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_4080840
_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         'C21 H16 B IR N4 O, C7 C8'
_chemical_formula_sum            'C28 H24 B Ir N4 O'
_chemical_formula_weight         635.52
_chemical_name_common            Complex_20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   18.4965(4)
_cell_length_b                   18.4965(4)
_cell_length_c                   38.7777(7)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      3.15
_cell_volume                     11489.3(4)
_computing_cell_refinement       'Apex II (Bruker-AXS, 2007)'
_computing_data_collection       'Apex II (Bruker-AXS, 2007)'
_computing_data_reduction
; 
 SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) 
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.766
_diffrn_measurement_device_type  '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  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            70035
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.61
_diffrn_reflns_theta_min         3.30
_exptl_absorpt_coefficient_mu    5.257
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.8872
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'sadabs - bruker 2008'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5580
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
Crystallised from toluene and pentane
;
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         6032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0140P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0425
_refine_ls_wR_factor_ref         0.0436
_reflns_number_gt                5141
_reflns_number_total             6032
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4002389_si_002.cif
_cod_data_source_block           Complex_20_nt_irborcobai
_cod_original_cell_volume        11489.2(4)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4080840