received'