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_4084796
_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         '(C29 H41 B N3 O3 Rh) 0.5 (C5 H12)'
_chemical_formula_sum            'C31.5 H47 B N3 O3 Rh'
_chemical_formula_weight         629.44
_chemical_name_common            Sad317
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_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                   29.675(19)
_cell_length_b                   9.355(6)
_cell_length_c                   11.583(7)
_cell_measurement_reflns_used    1959
_cell_measurement_temperature    173.(2)
_cell_measurement_theta_max      18.0672
_cell_measurement_theta_min      2.2592
_cell_volume                     3216(4)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.1835
_diffrn_reflns_av_sigmaI/netI    0.1001
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12408
_diffrn_reflns_theta_full        22.06
_diffrn_reflns_theta_max         22.06
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
The huge voids were observed in a crystal lattice. The quality of
data were very poor because of a bad quality of the only
available crystal and (related to this) very low resolution data.
SQUEEZE was used to treat electron density in those voids. The only
expected solvent in this structure was MeCN,l therefore 5 MeCN 
solvent molecules were added to the asymmetric unit of
 the crystall cell. The appropriate correction was applied to the 
UNIT instruction to obtain true metric results.

Two pentane solvent molecules per cell were assigned co compensate
calculated electron density in voids 

;
_refine_diff_density_max         1.513
_refine_diff_density_min         -1.794
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2071
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0855
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1235P)^2^+19.0807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2007
_refine_ls_wR_factor_ref         0.2128
_reflns_number_gt                1817
_reflns_number_total             2071
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500891h_si_002.cif
_cod_data_source_block           8ToMRhCOD
_cod_depositor_comments
'Adding full bibliography for 4084789--4084803.cif.'
_cod_original_cell_volume        3216.(4)
_cod_original_formula_sum        'C31.50 H47 B N3 O3 Rh'
_cod_database_code               4084796