Reversible Borylene Formation from Ring Opening of Pinacolborane and Other Intermediates Generated from Five-Coordinate Tris-Boryl Complexes: Implications for Catalytic C‒H Borylation
Ghaffari, Behnaz; Vanchura, Britt A.; Chotana, Ghayoor A.; Staples, Richard J.; Holmes, Daniel; Maleczka, Robert E.; Smith, Milton R.; Organometallics 34 (2015) 4732–; doi:10.1021/acs.organomet.5b00525

data_4086196
_publ_section_title
;
 Reversible Borylene Formation from Ring Opening of Pinacolborane and
 Other Intermediates Generated from Five-Coordinate Tris-Boryl Complexes:
 Implications for Catalytic C--H Borylation
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4732
_journal_paper_doi               10.1021/acs.organomet.5b00525
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C28 H70 Ir2 P4'
_chemical_formula_sum            'C28 H70 Ir2 P4'
_chemical_formula_weight         915.12
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.7800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2844(8)
_cell_length_b                   14.0396(10)
_cell_length_c                   12.9636(10)
_cell_measurement_reflns_used    7931
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.360
_cell_measurement_theta_min      2.204
_cell_volume                     1772.1(2)
_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  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_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_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14563
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.364
_diffrn_reflns_theta_min         2.092
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.698
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6372
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0785 before and 0.0465 after correction.
The Ratio of minimum to maximum transmission is 0.8551.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       plate
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.043
_refine_diff_density_max         2.447
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0450P)^2^+2.9670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2725
_reflns_number_total             3249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00525_si_004.cif
_cod_data_source_block           mrs515b
_cod_depositor_comments          'Adding full bibliography for 4086196.cif.'
_cod_database_code               4086196
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.733
_shelx_estimated_absorpt_t_min   0.416
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All Ir(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 Ir1(H,HA,HB)
2.b Ternary CH refined with riding coordinates:
 C3(H3), C6(H6), C9(H9), C12(H12)
2.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              38981
_shelx_hkl_checksum              80325
_olex2_submission_special_instructions 'No special instructions were received'