Mixed N-Heterocyclic Carbene‒Bis(oxazolinyl)borato Rhodium and Iridium Complexes in Photochemical and Thermal Oxidative Addition Reactions
Xu, Songchen; Manna, Kuntal; Ellern, Arkady; Sadow, Aaron D.; Organometallics 33 (2014) 6840–; doi:10.1021/om500891h

data_4084791
_publ_section_title
;
 Mixed N-Heterocyclic Carbene--Bis(oxazolinyl)borato Rhodium and Iridium
 Complexes in Photochemical and Thermal Oxidative Addition Reactions
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6840
_journal_paper_doi               10.1021/om500891h
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         '(C31 H44 B N4 O2 Rh) 0.5 (C7 H8)'
_chemical_formula_sum            'C34.5 H48 B N4 O2 Rh'
_chemical_formula_weight         664.49
_space_group_IT_number           14
_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           'APEX2 v2012.4-3'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.544(9)
_cell_length_b                   14.553(7)
_cell_length_c                   11.657(6)
_cell_measurement_reflns_used    3313
_cell_measurement_temperature    173.(2)
_cell_measurement_theta_max      21.6370
_cell_measurement_theta_min      2.2385
_cell_volume                     3316(3)
_computing_cell_refinement       'SAINT V7.66A (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 Suite (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.66A (Bruker AXS, 2009)'
_computing_molecular_graphics    'XSHELL (Bruker AXS, 2007)'
_computing_publication_material  'APEX2 Suite (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  ' BRUKER APEX2 CCD Diffractometer'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25670
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
SQUEEZE indicated two diffused toluene solvent per
cell resulting in a  halve of the solvent molecule
per cluster
;
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.912
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         5843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0571P)^2^+0.0750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1246
_reflns_number_gt                4166
_reflns_number_total             5843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500891h_si_002.cif
_cod_data_source_block           3ImBuRhCOD
_cod_depositor_comments
'Adding full bibliography for 4084789--4084803.cif.'
_cod_original_cell_volume        3316.(3)
_cod_original_formula_sum        'C34.50 H48 B N4 O2 Rh'
_cod_database_code               4084791