Insight into the Hydrogen Migration Processes Involved in the Formation of Metal‒Borane Complexes: Importance of the Third Arm of the Scorpionate Ligand
Tsoureas, Nikolaos; Hamilton, Alex; Haddow, Mairi F.; Harvey, Jeremy N.; Orpen, A. Guy; Owen, Gareth R.; Organometallics 32 (2013) 2840–; doi:10.1021/om4002389

data_4080839
_publ_section_title
;
 Insight into the Hydrogen Migration Processes Involved in the Formation
 of Metal--Borane Complexes: Importance of the Third Arm of the
 Scorpionate Ligand
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2840
_journal_paper_doi               10.1021/om4002389
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C36 H39 B Ir N6 O4 P'
_chemical_formula_sum            'C36 H39 B Ir N6 O4 P'
_chemical_formula_weight         853.71
_chemical_name_common            Complex_13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.987(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.3955(8)
_cell_length_b                   15.0565(8)
_cell_length_c                   33.9742(17)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.29
_cell_volume                     7641.8(7)
_computing_cell_refinement       'Bruker Apex2'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker ShelXTL'
_computing_publication_material  'Bruker ShelXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            285993
_diffrn_reflns_theta_full        30.55
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    3.581
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_platon_squeeze_details
; 
Crystallised from toluene.
;
_refine_diff_density_max         2.949
_refine_diff_density_min         -4.808
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         23344
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+25.7920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                19838
_reflns_number_total             23344
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4002389_si_002.cif
_cod_data_source_block           Complex_13_nt_irborco_phosphite
_cod_database_code               4080839